Current Issue : July-September Volume : 2013 Issue Number : 3 Articles : 107 Articles
A simple, selective, rapid, precise and economical reverse phase high performance liquid chromatographic method has been developed for the simultaneous estimation of Meclizine and Caffeine from pharmaceutical formulation. The method was carried out on a C18 (25 cm x 4.6 mm i.d., 5 μ) column with a mobile phase consisting of Methanol and water in the ratio of 70:30 v/v. The retention time of Meclizine and Caffeine was 3.3 min and 4.3 min respectively with the flow rate of 1mL/min. Eluents were detected at 230 nm. The linear regression analysis data for the linearity plot showed good linear relationship with correlation coefficient value for Meclizine and Caffeine were R2=0.9990 and R2=0.9999 in the concentration range of 10-60µg mL-1 , 8-48 µg. mL-1 respectively. The relative standard deviation for intra-day precision was lower than 2%. The method was validated according to the ICH guidelines. The method was also found to be robust. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantitation and solution stability. The proposed method can be used for the e0.stimation of these drugs in combined dosage forms....
A fixed dose of Valacyclovir is used in tablet dosage form for the treatment and prevention of infectious diseases caused by Herpes Zoster. A simple, precise and accurate HPTLC method was developed and validated for the determination of Valacyclovir in Tablet dosage form. Separation was obtained using Pre-coated silica gel aluminum plate 60 F254 TLC plate with mobile phase Ethanol:Ethyl acetate:Ammonia (7.5:2.5:0.6) in which spot was devoid of tailing and sharp with good Rf value of 0.68±0.02 at 254 nm in remission/extinction mode with CD60 TLC scanner using ProQuant software. The method was validated for linearity, precision, accuracy, solution stability and specificity. The accuracy and reliability of the method was assessed by evaluation of linearity (500-3000 ng/band), precision (intra-day % RSD 0.87-1.19 and inter-day % RSD 0.90-1.34, accuracy (%Recovery) (98.89-101.98 %) and specificity, in accordance with ICH guidelines. Limit of detection and limit of quantification was found to be 23.29 ng/band and 70.59 ng/band....
A simple, precise, specific and accurate RP-HPLC method has been developed for the simultaneous determination of Ketotifen and cetirizine dihydrochloride in tablet dosage form. The chromatographic separation was achieved on C18 column using UV detector.The mobile phase consisting of ammonium acetate buffer: acetonitrile (pH 3.5) ratio (60:40) at a flow rate of 1.0 ml/min was used. The method was validated according to the ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness....
A fixed dose combination of Ceftazidime (CEF-β lactam antibiotic) and Tazobactam (TAZO-β Lactamase inhibitor) is used in ratio of 8:1 as powder form of injection for the treatment of resistant lower respiratory tract and other infections. An attempt was done to develop simple precise, accurate and validated stability indicating HPTLC method for the estimation of CEF and TAZO in bulk and injectable dosage form. The compounds were separated on aluminium-backed silica gel 60 F254 plates with n-propanol: Water: Triethylamine (7.5:2.0:0.5 v/v/v) as mobile phase. These systems were found to give sharp spots of CEF and TAZO with the Rf value of 0.37 and 0.67 respectively. Densitometric analysis of CEF and TAZO were done at 254 nm. Regression analysis for the calibration plots was indicative of good linearity between response and concentration over the range 1000-6000 ng/band for CEF and 2000-12000 ng/band for TAZO with the correlation coefficient (r2) 0.9993 and 0.9991 respectively. CEF and TAZO were subjected to acid, Alkali, oxidative, dry heat and photo degradation. It was susceptible to acidic, alkaline and oxidative hydrolysis conditions. Statistical analysis proved that method is repeatable, selective, and accurate for simultaneous estimation of CEF and TAZO. So the method effectively separated the drugs from their degradation products, it can be used as a stability-indicating assay method....
A fixed dose of Valacyclovir is used in tablet dosage form for the treatment and prevention of infectious diseases caused by Herpes Zoster. A simple, precise and accurate isocratic RP-HPLC method was developed and validated for the determination of Valacyclovir in tablet dosage form. As per ICH guideline Q1A (R2), drug was subjected different stress condition such as hydrolysis (acidic and alkaline), oxidation (3% H2O2 v/v), photolytic and thermal degradation. All stressed samples were successfully analyzed on an ACE C18 column (150×4.6mm id, 5µm particle size) using the mobile phase 10 mM potassium di-hydrogen phosphate buffer: Methanol (80:20 v/v, pH 6.5) at a flow rate of 1.0 mL/min. The retention time of Valacyclovir was found to be 3.879 min. The detection was performed using PDA detector or 252 nm. The method was validated for linearity, precision, accuracy, robustness, solution stability and specificity. The method was linear in the concentration range of 20-140 µg/mL for with a correlation coefficient of 0.999. The accuracy (%recovery) was found to be in the range of 98.89-101.98%. It was found that drug was more degraded in acid, alkali and oxidative condition, while no prominent degradation was found in thermal and photolytic condition....
A simple, specific, accurate, precise and reproducible zero crossing difference spectrophotometric method has been developed and validated for the simultaneous estimation of Aspirin (ASP) and Dipyridamole (DIP) in their combined dosage form. Measurements of absorbance were carried out at zero-crossing wavelengths 318.6 and 251.6 nm for aspirin and dipyridamole by zero-crossing difference spectrophotometric method. Beer’s law is obeyed in the concentration range of 1–17 μg/mL (r2=0.9996) for aspirin and 3–23 μg/mL (r2=0.9999) for dipyridamole by zero-crossing difference spectrophotometric method. The method was successfully applied to pharmaceutical dosage form because no interference from the tablet excipients was found. The suitability of this method for quantitative determination of Aspirin and Dipyridamole was proved by validation and recovery studies. The method was validated as per International Conference on Harmonization (ICH) guideline in terms of accuracy, precision, linearity, limits of detection, limits of quantitation. This method has been successively applied to capsule formulation and no interference from the sample mixture’s excipients was found....
A simple, specific, accurate, precise and reproducible Dual Wavelength method has been developed and validated for the simultaneous estimation of Aspirin (ASP) and Dipyridamole (DIP) in their combined dosage form. Measurements of absorbance were carried out at 285.80 and 299.00 nm for aspirin and 265.20 and 281.40 nm for dipyridamole by dual wavelength method. Beer’s law is obeyed in the concentration range of 1–17 μg/mL (r2=0.9998) for aspirin and 3–23 μg/mL (r2=0.9999) for dipyridamole. The method was successfully applied to pharmaceutical dosage form because no interference from the tablet excipients was found. The suitability of this method for quantitative determination of Aspirin and Dipyridamole was proved by validation and recovery studies. The method was validated as per International Conference on Harmonization (ICH) guideline in terms of accuracy, precision, linearity, limits of detection, limits of quantitation. This method has been successively applied to capsule formulation and no interference from the sample mixture’s excipients was found....
A simple, specific, accurate, precise and reproducible Ratio spectra derivative spectrophotometric method has been developed and validated for the simultaneous estimation of Tramadol hydrochloride (TRM) and Aceclofenac (ACE) in their combined dosage form. The ratio derivative spectroscopic method involves measurement of first derivative amplitude of ratio spectra at 281.80 nm for TRM and 285.40 nm for ACE as two wavelengths for estimation. Beer's law is obeyed in the concentration range of 5-65 and 4-36 μg/mL for TRM and ACE, respectively. LOD values for TRM and ACE are found to be 0.467 μg/mL and 0.45 μg/mL, respectively. LOQ values for TRM and ACE are found to be 1.417 μg/mL and 1.373 μg/mL respectively. The results of analysis have been validated statistically and recovery studies carried out in the range 80-120% to confirm the accuracy of the proposed method. The method was validated as per International Conference on Harmonization (ICH) guideline in terms of accuracy, precision, linearity, limits of detection, limits of quantitation. This method has been successively applied to tablet formulation and no interference from the sample mixture’s excipients was found....
Simple, economic, sensitive and reproducible and rapid spectrophotometric and chromatographic methods have been developed and validated for the determination of Telmisartan (TR) and Paliperidone (PP) in tablets and as bulk drug. The methods applied were involing use Ferric Chloride (FeCl3). The method employs Ferric chloride reagent in presence of hydrochloric acid and Potassium ferricyanide to form greenish complex with λ max at 610 nm and 580 nm for Telmisartan (TR) and Paliperidone (PP) respectively. The concentration of Telmisartan (TR) and Paliperidone (PP) over a range of 10-60 μg/ml was found sufficient for obeying Beer’s law in the stated range. The results of the analysis have been validated statistically and by recovery studies....
The present manuscript describe simple, sensitive, rapid, accurate, precise and cost effective Area under curve spectrophotometric method for the simultaneous determination of Amitryptiline HCl and Chlordiazepoxide in combined tablet dosage form. It involved measurement of area under curve in the wavelength range 231-245 nm and 235-256 nm for AMI and CHLOR respectively. Beer’s law obeyed in concentration range of 3-10 µg/ml for both the drugs. The proposed methods are recommended for routine analysis since they are rapid, simple, accurateand also sensitive and specific. It involves no heating and no organic solvent extraction. These methods were validated for precision, reproducibility, linearity and accuracy as per ICH guidelines....
As herbal medicines have an important position in health care systems worldwide, their current assessment and quality control are a major bottleneck. Recent improvements in advanced analytical instrumentation with improved sensitivity and precision to allow greater resolution of multi-component mixtures are driving the quality-control standards of HMs towards universally acceptable standards. Many cutting-edge analytical technologies have been introduced to evaluate the quality of medicinal plants and significant amount of measurement data has been produced. Then, the application of chemometrics in the field of medicinal plants is spontaneous and necessary. Comprehensive methods and hyphenated techniques associated with chemometrics used for extracting useful information and supplying various methods of data processing are now more and more widely used in medicinal plants among which chemometrics resolution methods and PCA are most commonly used techniques. This review focuses on the various important recent analytical techniques, important chemometrics tools and interpretation of results by PCA and at last applications of chemometrics in quality evaluation of medicinal plants in the authenticity, efficacy and consistency....
Two simple chemometric assisted UV-Spectrophotometric methods; classical least square (CLS) and inverse least square (ILS) were developed for simultaneous assay of Cinitapride Hydrogen Tartrate (CNT) and Rabeprazole Sodium (RAB) in their pharmaceutical dosage form without any chemical separation and any graphical treatment of the overlapping spectra of two drugs. The UV absorption spectra of the drugs studied, in the range of 250-290 nm, showed a considerable degree of spectral overlapping. Beer’s law was obeyed for both drugs in the concentration ranges of 4-20 and 4-20 µg/ml for CNT and RAB, respectively. Fourteen mixed solutions were prepared for the chemometric calibration as training set and eight mixed solutions were prepared as validation set. The absorbance data matrix was obtained by measuring the absorbance at twenty one wavelength points, from 250 to 290 nm with the interval of 2 nm (Δ=2 nm). The developed calibrations were successfully tested for pharmaceutical formulation....
Two simple Chemometric assisted UV-Spectrophotometric methods; Classical Least Square (CLS) and Inverse Least Square (ILS) were developed for simultaneous estimation of Paracetamol (PCM) and Flupirtine maleate (FLU) in combined dosage form without any chemical separation and any graphical treatment of the overlapping spectra of two drugs. The UV absorption spectra of the drugs studied, in the range of 250–320 nm, showed a considerable degree of spectral overlapping. Beer’s law was obeyed for both drugs in the concentration ranges of 2–25 µg/mL. Fourteen mixed solutions were prepared for the chemometric calibration as training set and seven mixed solutions were prepared as validation set. The absorbance data matrix was obtained by measuring the absorbance at thirty six wavelength points, from 250 to 320 nm with the interval of 2 nm (Δ=2 nm). The developed calibrations were successfully tested for pharmaceutical formulation....
