Current Issue : January-March Volume : 2013 Issue Number : 1 Articles : 53 Articles
A Reverse phase high performance liquid chromatography method developed for the simultaneous estimation of ambroxol HCl and doxofylline in tablet formulation. The experiment was carried out on C2695 waters HPLC by using empower software. The separation was carried out by X-Terra C18 (150 mm x 4.6, 5μm) column and Ammonium acetate buffer (0.01M, 6.4PH): ACN (60:40) used as a mobile phase in isocratic technique, at a flow rate of 1 ml/min. The detection was carried out at 257nm. The retention time of Ambroxol HCl and Doxofylline were found to be 2.5 and 5.7 min, respectively. The method has been validated as for ICH guidelines for Accuracy, Precision, Linearity and robustness and the results obtained were within the limits. The Linearity for Ambroxol HCl and Doxofylline were found to be in the range of 0.75-4.5 ppm and 10-60 ppm, respectively. The mean recoveries obtained for Ambroxol HCl and Doxofylline were found to be 99.5% and 99.9%, respectively. The Developed method was found to be accurate, precise, selective for simultaneous estimation of Ambroxol HCl and Doxofylline in tablets....
Diclofenac is Non-steroidal anti-inflammatory drugs (NSAIDs) are the group most widely used in human and veterinary medicine, since it is available without prescription for treatment of fever and minor pain. The clinical and pharmaceutical analysis of these drugs requires effective analytical procedures for quality control and pharmacodynamics and pharmacokinetic studies. An extensive survey of the literature published in various analytical and pharmaceutical chemistry related journals has been conducted and the instrumental analytical methods which were developed and used for determination of diclofenac (an aryl acetic acid derivative) in bulk drugs, formulations and biological fluids have been reviewed. This review covers the time period from 1989 to 2012 during which 53 methods including spectroscopic, chromatographic titrimetric methods were reported. The application of these methods for the determination of diclofenac in pharmaceutical formulations and biological samples has also been discussed....
A simple, specific, sensitive and rapid reverse phase high performance liquid chromatographic (HPLC) method for the determination of racecadotril (RCD) was developed and validated. Sample preparation involved simple dissolution, followed by dilution with mobile phase to eliminate any chromatographic solvent effects. RCD was quantitated on a C18 column (4.6 mm i.d. × 300 mm length), using a mobile phase composed of acetonitrile: water (65:35 %v/v) which was delivered at a flow rate of 1.0 mL/min. The method was proven to be linear over a concentration range of 5 to 100 μg/mL with a mean correlation coefficient of 0.9991. The intra-day and inter-day precision (coefficient of variation) were in the range of 0.53% to 0.92% and 0.95% to 1.76%, respectively. The intra-day accuracy (relative error) were in the range of 2.53% to 4.47% and the inter-day accuracy were in the range of 3.11% to 4.92%. The limit of detection (LOD) and the limit of quantification (LOQ) of the developed method were determined to be 0.5 μg/mL and 5 μg/mL, respectively. The developed method was established as a rapid analytical tool as it required short retention time, high precision, sensitivity and small volumes of sample for analysis....
Three simple spectrophotometric methods have been developed for simultaneous estimation of Ibuprofen (IBU) and Famotidine (FAM) from tablet dosage form. Methanol (A.R. grade) was used as solvent. First method, multi-component mode of analysis (Method A), involves the measurement of absorbances at two wavelengths 264.0 nm (λmax of IBU) and 287.0 nm (λmax of FAM). Second method, Derivative spectroscopy (Method B), wavelength selected for quantitation were 287 nm (zero crossing point for IBU) for FAM in zero order derivative mode and 249 nm (zero crossing point for FAM) for IBU in third order derivative mode. Third method, Dual wavelength method (Method C), difference in absorbance at 264 nm and 306.5 nm give direct estimation of IBU in bulk and combined dosage form. The linearity lied between 200-1000 µg/ml and 2-10 µg/ml for IBU and FAM respectively for Method A, 200-500 µg/ml and 4-10 µg/ml for IBU and FAM respectively for Method B and 200-500 µg/ml for IBU for Method C. The accuracy and precision of the methods were determined and validated statically. The proposed methods were found to be rapid, specific, precise, and accurate and can be successfully applied for the routine analysis of Ibuprofen and Famotidine in bulk and combined dosage form....
A novel, simple, accurate, sensitive and reproducible spectroscopic method was developed and validated for the estimation of Rosuvastatin Calcium and Clopidogrel Bisulphate in combined dosage form. The method obeys Beer’s Law in concentration ranges of 4-12 µg/ml for Rosuvastatin Calcium and 30-90 µg/ml Clopidogrel Bisulphate both. The method was validated for linearity, accuracy and precision as per ICH guidelines. The zero crossing point for Rosuvastatin Calcium and Clopidogrel Bisulphate was 242.20 nm and 265.60 nm respectively in methanol. The LOD and LOQ value were found to be 1.86 µg/ml and 5.65 µg/ml for Rosuvastatin Calcium, 4.20 µg/ml and 12.72 µg/ml for Clopidogrel Bisulphate respectively. The accuracy of the method was assessed by recovery studies was found to be 100.23 ± 0.3055 and 99.78 ± 0.3426 for Rosuvastatin Calcium and Clopidogrel Bisulphate respectively. The developed and validated method was successfully used for the quantitative analysis of commercially available dosage forms....
A new simple, sensitive, rapid, accurate, precise and economical dual wavelength Spectrophotometric method for the simultaneous determination of Levosulpiride (LEVO) and Pantoprazole sodium (PANTO) in combined capsule dosage form was developed. The dual wavelength Spectrophotometric method was based the absorbance of the solutions were measured at 232.32 nm (λ1), 295 nm (λ2¬), 264 nm (λ3), 270 nm (λ4) for the estimation of both the drugs. The quantitative determination of LEVO is carried out by measuring absorbance difference between 232.32 nm and 295 nm and for PANTO by absorbance difference at 264 nm and 270 nm. The linearity was obtained in the concentration range of 15-90 μg/ml for LEVO and 8-48 μg/ml for PANTO The mean recovery was 98.44 –100.36% and 98.33 – 101.25% for LEVO and PANTO respectively. The results of analysis have been validated statistically as per ICH guidelines....
A new simple, sensitive, rapid, accurate, precise and economical first derivative Spectrophotometric method for the simultaneous determination of Levosulpiride (LEVO) and Pantoprazole sodium (PANTO) in combined capsule dosage form was developed. The derivative Spectrophotometric method was based on the determination of both the drugs at their respective zero crossing point (ZCP). The first order derivative spectrums were obtained in distilled Water and the determinations were made at 250.38 nm (ZCP of PANTO) for LEVO and 267.34 nm (ZCP of LEVO) for PANTO. The linearity was obtained in the concentration range of 5-45 μg/ml for LEVO and 5-45 μg/ml for PANTO The mean recovery was 97.73-101% and 99.25 – 99.75% for LEVO and PANTO respectively. The results of analysis have been validated statistically as per ICH guidelines....
A simple, precise, accurate and reproducible spectrophotometric method has been developed for simultaneous estimation of Paracetamol (PCM) and Pamabrom (PAM) by employing first order derivative zero crossing method in 0.1 N NaOH. The first order derivative absorption at 258 nm (zero cross point of Paracetamol) was used for quantification of Pamabrom and 280 nm (zero cross point of Pamabrom) for quantification of Paracetamol. The linearity was established over the concentration range of 2-12 µg/ml and 5-30 µg/ml for Paracetamol and Pamabrom with correlation coefficient r2 0.9977 and 0.9978, respectively. The mean % recoveries were found to be in the range of 99.33 % – 101.01 % and 98.96 % – 100.67 % for Paracetamol and Pamabrom, respectively. The proposed method has been validated as per ICH guideline and successfully applied to the estimation of Paracetamol and Pamabrom in bulk and in synthetic mixture....