Cleaning validation is a documented process that proves the effectiveness and consistency in cleaning pharmaceutical production equipment. This is necessary to assure the quality of future products using the equipment, to prevent cross-contamination, and as a World Health Organization, Good Manufacturing Practices requirement. We have applied the Total Organic Carbon (TOC) analysis method to a number of pharmaceutical products. In this article we discuss the TOC method that we developed for measuring residual ranitidine on surface of mixing vessel during manufacturing process. The method with correlation coefficient R²=0.999 and method offers low detection capability (0.89 parts per million) and rapid sample analysis time. The accurate recovery values ranged from 99.66±1.07 with method precision less than 2%RSD**. We found that the TOC method is applicable for determining residual ranitidine on pharmaceutical surfaces and will be useful for cleaning validation....
A simple, sensitive, rapid, accurate and precise spectrophotometric method was developed for simultaneous estimation of citicoline and methylcobalamin in tablet by employing absorption correction method and validated for accuracy, precision, linearity, LOD, LOQ. The wavelengths selected for quantitation were 271.0 nm for citicoline and 351.0 nm for methylcobalamin. Linearity was maintained within a wide concentration range from 5.0-25.0 μg/ml for citicoline and 10-50 μg/ml for methylcobalamin. The limit of detection and limit of quantification for citicoline were found to be 0.2335 and 0.7076 μg/ml respectively and for methylcobalamin 0.4819 and 1.4604 μg/ ml respectively. The method gives results of high accuracy confirmed by recovery studies. The mean % labeled claim for citicoline and methylcobalamin were 100.34±0.82% and 99.78±1.21% respectively. % R.S.D. values for precision studies were less than 2% indicates method is precise....
A selective stability-indicating RP-HPLC method has been developed and validated for analysis of Domperidone in bulk drug. Reversed phase chromatography was performed on a C18 column with Methanol: Ammonium acetate buffer, 60:40 (%, v/v), as mobile phase at a flow rate of 1.4 ml/min. Detection was performed at 287 nm and a sharp peak was obtained for Domperidone at a retention time of 7.83 ±0.01 min. The results of analysis have been validated as per ICH guidelines. It showed a linear response in the concentration range of 20-120 µg/ml; the regression coefficient was 0.998 and the linear regression equation was y = 20166x + 15030. The detection and quantification limits were 2.79 and 8.54 µg ml-1 respectively. The average percentage recovery for Domperidone was found to be 100.05%. It was subjected to acidic, alkaline, neutral, oxidative hydrolysis and dry heat condition. The result of degradation studies indicated that it was highly susceptible to the oxidative degradation and moderately susceptible to acidic, alkaline and neutral hydrolysis. The degradation products of Domperidone were well resolved from the pure drug with significant differences in their retention time values. This method can be successfully employed for routine analysis of Domperidone in bulk drug in stability samples....
A simple, precise, accurate, economic and reproducible spectrophotometric method has been developed for simultaneous estimation of Montelukast Sodium (MONTE) and Olopatadine Hydrochloride (OLO) by employing Absorption correction UV spectrophotometric method in 0.1 N NaOH. Wavelength Selected for detection of Montelukast Sodium 346.22 nm and for Olopatadine Hydrochloride 295.18 nm. The linearity was established over the concentration range of 20-40 µg/ml and 10-20 µg/ml for Montelukast Sodium and Olopatadine Hydrochloride with correlation coefficient 0.999 and 0.999, respectively. The mean % recoveries were found to be in the range of 99.76–100.20% and 99.65–100.10% for Montelukast Sodium and Olopatadine Hydrochloride respectively. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of Montelukast Sodium and Olopatadine Hydrochloride in their Synthetic mixture....
The present manuscript describe simple, sensitive, rapid, accurate, precise and economical Q-absorbance ratio method for the simultaneous estimation of Dithranol and Salicylic Acid in combined dosage form. Absorbance ratio method uses the ratio of absorbances at two selected wavelengths, one which is an iso-absorptive point at 278 nm in methanol. The second wavelength used is 258 nm, which is the ʎ-max of Dithranol in methanol. The linearity was observed in the concentration range of 1-5 µg/ml for both Dithranol and Salicylic Acid. The method was successfully applied to pharmacopoeial dosage form because no interference from the excipients was found. The results of analysis have been validated statistically and by recovery studies....
A simple, precise, accurate, economic and reproducible UV spectrophotometric method has been developed for simultaneous estimation of Montelukast Sodium (MONTE) and Olopatadine Hydrochloride (OLO) by employing first order derivative zero crossing method in 0.1 N NaOH. The wavelength 295.18 nm (zero cross point of Olopatadine Hydrochloride) was selected for quantification of Montelukast Sodium and wavelength 303.65 nm (zero cross point of Montelukast Sodium) was selected for quantification of Olopatadine Hydrochloride The linearity was established over the concentration range of 20-40 µg/ml and 10-20 µg/ml for Montelukast Sodium and Olopatadine Hydrochloride with correlation coefficient r2 0.998 of both the drugs. The mean % recoveries were found to be in the range of 99.82 %–100.52 % and 100.42%–101.21% for Montelukast Sodium and Olopatadine Hydrochloride, respectively. The proposed method has been validated as per ICH guideline and successfully applied to the estimation of Montelukast Sodium and Olopatadine Hydrochloride in synthetic mixture....
Four simple chemometric assisted UV-Spectrophotometric methods, classical least square (CLS), inverse least square (ILS), principal component regression (PCR) and partial least squares (PLS) were developed for simultaneous estimation of Cefixime Trihydrate (CEF) and Linezolid (LINE) in their combined dosage tablet formulation without any chemical separation and any graphical treatment of the overlapping spectra of two drugs. The UV absorption spectra of the studied drugs, in the range of 235–295 nm, showed a considerable degree of spectral overlapping. Beer’s law was obeyed for both drugs in the general concentration ranges of 2–6 µg/ml and 6–18 µg/ml for CEF and LINE, respectively. Eighteen mixed solutions were prepared for the chemometric calibration as training set and eight mixed solutions were prepared as validation set. The absorbance data matrix was obtained by measuring the absorbance at twenty one wavelength points, from 235 to 295 nm with the interval of 3 nm (Δ=3 nm). The developed calibrations were successfully tested for laboratory mixtures as well as commercial tablet formulation for their CEF and LINE concentration....
Four simple chemometric assisted UV-spectrophotometric methods, classical least square (CLS), inverse least square (ILS), principal component regression (PCR) and partial least squares (PLS) were developed for simultaneous estimation of Lornoxicam (LOR) and Tolperisone Hydrochloride (TPH) in their combined dosage tablet formulation without any chemical separation and any graphical treatment of the overlapping spectra of two drugs. The UV absorption spectra of the studied drugs, in the range of 230–278 nm, showed a considerable degree of spectral overlapping. Beer’s law was obeyed for both drugs in the general concentration ranges of 4–14 µg/ml. Eighteen mixed solutions were prepared for the chemometric calibration as training set and eight mixed solutions were prepared as validation set. The absorbance data matrix was obtained by measuring the absorbance at seventeen wavelength points, from 230 to 278 nm with the interval of 3 nm (Δ = 3 nm). The developed calibrations were successfully tested for laboratory mixtures as well as commercial tablet formulation for their LOR and TPH concentration....
The objective of this study was to develop simple, precise, accurate and sensitive UV spectrophotometric methods for the simultaneous determination of ofloxacin (OFX) and flavoxate HCl (FLX) in pharmaceutical formulations. In the method difference spectrophotometric at 239.6 nm for OFX (zero crossing for FLV) and at 332.4 nm for FLV (zero crossing for OFX) was used for the determination of the drugs and the linearity range was found to be 5 to 25 μg/ml for both OFX and FLV. The accuracy and precision of the methods were determined and validated statistically. This method showed good reproducibility and recovery with % RSD less than 1.5%. This method was found to be rapid, specific, precise and accurate and can be successfully applied for the routine analysis of OFX and FLV in combined dosage form....
The present manuscript describe simple, sensitive, rapid, accurate, precise and cost effective dual wavelength spectrophotometric method for the simultaneous determination of Domperidone and Cinnarizine in combined dosage form. The method was based on determination of Cinnarizine at 301.2 nm (λ1) and 248.2 nm (λ2) and Domperidone at 239 nm (λ3) and 258.2 nm (λ4). The difference in absorbance at λ1 and λ2 (A248.2–A301.2) cancels out the contribution of absorbance of Domperidone in measurement of Cinnarizine and the difference in the absorbance was proportional to the concentration of Cinnarizine in the combined mixture. While the difference in absorbance at λ4 and λ3 (A239–A258.2) cancels out the contribution of absorbance of Cinnarizine in measurement of Domperidone and the difference in the absorbance was proportional to the concentration of Domperidone in the combined mixture. The linearity was obtained in the concentration range of 10-40 μg/ml for Domperidone and 3-18 μg/ml for Cinnarizine. LOD and LOQ values were found to be 0.22 μg/ml and 0.11 μg/ml; 0.66 μg/ml and 0.35 μg/ml for Domperidone and Cinnarizine, respectively. Percent label claim of the compounds were 99.11±0.989 and 100.55±0.987 for Domperidone and Cinnarizine, respectively. Recovery data were found to be 99.86±0.65 for Domperidone and 99.45±0.50 for Cinnarizine. The method was successfully applied to pharmaceutical dosage form because no interference from excipients were found. The suitability of these methods for the quantitative determination of Domperidone and Cinnarizine was proved by validation. The proposed methods were found to be simple and sensitive for the routine quality control application of Domperidone and Cinnarizine in pharmaceutical dosage form. The results of analysis have been validated statistically and by recovery studies....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical dual wavelength UV Spectrophotometric method for the simultaneous determination of Lafutidine and Rabeprazole Sodium in combined dosage form. The principle for dual wavelength method is “The absorbance difference between two points on the mixture spectra is directly proportional to the concentration of the component of interest”. The wavelengths selected for determination of Lafutidine were 281 nm and 287.8 nm, whereas, the wavelengths selected for determination of Rabeprazole Sodium were 269.2 nm and 276.4 nm. Methanol was taken as a solvent. Regression analysis of Beer’s plots showed good correlation in concentration range of 10-45 μg/ml for Lafutidine and 6-22 μg/ml for Rabeprazole Sodium. The mean recovery was found to be 100.35% and 99.33% for Lafutidine and Rabeprazole Sodium, respectively. The precision (intra‐day, inter‐day and repeatability) of method was found to be within the limits as per ICH Guideline Q2(R1). The Proposed method was successfully applied for the simultaneous estimation of both the drugs in commercial Pharmaceutical dosage form....
A simple, efficient, accurate, precise and economical first order derivative spectrophotometric method was developed for the simultaneous determination of Xylometazoline hydrochloride and Ipratropium bromide in pharmaceutical dosage form. The derivative spectrophotometric method was based on the determination of both the drugs at their respective zero crossing point (ZCP). The first order derivative spectra were obtained in distilled water and the determinations were made at 264.41 nm (ZCP of Xylometazoline hydrochloride) for Ipratropium bromide and 261.58 nm (ZCP of Ipratropium bromide) for Xylometazoline hydrochloride. The linearity was obtained in concentration range 250-875 µg/ml for Xylometazoline hydrochloride and 300-1050 µg/ml for Ipratropium bromide. The accuracy of the method was determined by recovery studies and was found to be in the range of 99.73-100.35% and 99.87-100.26% for Xylometazoline hydrochloride and Ipratropium bromide, respectively. The method was validated as per ICH guidelines and statically. The method showed good recovery with % RSD less than 2. The method was found to be simple, economic, accurate and precise and can be used routine analysis of Xylometazoline hydrochloride and Ipratropium bromide in pharmaceutical dosage form. The results of analysis have been validated statistically and by recovery studies....