Avaleha is a traditional Ayurvedic oral herbal formulation consisting of five herbs, Vasaka (Adhatoda vasica Nees.), Pippali (Piper longum Linn.), Sugar, Ghee and Honey. It is available as a popular proprietary, from most manufacturers of ayurvedic drugs. A selective, precise and accurate High Performance Thin Layer Chromatography (HPTLC) method has been developed for the simultaneous quantification of Vasicine and Piperine in avaleha as well as its bulk drug. The method employed TLC aluminum plate precoated with silica gel 60 F254 as a stationary phase. The solvent system consists of Dioxane: Toluene: Ethyl acetate: Methanol: Ammonia (2.5:2:1:1:0.3 % v/v). This system was found to give compact spot for Piperin and Vasicine. Densiometric analysis was carried out in the absorbance mode at 285 nm. The linear regression analysis data for the calibration plot showed good linear relation with r = 0.992 and 0.993 with respect to peak area for Vasicine and Piperine respectively, in concentration range 2-10 µg/spot. The method was validated for precision, recovery, Limit of Detection and Limit of Quantification. The proposed HPTLC method was found to be simple, precised and accurate and can be used for the quality control of the raw materials as well as formulations....
A simple, sensitive and specific UV spectrophotometric method was developed for the estimation of MFNC in tablet dosage form. According to Indian pharmacopoeia and British pharmacopoeia MFNC freely soluble in 0.1 M NaOH. So UV spectrophotometric estimation was done in 0.1 M NaOH as solvent. The optimum conditions for the analysis of the drug were established. The wavelength maxima (λ max) for Mefenamic acid were found to be 285 nm in 0.1 M NaOH. Beer’s law was obeyed in the concentration range of 5‐30 µg/ml. The slope, intercept, correlation coefficient, detection and quantization limits were also calculated. The proposed method has been applied successfully for the analysis of the drug in pure and in its tablets dosage forms....
A precise, simple, accurate and specific ratio derivative UV spectrophotometric method were developed and validated for routine quantitation of Tamsulosin Hydrochloride (TAM) and Finasteride (FINA) in combined dosage form. The first derivative ratio spectrophotometric method, zero order spectra of Tamsulosin Hydrochloride and Finasteride were quite parallel and overlapping. Hence first derivative ratio spectrophotometry method was possible for simultaneous estimation of these drugs. Also matrix effect can be reduced by this method. In first derivative ratio spectra, estimation was done at peak minima of Tamsulosin Hydrochloride and Finasteride at 235.92 nm and 253.94 nm respectively. The calibration graphs were linear in the concentration range of 1.6-8.0 μg/mL for Tamsulosin Hydrochloride and 10-60 μg/mL for Finasteride with mean recoveries of 98.05-100.62 % and 98.02-100.79 % for Tamsulosin Hydrochloride and Finasteride respectively....
Dihydroartemisinin is a newer approach to the treatment of Malaria. Here, DHA has no strong UV absorbing groups and it is optically alive. It converts from α-DHA to β-DHA in organic solvents which can be estimated by RP-HPLC. The DHA was determined by RP-HPLC method by using Kromasil C18 (250 mm x 4.6 mm i.d., 5 µm particle size) column. A mobile phase composed of acetonitrile, methanol and water in proportion of 60:20:20 v/v, at flow rate of 0.8 ml/min was used for the separation. Detection was carried out at 215 nm. Method was 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 pharmaceutical formulations with good accuracy and precision. The method herein described can be employed for quality control and routine analysis of drugs in pharmaceutical formulations....
A Simple, Sensitive and Accurate Reversed Phase High Performance Liquid Chromatographic (RP HPLC) method for analysis of Drospirenone (DROSP) and Ethinyl Estradiol (ETE) drugs in tablet dosage form. Isocratic elution at a flow rate of 1.0ml/min was employed on a symmetry C18 (150x4.6mm, 5μm in particle size) at ambient temperature. The mobile phase consisted of Acetonitrile: Water (70:30). The UV detection of Wave length was 210 nm and 20μl sample was injected. The retention time for DROS was 2.78 min and ETE was 2.33 min. The % Recovery were found to be 99.28%-102% for DROSP and 99.33% - 98.64% for ETE. The proposed method is validated for Linearity, Accuracy and Precision, Limit of Detection (LOD) and Limit of Quantification (LOQ) as per the guidelines ofInternationational Conference on Harmonization (ICH)....
A simple, precise and RP-HPLC (reverse phase – high performance liquid chromatographic) method was developed and validated for the simultaneous determination of lercanidipine HCl (LDPH) and atenolol (AT) in pharmaceutical dosage form. The method involves the use of easily available inexpensive laboratory reagents. The separation was achieved on an Phenomenex Luna® C18 column with a particle size 5 µm, length 250 mm and internal diameter (i.d.) 4.6 mm with isocratic flow. The mobile phase at a flow rate of 1 mL/min consisted of 10 mM potassium dihydrogen phosphate (pH adjusted to 3.1 with 0.1 M ortho-phosphoric acid) and acetonitrile (65:35; v/v). A linear response was observed over the concentration range 2–18 µg/mL of LDPH and the concentration range 10–90 µg/mL of AT. Limit of detection and limit of quantitation for LDPH were 0.5 and 1.5 µg/mL, respectively and for AT were 1 and 3 µg/mL, respectively. The method was successfully validated in accordance to ICH guidelines acceptance criteria for system suitability, specificity, linearity, accuracy, precision and robustness. The analysis concluded that the method was selective for simultaneous estimation of LDPH and AT....
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 Febuxostat and Diclofenac potassium. Effect of different experimental parameters and various particulate columns on the analysis of these analytes was evaluated. The method showed adequate separation for Febuxostat and Diclofenac potassium and best resolution was achieved with Enable analytical C18, (250 mm × 4.6 mm × 5 μm) using acetonitrile-methanol-water (30:30:40, v/v; pH adjusted to 5.0 with TEA and o-phosphoric acid) as a mobile phase at a flow rate of 1 ml/min and wavelength of 280 nm. The calibration curves were linear over the concentration ranges of 4-24 μg/ml for Febuxostat and 10-60 μg/ml for Diclofenac potassium. The limit of detection (LOD) and limit of quantification (LOQ) for Febuxostat were 0.389 and 1.18 μg/ml while for Diclofenac potassium were 0.843 and 2.557 μg/ml, respectively. All the analytes were separated in less than 6.0 min. The proposed method could be applied for routine laboratory analysis of Febuxostat and Diclofenac potassium in pharmaceutical dosage form....
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 Ofloxacin and Flavoxate hydrochloride. Effect of different experimental parameters and various particulate columns on the analysis of these analytes was evaluated. The method showed adequate separation for Ofloxacin and Flavoxate hydrochloride and best resolution was achieved with Kromasil analytical C18, (250 mm × 4.6 mm × 5 μm) using acetonitrile-methanol-water (30:20:50, v/v; pH adjusted to 3.0 with TEA and o-phosphoric acid) as a mobile phase at a flow rate of 1ml/min and wavelength of 322 nm. The calibration curves were linear over the concentration ranges of 10-60 μg/ml for Ofloxacin and 10-60 μg/ml for Flavoxate hydrochloride. The limit of detection (LOD) and limit of quantification (LOQ) for Ofloxacin were 0.239 and 0.724 μg/ml while for Flavoxate hydrochloride were 0.496 and 1.506 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 Ofloxacin and Flavoxate hydrochloride in pharmaceutical dosage form....
A Rapid, sensitive and economical high performance liquid chromatographic method for determination of Linagliptin has been developed. The chromatography system containing reverse phase C18 Column (250×4.6mm, 5µm) with a mixture of Methanol: Water in a ratio of 40:60 with flow rate of 1.0 ml min-1. OPA was used as buffer to maintain the pH 3 of mobile phase. UV detector was used at 238 nm and 20µl sample was injected. The method was validated as per ICH guideline. The retention time of Linagliptin was found to be 7.3 min. The calibration curve is linear in the range of 2-10 µg/ml. The percentage RSD for precision and accuracy of method was found to be less than 2 %. The lower limit of detection (LOD) and limit of quantification (LOQ) was 0.015 and 0.04 ppm respectively. Recovery studies from tablet were between 98.76, 100.88, and 101.98%. The method can be successfully used for routine analysis of Linagliptin form tablets formulation....