Losartan Potassium and Atenolol are used in combination for treatment of blood pressure. The present work deals with simple spectrophotometric method development for simultaneous estimation of Losartan Potassium (LOS K) and Atenolol (ATE) in two component tablet formulation. The method employed is a first order derivative spectroscopy. For determination of sampling wavelength, 10 μg/ml of each of LOS K and ATE were scanned in 200-400 nm range and sampling wavelengths were 222.4 nm for LOS K where ATE showed zero crossing point and 274 nm for ATE where LOS K showed zero crossing point in first order derivative spectroscopy. For this method linearity observed in the range of 10-30 μg/ml for both ATE and LOS K. The recovery studies confirmed accuracy of proposed method and low values of standard deviation confirmed precision of method. The method is validated as per ICH guidelines....
A simple, precise, accurate and reproducible spectrophotometric method has been developed for simultaneous estimation of Amitriptyline HCl (AMI) and Chlordiazepoxide (CHLOR) by employing first order derivative zero crossing method in 0.1 N HCl. The first order derivative absorption at 239 nm (zero cross point of Amitryptiline HCl) was used for quantification of Chlordiazepoxide and 246 nm (zero cross point of Chlordiazepoxide) for quantification of Amitriptyline HCl. The linearity was established over the concentration range of 5-10 µg/ml and 6-16 µg/ml for Chlordiazepoxide and Amitriptyline HCl with correlation coefficient r2 0.9900 and 0.9983, respectively. The mean % recoveries were found to be in the range of 99.63%–100.27% and 98.89%–100.72% for Chlordiazepoxide and Amitriptyline HCl, respectively. The proposed method has been validated as per ICH guideline and successfully applied to the estimation of pharmaceutical dosage form....
A simple, rapid, accurate and precise first order derivative spectrophotometric method has been developed for simultaneous estimation of Cefpodoxime proxetil and Azithromycin Dihydrate in their combined pharmaceutical dosage form. This method utilizes methanol as a solvent. Zero crossing point (ZCP) of Cefpodoxime Proxetil and Azithromycin Dihydrate were found to be 234 nm and 283 nm respectively. Hence, estimation of Cefpodoxime Proxetil and Azithromycin Dihydrate were done at 283 nm and 234 nm respectively. Linearity was observed in the concentration range of 5-25 μg/ml for Cefpodoxime Proxetil (r2=0.9955) and 20-100 μg/ml for Azithromycin Dihydrate (r2=0.9968). The results of analysis have been validated statistically and by recovery studies. Developed method was applied to pharmaceutical dosage form. The results were found to be within acceptance criteria according to ICH guideline....
A new simple, sensitive high performance Liquid chromatographic (HPLC) method has been developed for the quantitative estimation of Levosulpride (LEVO) and Pantoprazole Sodium (PANTO) in combined dosage form using Hyperchrom ODS-BP C18250 x 4.6 mm i.d., (5 mm) was used as Stationary Phase. Acetonitrile: 0.05 M Potassium Dihydrogen Ortho Phosphate (50:50 v/v) (pH 3.0 adjusted by O-phosphoric acid) as mobile phase. LEVO and PANTO showed Rt value 3.344+0.005 and 4.753+ 0.006 and scanned at 288 nm. The method was validated in terms of linearity 38–114 μg/ml for LEVO and 20–60 μg/ml for LEVO. The limit of detection for LEVO and PANTO were found to be 1.0178 μg/ml and 0.5481 μg/ml, respectively and limit of quantification for LEVO and PANTO were found to be 3.0818 μg/ml and 1.660 μg/ml, respectively. The mean recovery was 98.32–101.00% and 98.50–101.85 % for LEVO and PANTO respectively. The method was found to be simple, sensitive, specific, accurate and precise and can be used for the routine quality control testing of Levosulpride and Pantoprazole Sodium dosage form....
A simple, specific, accurate and precise RP-HPLC method has been developed and validated for the Simultaneous Estimation of Paracetamol and Tapentadol hydrochloride in their combined dosage form (tablet). The separation of the two components were carried out using C18 (250 mm × 4.6 mm id, 5 µm particle size) column by isocratic elution with a flow rate of 1 ml/min. The mobile phase composition was water: methanol: triethylamine (60:40:0.1) of pH 3.5 adjusted with orthophosphoric acid and detection was carried out at 225 nm. The retention time for Paracetamol was 3.92 min and 5.30 min for Tapentadol hydrochloride. The method has been validated in terms of linearity, specificity, accuracy, precision, limit of detection, limit of quantitation, robustness as per ICH guidelines. The method has been found to be linear in the range of 32.5-97.5 µg/ml (R2=0.9982) for Paracetamol and 5-15 µg/ml (R2=0.9977) for Tapentadol hydrochloride. The limit of detection and limit of quantitation were 0.0304 and 0.0922 for Paracetamol and 0.0086 and 0.0262 for Tapentadol hydrochloride. The recoveries of Paracetamol and Tapentadol hydrochloride were 99.97% and 99.81% respectively and their relative standard deviations were less than 2%. Hence, the method could be successfully applied for routine analysis of Paracetamol and Tapentadol hydrochloride in combined tablet dosage form....
Ceftazidime pentahydrate (CEF-β lactam antibiotic) is used for the treatment of resistant lower respiratory tract and other infections. An attempt was done to develop simple precise, accurate and validated HPTLC method for the estimation of CEF in bulk and injectable dosage form. The compounds were separated on aluminium-backed silica gel 60 F254 plates with Methanol: Toluene: Water: TEA (7.5:2:0.5:0.2 v/v/v/v) as mobile phase. These systems were found to give sharp spots of CEF with the Rf value of 0.44. Densitometric analysis of CEF was done at 254 nm. Regression analysis for the calibration plot was indicative of good linearity between response and concentration over the range 1250-7500 ng/band with the correlation coefficient (r2) 0.9972. The mean recoveries obtained for CEF was found to be 99.27%-100.15%. Statistical analysis proved that method is repeatable, selective, and accurate for estimation of CEF....
This paper describes a validated high-performance thin-layer chromatography (HPTLC) method for simultaneous estimation of Diclofenac Potassium (DKP) and Febuxostat (FEB) in tablet dosage form. An HPTLC method separation is achieved on an aluminum sheet of silica gel 60F254 using Chloroform: Methanol: Formic acid (14:0.4:0.2 v/v/v) as mobile phase. Quantification is achieved with UV detection at 293 nm over a concentration range of 100-500 ng/spot and 40-200 ng/spot with mean recovery of 99.16 ± 0.63 and 99.52 ± 0.71 for DKP and FEB, respectively, in the HPTLC method. Results showed that this method was simple, precise, and sensitive and it is applicable for the simultaneous determination of DKP and FEB in tablet dosage form....
High performance thin layer chromatography (HPTLC) method has been developed and validated for simultaneous estimation of Diclofenac Potassium and Serratiopeptidase. The separation was achieved on precoated silica gel 60 F254 aluminum plate as stationary phase and n-Hexane: Toluene: Methanol (6.0: 2.5:1.5 v/v/v) as mobile phase. The densitometric scanning was carried out at 260 nm. The Rf values were found to be 0.2183±0.0040 and 0.5966±0.0051 for Diclofenac Potassium and Serratiopeptidase respectively. Beer’s law obeyed in concentration range of 100-500 ng/spot and 40-200 ng/spot in methanol for Diclofenac Potassium and Serratiopeptidase respectively. The method was validated for specificity, linearity, accuracy, precision, LOD and LOQ. The percent assay of marketed formulation was 100.35±0.5379 and 99.93±0.7637% (2061.90 units/mg) of Diclofenac Potassium and Serratiopeptidase respectively. The proposed methods are simple, accurate and precise since they are recommended for routine analysis....
To develop simple and economical UV spectrophotometric method for the simultaneous estimation of Olopatadine HCl and Ketorolac tromethamine in the combined ophthalmic dosage form available in the market for the prophylaxis of conjunctivitis. Two drugs Olopatadine HCl and Ketorolac tromethamine are present in the ratio of 1:4. The normal overlay spectra of two drugs in distilled water revealed an isoabsorptive point at 263 nm. The other wavelength selected was λmax of Olopatidine HCl (249 nm). The method was validated as per the ICH guidelines. Beer’s law followed in the range of 8-45 µg/ml for both Olopatadine HCl and Ketorolac tromethamine. Recovery studies by standard addition method were in the range of 97% to 101%. The relative standard deviation for intraday and interday precision was found to be less than 2% indicating the method to be repeatable. A simple, accurate, sensitive and economical UV-Spectrophotometric method for the simultaneous estimation of Olopatadine HCl and Ketorolac tromethamine in combined dosage form has been developed which can be employed in the industry for the routine analysis....
Simple, accurate, precise, and sensitive ratio spectra derivative spectrophotometric method for simultaneous estimation of Pantoprazole (PANTO) and Levosulpiride (LEVO) in Pharmaceutical dosage form have been developed and validated. The ratio derivative spectroscopic method involves measurement of first derivative amplitude of ratio spectra at 276.8 nm for PANTO and 241.4 nm for LEVO as two wavelengths for estimation. Beer's law is obeyed in the concentration range of 2-10 μg/ml for both PANTO and LEVO. LOD and LOQ values for PANTO were found to be 0.34 and 1.02 μg/ml and at 276.8 nm, respectively. LOD and LOQ values for LEVO were found to be 0.60 and 1.81 μg/ml and at 241.4 nm, respectively. The method was validated statistically and recovery studies were carried out. It was found to be accurate, precise and reproducible. The method was applied to the assay of the drugs in Tablet dosage form, which were found in the range of 99.72±0.31 for Pantoprazole and 99.94±0.18 for Levosulpiride of the labeled value for both Pantoprazole and Levosulpiride. Hence, the method herein described can be successfully applied in quality control of synthetic mixture....
A simple, precise, accurate, economic and reproducible spectrophotometric method has been developed for simultaneous estimation of Montelukast Sodium (MONTE) and Olopatadine Hydrochloride (OLO) by employing Ratio first derivative UV spectrophotometric method in 0.1 N NaOH. The Ratio Spectra of Montelukast Sodium were obtained by divisor of Olopatadine Hydrochloride (20 µg/ml) and Ratio Spectra of Olopatadine Hydrochloride were obtained by divisor of Montelukast Sodium (40 µg/ml) and resulting ratio spectra was converted to first order derivative spectra. Wavelength Selected for detection of Montelukast Sodium 268.40 nm and for Olopatadine Hydrochloride 289.80 nm. The linearity was established over the concentration range of 20-40 µg/ml and 10-20 µg/ml for Montelukast Sodium and Olopatadine Hydrochloride with correlation coefficient 0.999 and 0.998, respectively. The mean % recoveries were found to be in the range of 99.77–100.31% and 98.33–100.07% for Montelukast Sodium and Olopatadine Hydrochloride respectively. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of Montelukast Sodium and Olopatadine Hydrochloride in their Synthetic mixture....
Ratio Spectra First order Derivative Method has been developed for simultaneous estimation of Diclofenac Potassium and Serratiopeptidase. The method involved analytical signals were measured at maxima 266.80 nm and minima 257.0 nm for Diclofenac Potassium and Serratiopeptidase in the first order derivative spectra (∆ λ=8 nm and Scaling factor = 1) of the ratio spectra obtained by using 10 µg/ml SER and 10 µg/ml DP spectra as divisor for Diclofenac Potassium and Serratiopeptidase respectively. Beer’s law obeyed in concentration range of 2-18 µg/ml in methanol for both the drugs. The percent assay of marketed formulation was 99.93±1.0151 and 100.46±0.7790% (2072.84 units/mg) of Diclofenac Potassium and Serratiopeptidase respectively. The proposed methods are specific, sensitive, accurate and precise since they are recommended for routine analysis....
Ratio Spectra First Order Derivative Method has been developed for simultaneous estimation of Diclofenac Sodium and Tolperisone Hydrochloride. The analytical signals were measured at maxima 244.0 nm and minima 232.80 nm for Diclofenac Sodium and Tolperisone Hydrochloride respectively in the first order derivative spectra (∆ λ = 8 nm and Scaling factor = 1) of the ratio spectra. The ratio spectra obtained by dividing the mixture spectra using 16 µg/ml TOL and 17 µg/ml DFS spectra as divisor for Diclofenac Sodium and Tolperisone Hydrochloride respectively. Beer’s law obeyed in concentration range of 3-31 µg/ml and 4-28 µg/ml in distilled water for Diclofenac Sodium and Tolperisone Hydrochloride respectively. The percent assay of marketed formulation was 99.58±1.148 % and 99.86±1.369 % of Diclofenac Sodium and Tolperisone Hydrochloride respectively. The proposed methods are specific, selective, sensitive, accurate and precise since they are recommended for routine analysis....
Ratio Spectra First order Derivative Method has been developed for simultaneous estimation of Levosulpiride and Pantoprazole. The methanol and water was use as solvents. The method involved analytical signals were measured at maxima 258.2 nm and minima 251.1 nm for Levosulpiride and Pantoprazole in the first order derivative spectra (∆ λ = 8 nm and Scaling factor = 1) of the ratio spectra obtained by using 18 µg/ml PANTO and 75 µg/ml LEVO spectra as divisor for Levosulpiride and Pantoprazole respectively. Beer’s law obeyed in concentration range of 6-30 µg/ml for PANTO and 25-125 µg/ml for LEVO. The percent assay of marketed formulation was 99.79±1.1334 and 99.82±1.0182 of Levosulpiride and Pantoprazole respectively. The proposed methods are specific, accurate and precise so they are recommended for routine analysis....
A simple, fast, accurate and precise method has been developed for determination of eperisone hydrochloride from pharmaceutical formulation by Reversed-phase high performance liquid chromatography. The separation was carried out on C18 column using mobile phase consisting of a mixture of acetonitrile and water in the ratio 90:10 v/v (pH adjusted to 3.5 with orthophosphoric acid). The flow rate was maintained at 0.9 ml/min. The UV detection was carried out at wavelength 276 nm. The retention time for eperisone hydrochloride was found to be 3.79 min. Linear response obtained for eperisone hydrochloride in the concentration range 3-15 µg/ml (r2 =0.996). The relative standard deviation was found less than 2% for six replicates. The method was validated according to the ICH guidelines with respect to linearity, precision, accuracy, limit of detection, limit of quantification and robustness. Thus, proposed method can be successfully applicable to the pharmaceutical preparation containing the above mentioned drugs without any interference of excipients....
Isocratic, reversed phase liquid chromatographic assay method was developed for the quantitative determination of ibuprofen and phenylephrine hydrochloride in combined pharmaceutical dosage form. A Sunfire C18, 5 m column with mobile phase containing acetonitrile: methanol: phosphate buffer (50:20:30, v/v/v) (pH 6) adjusted with 0.01% O- phosphoric acid was used. The flow rate was 1.0 mL/min and effluents were monitored at 220 nm. The retention times of ibuprofen and phenylephrine hydrochloride were 13.6 min and 2.7 min, respectively. The linearity for ibuprofen and phenylephrine hydrochloride was in the range of 25-125 µg/ ml and 1.25–6.25 µg/ml, respectively. The proposed method was validated with respect to linearity, accuracy, precision, specificity and robustness. The method was successfully applied to the estimation of ibuprofen and phenylephrine hydrochloride in combined pharmaceutical dosage form....
This paper presents a RP-HPLC method for the simultaneous estimation of Cefixime and Levofloxacin in combined tablet dosage form. The process was carried out on C18 column (Luna 5 μm, 250 × 4.60 mm, i.d) using phosphate buffer pH 5.0 and Acetonitrile in the ratio of 70:30 v/v respectively as a mobile phase at a flow rate of 1.0 mL/min. Detection wavelength was fixed at isobestic point 283 nm. Linearity was observed in the concentration range of 20-100 μg/ml for Cefixime (r2 =0.9977) and 25-125 μg/ml for Levofloxacin (r2=0.9968). The retention time of Cefixime and Levofloxacin was found to be 2.898 and 6.091 minutes, respectively. The developed method is simple, precise, specific, robust, rapid, reproducible, and sensitive and it can be used for estimation of Cefixime and Levofloxacin in combined tablet dosage form....
A simple, sensitive, precise, accurate and rapid RP-HPLC method has been developed and validated for the simultaneous determination of Diclofenac sodium and Chlorzoxazone in combine dosage form. The RP-HPLC method was performed on sunshell C18 column (100 mm × 4.6 mm i.d., 2.5 μm particle sizes). Mobile phase consisted of a mixture of phosphate buffer (0.05 M KH2PO4, pH adjusted to 3.2 using Orthophosphoric acid): Acetonitrile : TEA (55: 45: 1 v/v/v) at a flow rate of 1.5 ml/min. The detection wavelength was at 240 nm. The proposed method was validated for linearity, accuracy, precision, LOD and LOQ. Retention time of Diclofenac sodium and Chlorzoxazone was 4.94±0.07 & 1.28±0.03, respectively with linearity range of 20-60 µg/mL and 100-300 µg/mL for Diclofenac sodium and Chlorzoxazone respectively. The mean recoveries were 100.19±0.518728 and 99.55±0.536201 for Diclofenac sodium and Chlorzoxazone, respectively. The LOD value were found to be 0.3428 and 4.3289 µg/mL, while LOQ value were found to be 1.0387 and 13.1187 µg /mL for Diclofenac sodium and Chlorzoxazone respectively. This method can now transfer to utilize for routine laboratory analysis and assay of Diclofenac sodium and Chlorzoxazone in their tablet dosage form....
A Reversed Phase–High Performance Liquid Chromatographic (RP-HPLC) method has been developed for simultaneous estimation of Fluocinolone acetonide and Miconazole nitrate in bulk drug and in pharmaceutical formulation using methanol as a solvent. The compounds were well separated on a Thermo Scientific C 18 Column (150 mm*4.6 mm, 5 µm) using mobile phase consisting of Methanol: Water (65:35 v/v) at a flow rate of 1.0 mL min-1 with detection wavelength at 232 nm. The linearity ranges were 0.5-4.5 µg/mL for Fluocinolone acetonide and 200-900 µg/mL for Miconazole nitrate. The recovery amount was more than 99 %. The high recovery and low relative standard deviation confirms the suitability of the method for determination of Fluocinolone acetonide and Miconazole nitrate in ointment dosage form. The results of analysis of all methods have been validated statistically. The developed method is simple, rapid, precise and accurate, hence can be used for routine estimation of these drugs in formulations. The results were found to be within acceptance criteria according to ICH Q2 R1 guideline....
This work is concerned with application of simple, precise, accurate and reproducible reverse phase high performance liquid chromatographic (RP-HPLC) method for simultaneous estimation of Hydralazine Hydrochloride (HLZ) and Propranolol (PRO) on RP Phenomenex C18 column (250 mm x 4.6 mm i.d., 5 μm particle size) using Acetonitrile +0.25 ml Triethylamine - Water (35:65%) pH adjusted to 3.5 with O- phosphoric acid as mobile phase at a flow rate of 1.0 ml/min and the detection wavelength was 273 nm. The retention time for HLZ and PRO was found to be 5.297 and 3.183 min, respectively. Proposed method was validated for precision, accuracy, linearity range, robustness....
A simple, precise, specific and accurate RP-HPLC method has been developed for the simultaneous determination of Ketotifen and Salbutamol in tablet dosage form. The chromatographic separation was achieved on C18 column using UV detector. The mobile phase consisting of ammonium acetate buffer: acetonitrile (pH 3.5) ratio (60:40) at a flow rate of 1.0 ml/min was used. The rang for ketotifen and salbutamol respectively 2.5-7.5 and 5-15. The detection of both drug at 245nm. The method was validated according to the ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness....
A novel, precise, accurate and rapid isocratic reversed-phase high performance liquid chromatographic/ultraviolet (RP-HPLC/UV) method was developed, optimized and validated for simultaneous determination of Tramadol HCl and Aceclofenac. The method showed adequate separation for Tramadol HCl and Aceclofenac and best resolution was achieved with Phemnomenex C18 column (250 mm x 4.6 mm i.d., 5 µm particle size) using Water: Acetonitrile: Triethylamine [50:50:0.5, v/v/v] pH adjusted to 6 with o-phosphoric acid as a mobile phase at a flow rate of 1 ml/min and wavelength of 271 nm. The calibration curves were linear over the concentration ranges of 3.75-22.5 μg/ml and 10-60 for Tramadol HCl and Aceclofenac respectively. The limit of detection (LOD) and limit of quantification (LOQ) for Tramadol HCl were 0.240 and 0.729 μg/ml while for Aceclofenac were 0.661 and 2.004 μg/ml, respectively. All the analytes were separated in less than 7.0 min. The proposed method could be applied for routine laboratory analysis of Tramadol HCl and Aceclofenac in pharmaceutical dosage form. Methods were validated statistically and recovery studies were carried out. The proposed methods have been applied successfully to the analysis of cited drug either in pure form or in synthetic mixture of both drugs with good accuracy and precision. The method herein described can be employed for quality control and routine analysis of drugs in pharmaceutical formulations....
A new, accurate, precise, and rapid RP-HPLC method has been developed and validated for the simultaneous estimation of diacerein and celecoxib in capsule dosage. The separation was achieved by using C18 column (Thermo scientific, 250×4.6 mm, 5 μm Particle Size) and the mobile phase consisting of 0.02 M potassium dihydrogen phosphate (containing 0.1% triethylamine and pH adjusted to 3.50±0.05 using 20% orthophosphoric acid) and acetonitrile and in the proportion of 60:40 (v/v/v). Detection was carried out at 255 nm. Retention time of celecoxib and diacerein was found to be 5.72±0.67 and 3.76±0.5 min, respectively. The method has been validated for linearity, accuracy and precision and robustness. Linearity for celecoxib was in the range of 20-60 μg/ml and for diacerein in the range of 5-15 μg/ml. The percentage recoveries obtained for celecoxib and diacerein were in range of 99.54-100.65% and 98-100.41% respectively and can be successfully applied for the routine analysis in pharmaceutical capsule dosage form....
This paper presents a RP-HPLC method for the simultaneous estimation of Dicyclomine and Tramadol Hydrochloride in combined tablet dosage form. The process was carried out on Sunshell Fused Core Shell C18 ( 100 x 4.6 mm), 2.6 μ column using phosphate buffer and Acetonitrile pH 7.5 in the ratio of 70:30 v/v respectively as a mobile phase at a flow rate of 1.5 mL/min. Detection wavelength was fixed at 224 nm. Linearity was observed in the concentration range of 4-20 μg/ml for Dicyclomine (r2=0.998) and 20-100 μg/ml for Tramadol Hydrochloride (r2=0.998). The retention time of Dicyclomine and Tramadol Hydrochloride was found to be 1.53 and 1.10 minutes, respectively. The developed method is simple, precise, specific, robust, rapid, reproducible, and sensitive and it can be used for estimation of Dicyclomine and Tramadol Hydrochloride in combined tablet dosage form....