Dihydroartemisinin is a newer approach to the treatment of Malaria. It is available in the combination with Piperaquine Phosphate in various dosage forms. Here, DHA has no strong UV absorbing groups and it is optically alive. It converts from α-DHA to β-DHA in organic solvents. Simultaneous estimation of these both drug is not possible, therefore these drugs are estimated separately in their formulation. The DHA was determined by RP-HPLC method by using Kromasil C18 (250 mm x 4.6 mm i.d., 5 µm particle size) column. A mobile phase composed of acetonitrile, Methanol, Water in proportion of 60:20:20 v/v, at flow rate of 0.8 ml/min was used for the separation. Detection was carried out at 215 nm. PQP was determined by using Acetonitrile, 0.1 mM phosphate buffer, 1 ml triethylamine (pH-2.5 is adjusted with o-phosphoric acid). 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 pharmaceutical formulations with good accuracy and precision. The method herein described can be employed for quality control and routine analysis of drugs in pharmaceutical formulations....
A novel, precise, accurate, rapid and cost effective isocratic reversed-phase high performance liquid chromatographic/ultraviolet (RP-HPLC/UV) method was developed, optimized and validated for estimation of Piperaquine phosphate. Effect of different experimental parameters and various particulate columns on the analysis of these analytes was evaluated. PQP was determined by using Acetonitrile, 0.1mol L-1 phosphate buffer, 1 ml triethylamine (pH-2.5 is adjusted with o-phosphoric acid) as a mobile phase at a flow rate of 1 ml/min and wavelength of 322 nm. The calibration curves were linear over the concentration ranges of 10-80 μg/ml. The limit of detection (LOD) and limit of quantification (LOQ) for PQP were 0.0323 μg/ml and 0.0981 μg/ml respectively. The analyte was eluted in less than 5.0 min. The proposed methods have been applied successfully to the analysis of cited drug either in pure form or in pharmaceutical formulations with good accuracy and precision. The method herein described can be employed for quality control and routine analysis of drugs in pharmaceutical formulations....
UV Spectrophotometric method has been developed for simultaneous estimation of Cefpodoxime proxetil (CPD) and Levofloxacin hemihydrate (LVX) in bulk drug and in pharmaceutical formulation. This method utilizes methanol as a solvent and λmax of Cefpodoxime proxetil and Levofloxacin hemihydrate selected for analysis were found to be 235 nm and 300 nm respectively. Linearity was observed in the concentration range of 2-10 μg/ml for Cefpodoxime proxetil and 2.5-10.5 μg/ml for Levofloxacin hemihydrate. The method was validated statistically and by recovery studies. The mean % recovery was 99.03–100.63 % and 99.56–100.27 % for Cefpodoxime proxetil and Levofloxacin hemihydrate respectively. Amounts of drug estimated from tablet formulation were in good agreement with label claim. The results were found to be within acceptance criteria according to ICH guideline. This method was simple, rapid, accurate and sensitive. Hence, can be used for quality control of combined pharmaceutical dosage forms....
UV Spectrophotometric method has been developed for simultaneous estimation of Paracetamol (PCM) and Pamabrom (PAM) in bulk drug and in laboratory mixture. This method utilizes 0.1 N NaOH as a solvent and λmax of Paracetamol and Pamabrom selected for analysis was found to be 257 nm and 280 nm respectively. Linearity was observed in the concentration range of 2-12 μg/ml for Paracetamol (r2=0.999) and 5-15 μg/ml for Pamabrom (r2=0.999). The method was validated statistically and by recovery studies. The mean % recovery was 99.63-100.83% and 98.70-101.98% for Paracetamol and Pamabrom 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....
The present research work aims to develop a simple, sensitive, accurate and reproducible method for the simultaneous estimation of Alprazolam and Omeprazole by two different spectroscopic method viz, Simultaneous equation Method (Vierodt's method) (Method-A) and Q-Absorption method (Method-B). Absorbance maxima for Alprazolam and Omeprazole were found to be at 221 nm and 301 nm respectively for method-A, and Iso-absorptive point for both drugs was found to be 261.2 nm for method-B by using Methanol as a solvent. Absorption maxima of Omeprazole at 301nm, was taken as second wavelength for determination by method-B. Linearity for both the methods was observed in concentration range of 1-5 µg/ml for both drug Alprazolam and Omeprazole. The correlation coefficients for both the methods obtained were near to 1. The accuracy of both methods was evaluated by recovery studies and recovery results were obtained from 98 % to 102% for both the methods and the relative standard deviations below 2% were achieved. Validation was done as per ICH guidelines. Proposed methods can estimate Alprazolam and Omeprazole simultaneously in combined dosage form without the interference of common excipients....
A simple, economic, selective and precise stability-indicating RP-HPLC method has been developed and validated for analysis of Beclomethasone dipropionate(BD),an anti inflammatory, in pharmaceutical dosage form. Reversed-phase chromatography was performed on a ACE C18, 5μ, 15 cm × 4.6 mm column with ACN–water, 60:40 (%, v/v), as mobile phase at a flow rate of 1.0 ml/min. Detection was performed at 238 nm .The drug was subjected oxidation, hydrolysis, heat and light to apply stress conditions. The drug was found to be hydrolyzed in acidic and alkaline conditions. We had also found the degradation under photolytic stress condition. The developed method was able to separate all degradation product generated under forced degradation studies and drug peak was eluted at 7.9 min. The developed method was validated as per ICH guideline for the parameters such as specificity, linearity, precision, accuracy, limit of detection, limit of quantification and found to be satisfactorily. Linear regression analysis data for the calibration plot showed there was a good linear relationship between response and concentration in the range 2-16μg/ml the regression coefficient was 0.9998 and the linear regression equation was y = 12413x + 1979.2. The detection (LOD) and quantification (LOQ) limits were 0.039 and 0.12μg/ml respectively....
An accurate, precise, sensitive, specific, robust, rugged simple and cost effective UV spectroscopic method has been developed for estimation of Ketoconazole (KZ) in bulk and tablet dosage form using methanol as a solvent. The degradation studies of KZ were studied as per guidelines of International Conference on Harmonisation (ICH). The λ max of KZ was found to be 203 nm. The method exhibited high accuracy and sensitivity, in a linear range of 2-7 µg/ml. The Limit of Detection (LOD) and Limit of Quantification (LOQ) were found to be 0.003 and 0.064 µg/ml respectively. All the concentrations were linear with the absorbance having a correlation coefficient 0.9956. The regression equation of calibration curve was found to be y = 0.1502x + 0.4168. The accuracy was found to be 99.17 ± 0.601026% with percentage recovery of 99.44 ± 0.35746%. Sample solution was stable for five hours, so that it could be concluded that the developed method would be applicable for the analysis for the KZ in bulk as well as in pharmaceutical formulations....
A simple, sensitive and specific UV spectrophotometric method was developed for the estimation of FLVX in tablet dosage form. According to British pharmacopeia FLVX is freely soluble in water. So UV spectrophotometric estimation was done in distilled water as solvent. The optimum conditions for the analysis of the drug were established. The wavelength maxima (λmax) for Flavoxate hydrochloride were found to be 317 nm in distilled water. Beer’s law was obeyed in the concentration range of 5‐30 µg/ml. The slope, intercept, correlation coefficient, detection and quantification limits were also calculated. The proposed method has been applied successfully for the analysis of the drug in pure and in its tablets dosage forms....
A new absorption ratio method was developed and validated for the determination of Paracetamol and pamabrom in Bulk and binary mixture. The method involved Q-absorption analysis based on the measurement of absorbance at two wavelengths, i.e λmax of Pamabrom (279.0 nm) and Iso-absorptive point of both drugs (265.0 nm). Beer’s law was obeyed in the concentration range between 4-14 μg/ml for Paracetamol and 2-12 μg/ml for Pamabrom. 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....