A specific, accurate, precise and reproducible method has been developed and validated for the simultaneous estimation of amoxycillin trihydrate and tinidazole in combined dosage form by UV Spectrophotometer by applying Simultaneous Equation method. For development of method wavelengths selected were 229 nm and 310.40 nm for estimation of amoxycillin trihydrate (AMX) and tinidazole (TIN) respectively. The two drugs obeyed Beer-Lambert’s law over the concentration range of 8-18 μg/ml for amoxycillin trihydrate and 6-21 μg/ml for tinidazole. Validation of the proposed method was carried out for its specificity, linearity, range, accuracy, precision, Limit of detection, Limit of quantitation according to ICH guidelines. Recovery was found in the range of 99.41 to 100.47% for tinidazole and amoxycillin trihydrate in the formulation. The % assay of tinidazole and amoxycillin trihydrate was found to be in the range 99.54–94.90% by the proposed method. The results of analysis have been validated statistically and recovery studies confirmed the accuracy and reproducibility of the proposed method which was carried as per ICH guidelines. The proposed method was successfully applied in routine work for the determination of amoxycillin trihydrate and tinidazole in combined tablet dosage form....
Absorption ratio method was developed and validated for the determination of Levosulpiride and Pantoprazole in capsules. The method involved Q-absorption analysis based on the measurement of absorbance at two wavelengths, i.e λmax of Pantoprazole (287.8 nm) and Iso-absorptive point of both drugs (262.6 nm). Beer’s law was obeyed in the concentration range for LEVO was found to be in the range of 25-125 μg/ml and for PANTO 6-30 μg/ml. The results of analysis have been validated statistically and by recovery studies. The method was found to be simple, precise, reproducible and economical. Hence it is more suitable for routine analysis of these drugs in combined dosage forms....
A simple and sensitive spectrofluorimetric method has been developed for the estimation of telmisartan in tablet dosage form. Telmisartan (TEL) has imidazole and biphenyl groups in its structure, which are the fluorescent groups. Based on the fluorescent groups, telmisartan produces strong fluorescence in NaOH. Fluorescence intensity was measured at 363 nm (λem) with excitation at 298 nm (λex). Linearity range was found to be 200-1200 ng/ml with mean recovery 99.78%. The correlation co-efficient was found to be 0.9992. The method was validated in terms of % RSD of repeatability (0.29), precision (intra-day variation, 0.28 to 1.45 and inter-day variation, 0.92 to 2.57 ). The limit of detection (LOD) and limit of quantification (LOQ) for telmisartan were found to be 3.89 and 11.79 ng/ml, respectively. The developed method was successfully used for the assay of telmisartan tablet formulations. The content of TEL in two marketed formulations was found to be 103.38% and 99.73% of labelled amount. The spectrofluorimetric method was found to be specific, sensitive, accurate and precise and can be used for the routine quality control testing of telmisartan in tablet dosage form....
The aim of this work was to develop and validate a dissolution test for Eperisone Hydrochloride in Tablets using spectrophotometric method. The dissolution established conditions were 0.1N HCL 900 mL for 2 hrs as dissolution medium, using a(USP-II) paddel apparatus at a rotating rate of 75 rpm. The drug release was evaluated by UV spectrophotometric method at 261 nm. The method was validated to meet requirements for a global regulatory filing. The validation included specificity, linearity, precision and accuracy....
Accurate, precise, and rapid UV Spectrophotometric area under curve method was developed for the estimation of estimation of Eperisone hydrochloride in pharmaceutical dosage form. The principle for Area under Curve is “the area is measured around wavelength maxima of drug”. Area selected for Quantitation was 228.0-291.0 nm for Eperisone Hydrochloride in distilled water. Linearity observed in the concentration range was 2-10 µg/ml .The accuracy and precision were determined and found to comply with ICH guidelines....
A simple, rapid, accurate and precise spectrophotometric method has been developed for simultaneous estimation of Cefpodoxime proxetil and Azithromycin Dihydrate in their combined pharmaceutical dosage form. This method utilizes methanol as a solvent. λmax of Cefpodoxime Proxetil and Azithromycin Dihydrate for analysis were found to be 234 nm and 353 nm respectively. Linearity was observed in the concentration range of 5-25 μg/ml for Cefpodoxime Proxetil (r2=0.9998) and 20-100 μg/ml for Azithromycin Dihydrate (r2=0.9998). The results of analysis have been validated statistically and by recovery studies. Developed method was applied to pharmaceutical dosage form. The results were found to be within acceptance criteria according to ICH guideline....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical Q-absorbance ratio method for the simultaneous determination of Ceftazidime and Clavulanic acid in bulk and in pharmaceutical dosage form. Absorbance ratio method uses the ratio of absorbance at two selected wavelengths, one which is an isoabsorptive point and other being the λ-max of one of the two components. Ceftazidime and Clavulanic acid show an isoabsorptive point at 269 nm in dist. water. The second wavelength used is 256 nm, which is the λ-max of Ceftazidime in dist. water. The linearity was obtained in the concentration range of 4-16 μg/ml for Ceftazidime and 50-250 μg/ml Clavulanic acid. The concentrations of the drugs were determined by using ratio of absorbance at isoabsorptive point and at the λ-max of Ceftazidime. The method was successfully applied to pharmaceutical dosage form because of no interference. The results of analysis have been validated by recovery studies....
UV Spectrophotometric method has been developed for simultaneous estimation of Dicyclomine (DCY) and Tramadol Hydrochloride (TRA) in bulk drug and in laboratory mixture. This method utilizes 0.1 N NaOH as a solvent and λmax of Dicyclomine and Tramadol Hydrochloride selected for analysis was found to be 224 nm and 276 nm respectively. Linearity was observed in the concentration range of 2.5-15 μg/ml for Dicyclomine (r2=0.997) and 12.5-75 μg/ml for Tramadol Hydrochloride (r2=0.996). The method was validated statistically and by recovery studies. The mean % recovery was 99.22-100.27% and 98.94-100.33% for Dicyclomine and Tramadol Hydrochloride respectively. Developed method was applied to laboratory mixture. The results were found to be within acceptance criteria according to ICH guideline. This method was simple, rapid, accurate and sensitive....
In the present study deals the simultaneous estimation of Hydralazine hydrochloride and Propranolol in combined tablet dosage form have been developed using Distilled water as a solvent. Two method is developed one is simultaneous equation method at 260 nm and 288 nm. The second is the Q – analysis (absorption ratio) method, which involves the formation of absorbance equation at 273 nm (isoabsorptive point) and at 288 nm the (maximum absorption of Propranolol). Beer’s law Obeyed in concentration range of 4-20 μg/ mL and 10-50 μg/ mL for Hydralazine Hydrochloride and Propranolol respectively. The accuracy of the methods was assessed by recovery studies was found to be 99.80±0.316 and 99.65±0.209 for simultaneous equation method and 99.86±0.556 and 99.55±0.856for Q analysis (absorption ratio) method for Hydralazine hydrochloride and Propranolol respectively. These methods are simple, accurate and rapid; those require no preliminary separation and can therefore be used for routine analysis of both drugs in quality control laboratories....
Citicoline sodium subjected to different ICH prescribed stress conditions. Degradation was found to occur in hydrolytic, oxidative, thermal condition, while the drug was stable to photolytic and humidic condition. A stability indicating high performance liquid chromatography (HPLC) method was developed for analysis of drug in the presence of degradation products. The chromatographic method was fine tuned using the sample generated from forced degradation studies. Good resolution between the peaks corresponds to degradation products and the analyte was achieved on 5 , 250 mm × 4.6 mm i.d., C18 column (Phenomenox, USA). Mobile phase consists of mixture of water: orthophosphoric acid (99:1, v/v) (pH 4.0). Quantitation was achieved with UV detection at 272 nm based on peak area. The method was validated for accuracy, precision, linearity, range and selectivity....
The present manuscript describes simple, rapid, accurate, precise and economical stability indicating assay method for analysis of Citicoline sodium by UV spectrophotometric method. The analysis is based on the stability indicating assay method for using distill water as a solvent. Citicoline sodium has absorbance maxima at 272 nm in distill water. The linearity was obtained in the concentration range of 10-60 μg/ml for Citicoline sodium, respectively. The mean recovery was 100.20±1.16 for Citicoline sodium, respectively. The method was applied for the forced degradation study of this drug. The suitability of this method for the quantitative determination of Citicoline sodium was proved by evaluating different validation parameters. The proposed method was found to be simple and sensitive for the routine estimation of this drug. The results of analysis have been validated by recovery studies....
A specific, accurate, precise and reproducible stability indicating HPLC method has been developed and subsequently validated for the simultaneous determination of levosulpiride and pantoprazole in Dosage form. The proposed HPLC method utilizes hypersil (Thermo scientific) C18 column (250 mm × 4.6 mm id, 5 μm particle size), and mobile phase consisting of acetonitrile - 0.05M potassium dihydrogen phosphate buffer - 0.1% triethylamine in the ratio of 45:55:2.5 and pH adjusted to 4.0 with orthophosphoric acid at a flow rate of 1.0 ml/min. Quantitation was achieved with UV detection at 290 nm based on peak area with linear calibration curves at concentration ranges 7.5-22.5 μg/ml for levosulpiride and 4-12 μg/ml for pantoprazole. The retention time of levosulpiride and pantoprazole were found to be 3.37 min and 4.94 min respectively. The method was validated in terms of accuracy, precision, linearity, limits of detection, limits of quantitation and robustness. This method has been successively applied to capsule dosage form and no interference from the excipients was found. Levosulpiride, pantoprazole and their capsule dosage form were exposed to acid, base, oxidation, dry heat and sunlight stress conditions and the stressed samples were analyzed by the proposed method. As the proposed method could effectively separate the drug from its degradation products, it can be employed as stability-indicating method for the determination of instability of these drugs in bulk and commercial pharmaceutical formulations....
Reverse phase-high performance liquid chromatographic method and high performance thin layer chromatography were developed for the determination of Fosinopril Sodium in pharmaceutical dosage form and validated. The chromatographic conditions comprised of a reversed-phase C18 column (250 x 4.6 mm), 5 µ with a mobile phase consisting of Methanol: Buffer (0.2 % H3PO4) in the ratio (85:15v/v). Flow rate was 1 mL / min. Detection was carried out at 215 nm. The retention time was 8.5 min. It was subjected to acid & alkali hydrolysis, oxidation, photochemical and thermal degradation. The linearity curve was found to be linear over 40-160 µg/ml. The value of correlation coefficient, slope and intercept were, 0.9999, 40.29 & 13.06 respectively. The method was found to be accurate over 97.5% – 102.0%. The method was found to be precise with % RSD 0.100–0.114 for intra-day (n=3) and % RSD 0.110–0.130 for inter-day (n=3). The LOD and LOQ were found to be 1.00 μg/ml and 3.00 μg/ml respectively....
The objective of the current study was to develop and validate a rapid, precise, specific and stability-indicating reverse phase HPLC for the quantitative determination of olsalazine in its dosage form. The determination is done for the active pharmaceutical ingredient in its pharmaceutical dosage form in the presence of degradation products. The drug was subjected to stress conditions of acid, alkali, thermal, photolytic, humidity and peroxide. As per international conference on harmonization (ICH) prescribed stress conditions to show the stability-indicating power of the method. It was found olsalazine is very sensitive to various stress conditions. The chromatographic conditions were optimized using the samples generated from forced degradation studies. Regression analysis shows an r value (correlation coefficient) 0.99 for olsalazine. The chromatographic separation was achieved on a symmetry Hypersil BDS C18V 4.6 mm x 150 mm, 5 µm. The method employed an isocratic elution and the detection wave-length was set at 290 nm. The mobile phases consists of ACN:Potassium dihydrogen phosphate in 1000 ml water. (Buffer) pH 6.0 delivered at a flow rate of 1.0 ml per min. The developed RP-HPLC method was validated with respect to linearity, accuracy, precision and robustness....
UV spectrophotometric Area under curve method has been developed for simultaneous estimation of Diazepam and Imipramine Hydrochloride. The method involved measurement of area at 279-289 nm (Diazepam) and at 245-255.0 nm (Imipramine Hydrochloride) of Diazepam and Imipramine Hydrochloride respectively. Beer’s law obeyed in concentration range of 3-15 µg/ml for Diazepam and 5-25 µg/ml for Imipramine Hydrochloride in 0.1 M HCl. The percent assay of marketed formulation was 100.30±0.53 and 100.45±0.71 of Diazepam and Imipramine Hydrochloride respectively. The proposed methods are rapid, simple, accurate and precise since they are recommended for routine analysis....
UV spectrophotometric Dual wavelength method has been developed for simultaneous estimation of Diazepam and Imipramine Hydrochloride. The method involved measurement of absorbance difference at 267.2 nm and 304.0 nm (where Imipramine Hydrochloride have same absorbance) and absorbance difference at 235.6 nm and 278.0 nm (where Diazepam have same absorbance) of Diazepam and Imipramine Hydrochloride respectively. Beer’s law obeyed in concentration range of 3-15 µg/ml for Diazepam and 5-25 µg/ml for Imipramine Hydrochloride in 0.1 M HCl. The percent assay of marketed formulation was 100.30±0.53 and 100.45±0.71 of Diazepam and Imipramine Hydrochloride respectively. The proposed methods are rapid, simple, accurate and precise since they are recommended for routine analysis....
UV spectrophotometric Dual wavelength method has been developed for simultaneous estimation of Drotaverine Hydrochloride and Diclofenac Potassium. The method involved measurement of absorbance difference at 262.0 nm and 287.6 nm (where Diclofenac potassium have same absorbance) and absorbance difference at 294 nm and 311.8 nm (where Drotaverine Hydrochloride have same absorbance) of Drotaverine Hydrochloride and Diclofenac Potassium respectively. Beer’s law obeyed in concentration range of 7-23 µg/ml and 4-20 µg/ml in distilled water for Drotaverine Hydrochloride and Diclofenac Potassium respectively. The percent assay of marketed formulation was 99.10% ± 0.5666 and 99.52% ± 1.3032 of Drotaverine Hydrochloride and Diclofenac Potassium respectively. The proposed methods are simple, accurate and precise since they are recommended for routine analysis....
High Performance Thin Layer Chromatography has been developed for simultaneous estimation of Diazepam and Imipramine Hydrochloride. The method involved measurement of absorbance difference at 274.0 nm The separation was carried out on Merck HPTLC aluminum sheets of silica gel 60F254 using Toluen:Methanol:FormicAcid (8:2.0:0.2 v/v/v/v) as mobile phase. The linear regression analysis data was used for the regression line in the range of 300–800 ng/spot and 2250–6000 ng/spot for DIZ and IMP, respectively. The percent assay of marketed formulation was 100.10±0.12 and 99.96±0.26 of Diazepam and Imipramine Hydrochloride respectively. The proposed methods are rapid, simple, accurate and precise since they are recommended for routine analysis....
A simple, selective, precise and accurate colorimetric method of analysis of Anidulafungin in pharmaceutical dosage form was developed and validated. The solvent used was methanol with methyl orange as a colorimetric reagent. Anidulafungin was detected at 464 nm at room temperature. The linear regression analysis data for the linearity plot showed good linear relationship with correlation coefficient value, R2=0.998 in the concentration range 5–50 µg/ml with slope 0.008, intercept -0.021. The method was validated according to the International Conference on Harmonization (ICH) guidelines for linearity, range, accuracy, precision and specificity and applied on bulk powder and pharmaceutical formulations. Anidulafungin was determined in sterile dosage form in range of 99.73% with 0.327 standard deviation. The accuracy of the method was validated by recovery studies and was found to be significant and under specification limits, with % Recovery 99–101.1 (within acceptable range (98–102%)....
A simple, economical, precise, and accurate zero crossing difference spectrophotometric method for simultaneous determination of cefadroxil and probenecids in synthetic mixture have been developed. Measurements of absorbance were carried out at zero-crossing wavelengths 313 nm and 232 nm for cefadroxil and probenecid by zero-crossing difference spectrophotometric method. Beer’s law is obeyed in the concentration range of 4-36 μg/ml for cefadroxil and 5-25 μg/ml for probenecid by zero-crossing difference spectrophotometric method. The method was validated in terms of accuracy, precision, linearity, limits of detection, limits of quantitation. This method has been successively applied to synthetic mixture and no interference from the synthetic mixture’s excipients was found....
The aim of this study was to develop and validate a dissolution test for the quality control of Atenolol and Indapamide, using RP-HPLC method. The optimised dissolution conditions includes USP apparatus II at a paddle rotation rate of 50 rpm and 900 ml of modified acetate buffer (pH=4.6) at 37°C±0.5°C. Under these conditions, the in-vitro release profiles of Atenolol and Indapamide showed good results. The drug release was evaluated by RP-HPLC using column Hyperchrom ODS 5 µ C18 (250X4.6 mm, 100°A), detection wavelength 240 nm having the flow rate 1.0mL/min using using methanol: water in the proportion of 80:20 and adjusted pH to 3.0 with10% orthophosphoric acid. The method validation was carried out as per for USP guidelines and it was found that the results obtained by proposed method for dissolution test for tablet formulation containing Atenolol and Indapamide are reliable, precise and accurate. Hence it was routinely adopted for dissolution analysis of the said drugs in the formulation....
A simple, accurate, and precise Simultaneous Equation spectrophotometric method was developed for simultaneous determination of Lignocaine and Propofol. The method involves determination of Lignocaine at 224.2-240.6nm and Propofol at 258.6-284nm. Both drugs follow Beer-Lambert’s law over the concentration range of 20-100 μg/ml and 10-50 μg/ml for Lignocaine and Propofol respectively. The % assay of the drugs was found to 98.7±1.63 and % 98.8±1.48 for Lignocaine and Propofol respectively. Validation of the proposed method was carried out for its linearity, accuracy, precision, LOD, and LOQ, according to ICH guidelines. The recovery of the Lignocaine and Propofol were found to 99.33±0.82% and 99.60±0.56% for Lignocaine and Propofol respectively. The proposed methods can be successfully applied in routine work for determination of Lignocaine and Propofol in pharmaceutical dosage form....
The present manuscript describe simple, sensitive, rapid, accurate, precise and cost effective dual wavelength spectrophotometric method for the simultaneous determination of Amitryptiline HCl and Chlordiazepoxide in combined tablet dosage form. The utility of dual wavelength data processing program is its ability to calculate unknown concentration of components of interest in a mixture containing an interfering component. The principle for dual wavelength method is “the absorbance difference between two points on the mixture spectra is directly proportional to the concentration of the component of interest”. The method was based on determination of Amitryptiline HCl at the absorbance difference between 237 nm and 254 nm and Chlordizepoxide at the absorbance difference between 231 nm and 245 nm. 0.1 N HCl was taken as a solvent. Regression analysis of Beer’s plots showed good correlation range of 6-16 µg/ml for Amitryptiline HCl and 3-10 µg/ml for Chlordizepoxide with correlation coefficient r2 0.9976 and 0.9946, respectively. The mean % recoveries were found to be in the range of 98.63 % - 100.16 % and 98.89 % - 99.72 % for Amitryptiline HCl and Chlordizepoxide, respectively. The proposed method has been validated as per ICH guideline and successfully applied to the estimation of pharmaceutical dosage form....
Ilaprazole is a substituted benzimidazole that inhibits gastric acid secretion and used for the treatment of erosive or ulcerative GERD, DU and hypersecretory syndromes. In present work Simple, sensitive and specific spectrophotometric method were developed and validated for quantification of Ilaprazole by difference spectroscopy. Ilaprazole exhibits a substantial difference in absorbance in the two solvents that is in 0.1 M HCl and 0.1 M NaOH at 256 nm and 307 nm respectively. Beer’s law was obeyed in the concentration range of 3 to 18 μg ml-1for Ilaprazole. Results of tablet analysis showed standard deviation in the range of 99.75% for ENL which indicate repeatability of the method. The results indicated excellent recoveries ranging from 99.23 to 99.35 %. Recoveries obtained do not differ significantly from 100% showed that there was no interference from the common excipients used in the tablet formulation indicating accuracy and reliability of the method....
A new absorption ratio method was developed and validated for the determination of Ketotifen and Cetirizine Dihydrochloride in tablet. The method involved Q-absorption analysis based on the measurement of absorbance at two wavelengths, i.e. λmax of cetirizine dihydrochloride (230.0 nm) and Iso-absorptive point of both drugs (240.0 nm). Beer’s law was obeyed in the concentration range for KETO and CET was found to be in the range of 4-20 μg/ml for both. The results of analysis have been validated statistically and by recovery studies. The method was found to be simple, precise, reproducible, less time consuming and economical. Hence it is more suitable for routine analysis of these drugs in combined dosage forms....
Tramadol hydrochloride and Diclofenac sodium are used in combined dosage form for used for the symptomatic treatment of moderate to severe pain in adult patients. Present work consist development and validation of HPTLC estimation of Tramadol hydrochloride (TRA) and Diclofenac sodium (DCS) in Synthetic mixture. These UV spectroscopy methods are developed using CAMAG loaded with Win Cats software.for wavelengths were selected 280 nm for TRA and DCS as Toluene,Ethylacetate,Methanol and Ammonia used as a solvent. In this HPTLC methods linearity of TRA and DCS were found to be in range of 2500-7500 ng/spot and 3750-11250 ng/spot respectively with correlation coefficient > 0.998. this method are simple, accurate, precise, economical and statistically validated. There was no interference of any excipient in the determination of drugs in synthetic mixture. These method can be applied for routine quality control analysis and dissolution study....
A simple, precise, accurate and reliable HPTLC method has been developed and validated for analysis of Eperisone hydrochloride (EPE) and Diclofenac sodium (DIC) in their combined dosage form. Identification and analysis were performed on 100 mm x 100 mm layer thickness 0.2 mm, pre-coated silica gel G60-F254 aluminum sheet, prewashed with methanol and dried in an oven at 50°C for 5 min. Toluene : methanol : ethyl acetate : ammonia (6:2:2:0.05) (v/v/v/v) was used as mobile phase. Calibration plots were established showing the dependence of response (peak area) on the amount chromatographed. The validated calibration ranges were 450-1950 ng/spot and 300-1300 ng/spot for EPE and DIC with correlation coefficient (R2) 0.9958 and 0.9984 respectively. Average % recovery was between 99.55–100.11% and 99.09–102.41% for EPE and DIC respectively. The spots were scanned at 255 nm in a reflectance mode. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of EPE and DIC in their combined capsule dosage form....
A simple, economic, accurate chemical derivatization method was developed for the sertraline Hydrochloride (racemic mixture) in bulk and tablet dosage form. 3-Methyl 2-Benzo Thiazolinone Hydrozone Hydrochloride Monohydrate (MBTH) reagent was used for the chemical derivatization. The maximum absorption was observed at 622.5 nm. The linearity range was found to be 10 - 30 µg/ml. The proposed method was validated. The reports was expressed that the proposed method was found to be simple, precise, accurate and rapid for determination of sertraline Hydrochloride from pure and its dosage forms....
HPLC in the present era is an important tool in the separation, identification and quantification of bulk drug and different pharmaceutical formulations. Bepotastine Besilate being a selective histamine H1 antagonist is used in the treatment of allergic rhinitis and chronic utricaria. The present research work emphasizes on the development and validation of an RP-HPLC method with UV detection for the estimation of Bepotastine Besilate in bulk drug and in ophthalmic solution. The separation of the drug is achieved isocratically on a Kromasil C18 column (4.6 mm × 101 mm) with a mobile phase consisting of methanol (60 volumes) and phosphate buffer (40 volumes) with apparent pH of 3.0 (±0.1). The flow rate was maintained constant at 1.0 ml/min. The wavelength of detection was 259 nm. The method is found to be linear (r=0.9904) at a concentration range of 20µg/ml to 100 µg/ml. The intra and inter day precision studies were found to be satisfactory with %RSD not exceeds by 2%. The developed method was found to be accurate. The proposed method is having a thorough output as the analysis involved short run-time i.e. about 4 minutes. The method is meeting with the ICH regulatory requirements as per ICH Q2 (R1) guidelines. Thus the method developed was successfully applied for the estimation of Bepotastine Besilate in bulk and ophthalmic solution as a dosage form with acceptable accuracy and precisions....
A simple, precise, accurate and reliable HPTLC method has been developed and validated for analysis of Eperisone hydrochloride (EPE) and in their combined dosage form. Identification and analysis were performed on 100 mm x 100 mm layer thickness 0.2 mm, pre-coated silica gel G60-F254 aluminum sheet, prewashed with methanol and dried in an oven at 50°C for 5 min. Toluene : methanol : ethyl acetate : ammonia (6:2:2:0.05) (v/v/v/v) was used as mobile phase. Calibration plots were established showing the dependence of response (peak area) on the amount chromatographed. The validated calibration ranges were 450-1950 ng/spot for EPE with correlation coefficient (R2) 0.9958. Average % recovery was between 99.55–100.11% for EPE. The spots were scanned at 255 nm in a reflectance mode. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of EPE in their tablet dosage form....
The simple, specific, accurate, precise and reproducible methods have been developed and validated for the simultaneous estimation of both drugs in their combined dosage form. In RP-HPLC, analysis is carried out using Buffer (KH2PO4 50 mM 4.5 pH): Methanol (55:45 % v/v) pH 4.5 adjusted by Orthophosphoric acid) mobile phase and BDS hypersil C18, 250 mm × 4.6 mm, 5 µ (particle size), Thermo scientific as stationary phase with detection wavelength of 232 nm. Linearity was obtained in the concentration range of 5-15 μg/ml and 50-150 μg/ml for Linagliptin and Metformin Hydrochloride respectively. The % recoveries of the both the drugs were found to be 99.81-100.21% and 99.74-100.15% respectively. LOD were found to be 0.18 μg/ml and 6.24 μg/ml at nm for Linagliptin and Metformin Hydrochloride respectively. Methods were statistically validated for accuracy, precision, specificity, LOQ, robustness and ruggedness according to ICH guidelines and can be used for analysis of combined dosage form....
The present manuscript describe simple, sensitive, rapid, accurate, precise and economical first derivative spectrofluorimetric method for the simultaneous determination of Diclofenac potassium and Febuxostat in combined tablet dosage form. The derivative spectrofluorimetric method was based on the determination of both the drugs at their respective zero crossing point (ZCP). The first order derivative spectra were obtained in and the determinations were made at 384.160 nm (ZCP of Febuxostat) for Diclofenac potassium and 364.321 nm (ZCP of Diclofenac potassium) for Febuxostat. The linearity was obtained in the concentration range of 1000-5000 ng/ml for Diclofenac potassium and 400-2000 ng/ml for Febuxostat. The mean recovery was 99.87±0.77 and 99.95±0.46 for Diclofenac potassium and Febuxostat, respectively. The method was found to be simple, sensitive, accurate and precise and was applicable for the simultaneous determination of Diclofenac potassium and Febuxostat in pharmaceutical tablet dosage form. The results of analysis have been validated statistically and by recovery studies....
A simple, sensitive, rapid, accurate, precise and economical Q-absorbance ratio method has been developed for the simultaneous determination of Amitryptiline HCl and Chlordizepoxide in combined dosage form. Absorbance ratio method uses the ratio of absorbances at two selected wavelengths, one which is an isoabsorptive point and other being the λ-max of one of the two components. Amitryptiline HCl and Chlordizepoxide show an isoabsorptive point at 220 nm in 0.1 N HCl. The second wavelength used is 246 nm, which is the λ-max of Chlordizepoxide in 0.1 N HCl. The linearity was obtained in the concentration range of 5-10 μg/ml for Amitryptiline HCl and 5-10 μg/ml for Chlordizepoxide. The concentrations of the drugs were determined by using ratio of absorbances at isoabsorptive point and at the λ-max of Chlordizepoxide. The method was successfully applied to pharmaceutical dosage form because of no interference. The results of analysis have been validated by recovery studies....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical Q-absorbance ratio method for the simultaneous determination of Dicyclomine and Tramadol Hydrochloride in bulk and in combined dosage form. Absorbance ratio method uses the ratio of absorbance at two selected wavelengths, one which is an isoabsorptive point and other being the λ-max of one of the two components. Dicyclomine and Tramadol Hydrochloride show an isoabsorptive point at 222 nm in 0.1 N NaOH. The second wavelength used is 276 nm, which is the λ-max of Tramadol Hydrochloride in 0.1 N NaOH. The linearity was obtained in the concentration range of 2.5-15 μg/ml for Dicyclomine and 12.5-75 μg/ml Tramadol Hydrochloride. The concentrations of the drugs were determined by using ratio of absorbance at isoabsorptive point and at the λ-max of Tramadol Hydrochloride. The method was successfully applied to pharmaceutical dosage form because of no interference. The results of analysis have been validated by recovery studies....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical Q-absorbance ratio method for the simultaneous determination of Naproxen and Paracetamol in their tablet dosage form. Absorbance ratio method uses the ratio of absorbance at two selected wavelengths, one which is an isoabsorptive point and other being the λ-max of one of the two components. Naproxen and Paracetamol show an isoabsorptive point at 239 nm in 0.1 N NaOH. The second wavelength used is 257 nm, which is the λ-max of Paracetamol in 0.1 N NaOH. The linearity was obtained in the concentration range of 0.5-2.5 μg/ml for Naproxen and 0.83-4.15 μg/ml Paracetamol. The concentrations of the drugs were determined by using ratio of absorbance at isoabsorptive point and at the λ-max of Paracetamol. The method was successfully applied to pharmaceutical dosage form because of no interference. The results of analysis have been validated by recovery studies....
Tramadol Hydrochloride and Diclofenac Sodium are used in combined dosage form for used for the symptomatic treatment of moderate to severe pain in adult patients. Present work sconsist development and validation of Ratioderivative UV Spectrophotometric for simultaneous estimation of Tramadol Hydrochloride (TRA) and Diclofenac Sodium (DCS) in Synthetic mixture. These UV spectroscopy methods are developed using Shimadzu double beam UV visible spectrophotometer (Model 1800) loaded with UV Probe 2.32 software. For ratio first derivative wavelengths were selected 230 nm for TRA and 245.2 nm for DCS Methanol used as a solvent. In this UV spectrophotometric methods linearity of TRA and DCS were found to be in concentration range of 4-24 µg/mL and 6-36 µg/mL respectively with correlation coefficient >0.998. This method is simple, accurate, precise, economical and statistically validated. There was no interference of any excipient in the determination of drugs in synthetic mixture. These method can be applied for routine quality control analysis and dissolution study....
The ratio spectra derivative spectrophotometric method was developed for resolving binary mixture of cefixime trihydrate and levofloxacin hemihydrate in tablet formulation. The method involves the use of the first derivative of the ratio of spectra. The absorption spectrum of mixture was obtained and the amplitudes at appropriate wavelengths were divided by the corresponding amplitudes in the absorption spectrum of standard solution of one of the components, and the first derivative of the ratio spectrum was obtained. For the determination of cefixime trihydrate, 4 µg/mL solution of levofloxacin hemihydrate was used as divisor and the 1DD (∆λ=8) amplitudes at 318.6 nm, were plotted against levofloxacin hemihydrate concentration; while – by using 4 µg/mL solution of levofloxacin hemihydrate as divisor – the 1DD (∆λ=8) amplitudes at 338.4.6 nm were found to be proportional to cefixime trihydrate concentration. The calibration curve was established in concentration range of 2-24 µg/mL with correlation coefficient of 0.9960, and 2-14 µg/mL with correlation coefficient of 0.9998 for cefixime trihydrate and levofloxacin hemihydrate, respectively, by measuring signal in respective first derivative ratio spectra. Results of analysis were validated statistically and recovery study. The method has been applied for resolving binary mixture of cefixime trihydrate and levofloxacin hemihydrate in tablet formulation....
A simple, precise, accurate, reproducible Second order derivative Spectroscopic method was developed for the estimation of Rivaroxaban in bulk and dosage form. The study was conducted in Methanol. The method was found to be linear in the range of 2-12 μg/ml (r2=0.9998) for Rivaroxaban at λmax=300 nm and λmin=280 nm. The proposed method was validated for linearity, precision, accuracy and ruggedness according to ICH guideline for routine estimation purpose of drug in bulk and dosage form. Since the 2nd derivative method has been developed and validated to ensure that the performance characteristic of the method meets the requirements for the intended analytical applications....
A simple, accurate, and precise Simultaneous Equation spectrophotometric method was developed for simultaneous determination of Ketorolac Tromethamine and Olopatadine Hydrochloride. The method involves determination of Ketorolac Tromethamine at 320.0 nm and Olopatadine Hydrochloride at 206.0 nm. Both drugs follow Beer-Lambert’s law over the concentration range of 4-20 μg/ml and 2-10 μg/ml for Ketorolac Tromethamine and Olopatadine Hydrochloride respectively. The % assay of the drugs was found to 98.99±0.7619 and %99±1.3228 for Ketorolac Tromethamine and Olopatadine Hydrochloride respectively. Validation of the proposed method was carried out for its linearity, accuracy, precision, LOD, and LOQ, according to ICH guidelines. The recovery of the Ketorolac Tromethamine and Olopatadine Hydrochloride were found to 100.18±0.072167% and 99.55±0.010516% for Ketorolac Tromethamine and Olopatadine Hydrochloride respectively. The proposed methods can be successfully applied in routine work for determination of Ketorolac Tromethamine and Olopatadine Hydrochloride in pharmaceutical dosage form....
A simple, accurate, and precise dual wavelength spectrophotometric method was developed for simultaneous determination of Montelukast sodium and Olopatadine hydrochloride in synthetic mixture. The method is based on the principle that “the absorbance difference between two points on the mixture spectra is directly proportional to the concentration of the component of interest”. The method involves determination of Montelukast at 232.0 nm and Olopatadine at 206.0 nm. Both drugs follow Beer-Lambert’s law over the concentration range of 5-25 μg/ml and 2-10 μg/ml for Montelukast and Olopatadine, respectively. The % assay of the drugs was found near to 100% representing the accuracy of the method. The recovery of the Montelukast and Olopatadine were found near to 100%. Validation of the proposed method was carried out for its accuracy, precision, specificity and ruggedness according to ICH guidelines. Assay results for both drugs obtained by newly developed method were statistically compared with the reported methods for respective drugs which establish the reliability of the proposed method. The proposed methods can be successfully applied in routine work for determination of Montelukast and Olopatadine in synthetic mixture....
A simple, rapid, accurate, precise and economical reverse phase high performance liquid chromatographic method is developed for simultaneous separation and quantification of two anti-hypertensive drugs, viz., chlorthalidone and nebivolol hydrochloride. The separation of both the drugs was achieved on Zorbax eclipse XDB C8 column (250 x 4.6 mm id, 5 µm particle size) column using a mobile phase of Potassium dihydrogen phosphate and triethylamine buffer solution (at pH 3): acetonitrile (65:35 v/v). The flow rate was 1 ml/min and detection was done at 280 nm. The retention time for chlorthalidone was 4.36 min and nebivolol hydrochloride was 9.68 min. Chlorthalidone and nebivolol hydrochloride showed a linear response in the concentration range of 31.25-187.5 µg/ml and 12.5-75 µg/ml respectively. The correlation co-efficients for Chlorthalidone and Nebivolol hydrochloride were 0.9998 and 0.9999 respectively. The percentage recoveries obtained for chlorthalidone and nebivolol hydrochloride ranges from 99.4% to 100.5% and 99.4% to 99.8% respectively. The results of analysis have been validated as per ICH guidelines. Validation results indicated that method shows satisfactory linearity, accuracy, precision and ruggedness. The extremely low flow rate, simple mobile phase composition makes this method cost effective, rapid and non-tedious and can also be successfully employed for simultaneous estimation of both drugs in commercial products....
A simple, rapid, accurate, precise and economical reverse phase high performance liquid chromatographic method is developed for simultaneous separation and quantification of two anti-hypertensive drugs, viz., chlorthalidone and olmesartan medoxomil. The separation of both the drugs was achieved on Inertsil ODS 3V C18 column (250 x 4.6 mm id, 5 µm particle size) column using a mobile phase of sodium dihydrogen phosphate buffer solution (at pH 3): acetonitrile (48:52 v/v). The flow rate was 1 ml/min and detection was done at 270 nm. The retention time for chlorthalidone was 3.65 min and olmesartan medoxomil was 6.23 min. Chlorthalidone and olmesartan medoxomil showed a linear response in the concentration range of 6.25-37.50 µg/ml and 10-60 µg/ml respectively. The correlation co-efficients for Chlorthalidone and olmesartan medoxomil were 0.9999 and 0.9998 respectively. The percentage recoveries obtained for chlorthalidone and olmesartan medoxomil ranges from 99.5% to 100.1% and 99.1% to 100.4% respectively. The results of analysis have been validated as per ICH guidelines. Validation results indicated that method shows satisfactory linearity, accuracy, precision and ruggedness. The extremely low flow rate, simple mobile phase composition makes this method cost effective, rapid and non-tedious and can also be successfully employed for simultaneous estimation of both drugs in commercial products....
A simple and rapid Q-Absorbance ratio method has been developed for simultaneous estimation of Metronidazole and Norfloxacin in suspension. Methanol was used as solvent & calibration curve was linear over the concentration range 4-24 µg/ml for MET & 2-14 µg/ml for NOR in Q-absorbance ratio method. For Q absorption ratio method 281.6 nm (λmax of NOR) and at 292 nm (Iso-absorptive point) was selected as analytical wavelength & % recovery for MET & NOR was found to be 98.44-99.93 and 99.27-99.91 respectively....
A simple and rapid Simultaneous equation method has been developed for simultaneous estimation of Metronidazole and Norfloxacin in suspension. Methanol was used as solvent & calibration curve was linear over the concentration range 4-24 µg/ml for MET and 2-14 µg/ml neither for NOR in simultaneous equation method. For simultaneous equation method 311 nm (λmax of MET) and 281.6 nm (λmax of NOR) was selected as analytical wavelength and % recovery was found to be 99.84-100.47 and 99.32-100.36 respectively for MET and NOR....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical derivative spectroscopic method for the simultaneous determination of Nifedipine (NFP) and Lidocaine (LDC) in cream. Derivative spectroscopy offers a useful approach for the analysis of drugs in cream. In this study a first-derivative spectroscopic method was used for simultaneous determination of Nifedipine and Lidocaine using the zero-crossing technique. The measurements were carried out at wavelengths of 257 nm and 235 nm for Nifedipine and Lidocaine respectively. The method was found to be linear (r2=0.991) in the range of 2-28 μg/ml for Nifedipine at 257 nm. The linear correlation was obtained (r2=0.990) in the range of 2-28 μg/ml for Lidocaine at 235 nm. The limit of detection was found to be 0.39 and 0.77 μg/ml for Nifedipine and Lidocaine respectively. The limit of quantification was found to be 1.19 and 2.34 μg/ml respectively. The method was successfully applied for simultaneous determination of Nifedipine and Lidocaine in cream....
A simple, specific, accurate and precise RP-HPLC method has been developed and Validated for the Simultaneous Estimation of Paracetamol, Cetirizine hydrochloride, Chlorpheniramine maleate and Dextromethorphan hydrobromide in their combined dosage form (tablet). The separation of four components was carried out using Hypersil C18 (250 × 4.6 mm, 5 µm or equivalent) column by isocratic elution with a flow rate of 1.2ml/min. The mobile phase composition was 0.01 M Sodium perchlorate buffer solution adjusted to a pH of 3 with orthophosphoricacid: acetonitrile (60:40 v/v) and detection was carried out at 210 nm. The retention time of Paracetamol, Cetirizine hydrochloride, Chlorpheniramine maleate and Dextromethorphan hydrobromide were 2.943 min, 9.950 min, 2.447 min and 6.577 min respectively. The method has been validated in terms of linearity, specificity, accuracy, precision, limit of detection, limit of quantitation, robustness as per ICH guidelines. The method has been found to be linear in the range of 325-975 µg/ml (R2=0.9987) for Paracetamol, 5-15 µg/ml (R2=0.999) for Cetirizine hydrochloride, 2-6 µg/ml (R2=0.999) for Chlorpheniramine maleate and 15-45 µg/ml (R2=0.9984) for Dextromethorphan hydrobromide respectively. The limit of detection and limit of quantitation were 0.391 and 0.9671 for Paracetamol, 0.0092 and 0.0279 for Cetirizine hydrochloride, 0.0203 and 0.0617 for Chlorpheniramine maleate and 0.0114 and 0.0346 for Dextromethorphan hydrbromide respectively. The recoveries of Paracetamol, Cetirizine hydrochloride, Chlorpheniramine maleate and dextromethorphan hydrobromide were 99.85%, 99.91%, 99.36% and 99.82% respectively and their relative standard deviations were less than 2%. Hence, the method could be successfully applied for routine analysis of Paracetamol, Cetirizine hydrochloride, Chlorpheniramine maleate and Dextromethorphan hydrobromide in their combined tablet dosage form....
A rapid, precise, specific, accurate and simple UV spectrophotometric method was developed and validated for the estimation of Rosuvastatin calcium and clopidogrel bisulphate in combined pharmaceutical dosage forms and laboratory prepared mixtures. The method was validated in terms of linearity, accuracy, precision, and specificity, limit of detection (LOD) and limit of Quantitation (LOQ) as per ICH guideline. To overcome the problem of spectral interference first order derivative spectroscopic method were adopted. The method obeys Beer’s Law in concentration ranges of 2-10 µg/ml for both drug. The λmax of Rosuvastatin calcium and Clopidogrel bisulphate were found to be at 244 nm and 219 nm respectively. The linearity ranges of both drugs were found to be in the range of 2- 10 μg/ml. The selected wavelengths by first order derivative method were found to be 323 nm for Rosuvastatin calcium and 243 nm for Clopidogrel bisulphate. The LOD and LOQ value were found to be 0.420 µg/ml and 0.874 µg/ml for Rosuvastatin calcium and 0.120 µg/ml and 0.365 µg/ml for Clopidogrel bisulphate respectively. The optimum conditions for the analysis of the drug were established. The percentage recovery of Rosuvastatin calcium and Clopidogrel bisulphate were 97-99.40 and 99.6-101.36 respectively. The developed method was successfully applied to the laboratory prepared mixtures....
This work is concerned with application of simple, accurate, precise and highly selective UV First derivative spectrophotometric and reverses phase high performance liquid chromatographic (RP-HPLC) method for simultaneous estimation of Simvastatin and Gefitinib in synthetic mixture. The first method was based on UV-First derivative spectrophotometric determination of two drugs which involves absorbance measurement at 237.2 nm (Simvastatin) and 348.0 nm (Gefitinib) in methanol. Linearity was obtained in the range of 1-3.5 μg/ml and 6-21 μg/ml for Simvastatin and Gefitinib respectively. Chromatographic separation was achieved isocratically at 25°C±0.5°C on Enable C18 column (250 х 4.6 mm i.d.) with a mobile phase composed of acetonitrile: methanol: water in the ratio of 60: 30: 10 % v/v/v at flow rate of 1.0 ml/min. The retention time of Simvastatin and Gefitinib was found to be 7.73 min and 5.23 min. respectively. The method was found to be linear in the range of 0.1-15 μg/ml for Simvastatin and 0.6-90 μg/ml for Gefitinib with mean recovery of 101.43±0.48% for Simvastatin and 100.63±0.45% for Gefitinib. The correlation coefficients for all components are close to 1. The developed methods were validated according to ICH guidelines and values of accuracy, precision and other statistical analysis were found to be in good accordance with the prescribed values. Thus the proposed method was successfully applied for simultaneous determination of Simvastatin and Gefitinib in routine analysis....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical spectrophotometric method for the simultaneous determination of Meropenem and Sulbactam Sodium in bulk and combined dosage form. The method is based on the simultaneous equations for analysis of both the drugs using 0.1 M KOH as solvent. Meropenem has absorbance maxima at 298 nm and Sulbactam Sodium has absorbance maxima at 260 nm in 0.1 M KOH. The linearity was obtained in the concentration range of 5-70 μg/ml and 2-21 μg/ml for Meropenem and Sulbactam Sodium, respectively. The concentrations of the drugs were determined by using simultaneous equations at both the wavelengths. The mean recovery was 99.5±0.26 and 99.87±0.35 for Meropenem and Sulbactam Sodium, respectively. The method was successfully applied to combined dosage form. The suitability of this method for the quantitative determination of Meropenem and Sulbactam Sodium was proved by validation. The proposed method was found to be simple and sensitive for the routine quality control application of Meropenem and Sulbactam Sodium in combination. The results of analysis have been validated statistically and by recovery studies....
Two simple, rapid, precise and accurate spectrophotometric methods have been developed for simultaneous estimation of Paracetamol (PCM) and Flupirtine meleate (FLU) in combined dosage form. Method A, Absorbance Correction Method, involves measurment at 320.00 nm (Corrected wavelenth) and 249.80 nm (λmax of Paracetamol) in zero order spectra. Method B, Ratio Derivative Method, involves division of spectra of Paracetamol by one selected standard spectrum of Flupirtine maleate and then measuring absorbance at 295.25 nm in ratio derivative spectra for estimation of Paracetamol. Similarly, spectra of Flupirtine maleate are divided by one selected standard spectrum of Paracetamol and then measuring absorbance at 297.60 nm in ratio derivative spectra for estimation of Flupirtine maleate. Developed methods were validated according to ICH guidelines. The calibration graph follows Beer’s law in the range of 2.0-25.0 μg/mL for both drug with R square value greater than 0.999. Accuracy of all methods was determined by recovery studies and showed % recovery between 98 to 102%. The methods were successfully applied for estimation of Paracetamol and Flupirtine meleate in marketed formulation....
Nebivolol HCl and Indapamide tablet is newly approved combination by CDSCO for the treatment of treatment of hypertension in patients whose blood pressure is not adequately controlled by monotherapy on 12 May 2010. Stability indicating HPLC method was developed using C18 (250 mm x 4.6 mm i.d., 5 μm particle size) column with Buffer : ACN (Acetonitrile) (25:75, pH 3.5 0.02 m KH2PO4 with Tryethylamine) as mobile phase with flow rate was 1.0 ml/min and detection wavelength 310 nm. In RP-HPLC method linearity ranged from 25-75 μg/mL for Nebivolol HCl and 7.5-22.5 μg/mL for Indapamide. Correlation coefficient was greater than 0.999 and accuracy (%Recovery) was between 98% - 102% for both drugs. The method successfully separated both the drugs from degradation products formed under acid hydrolysis, alkali hydrolysis, oxidative, photolytic and thermal stress conditions establishing specifity of the method. Moreover, the % RSD for repeatability, inter and intraday precision was found to be less than 2%, which reveals that the method is precise. In stress study both the drugs were found to degrade significantly under hypo alkaline acidic, oxidative and thermal conditions whereas the degradation was marginal under the sunlight exposure conditions. The proposed RP-HPLC stability indicating method can be successfully employed in estimation of tablet dosage form in regular QC and stability analysis....
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