A simple and sensitive spectrophotometric method has been developed for simultaneous Determination of Paracetamol and Pamabrom in a binary mixture. In the proposed method, the absorbances were measured at 245.0 nm and 279.0 nm corresponding to the absorbance maxima of Paracetamol and Pamabrom in Dist. Water respectively. Linearity range was observed in the concentration range of 4-14μg/ml for Paracetamol and 2-12 μg/ml for Pamabrom. Concentration of each drug was obtained by using the absorptivity values calculated for both drugs at two wavelengths, 245.0 nm and 279.0 nm and solving the simultaneous equation. Developed method was applied to laboratory mixture. The method was validated statistically and recovery study was performed to confirm the accuracy of the method. The method was found to be rapid, simple, accurate and precise....
The simple accurate and sensitive UV spectrophotometric method has been developed for the quantitative estimation of Darunavir in bulk and its pharmaceutical formulation. In this method 70% methanol was used as solvent. Darunavir shows maximum absorbance at 262.5 nm and obeys Beer-Lamberts law in the concentration range of 2-25 µg/ml. The linearity was observed in concentration range of 2-25 µg/ml. The method was validated statistically for accuracy, precision and sensitivity....
A simple, sensitive and specific UV Spectrophotometric method was developed for the estimation of Bromfenac sodium in pharmaceutical formulation. The wavelength maximum (λ max) for Bromfenac sodium was found to be 268.0 nm. Beer’s law was obeyed in the concentration range of 4-20 mcg mL‐1 with 13.003 × 103 L mol‐1 cm‐1, slope, intercept, correlation coefficient, detection and quantization limits were also calculated. The proposed method has been applied successfully for the analysis of the drug in pure and in its pharmaceutical formulation....
A simple, sensitive, specific, spectrophotometric method was developed for the detection of Phenytoin Sodium (PS). The optimum condition for the analysis of the drug was studied. PS was subjected to stress degradation under different conditions recommended by the International Conference on Harmonization (ICH). The samples so prepared were used for degradation studies by using the developed method. The absorbance maxima (λmax) of the PS was found to be 202.40 nm. The method reveals high sensitivity, with linearity in the 2 to 10 µg/ml range. The lower limit of detection was found to be 0.05 µg/ml and the limit of quantification was found to be 0.13 µg/ml. All the calibration curves demonstrated a linear relationship between the absorbance and concentration, with the correlation coefficient higher than 0.99. The regression equation of the curve was Y=0.0963x + 0.2137. The precision of the method was found to be 0.739 ± 0.002733. The %recovery was found to be 100.234. The sample solution was stable for 7 days in refrigerator....
A new, trouble-free, economic, reproducible and accurate stability indicating assay method using UV-Visible spectrophotometer for the quantitative evaluation of Tinidazole in bulk and pharmaceutical dosage forms has been developed. 0.1 N HCl was chosen as the solvent system for developing assay method. The absorbance maximum (λmax) for Tinidazole was found to be 277 nm. The responses were linear in the range of 10-80 μg/ml. The regression equation of the calibration graph and correlation coefficient were found to be y = 0.030 x + 0.022 and 0.999 respectively. The method was validated statistically and found to be accurate with 99.71±0.11203 % recovery), precise at intraday (0.0923 %RSD) and inter day (0.4825 %RSD), specific (99.86 ± 0.076 %). LOD and LOQ were found to be 0.04 μg/ml and 0.1 μg/ml respectively. This method was precisely determining the concentration of Tinidazole in marketed brand namely Tiniba 300 and the results were in good agreement with the label claim....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical dual wavelength spectrophotometric method for the simultaneous determination of Doxofylline and Ambroxol Hydrochloride in pure and bulk form. All these methods utilize Distilled Water as a solvent. In Dual wavelength method, the determination of Doxofylline was carried out at the absorbance difference between 240.60 nm and 245 nm and of Ambroxol Hydrochloride at the absorbance difference between 306.60 nm and 315 nm. The results of analysis have been validated statistically. The proposed methods were found to be simple and sensitive for the routine quality control application of Doxofylline and Ambroxol Hydrochloride in pure and bulk form. The results were found to be within acceptance criteria according to ICH Q2 R1 guideline....
To study effect of homogenization of drug & excipients mainly cross checking method is utilized that in every case of evaluation study there will be same result will be produced & it also reproducible too, that there will be only one strength of API throughout the formulation so only one result is reflect in every methods. If there are different results means that there will be no homogenization of drug & excipients...
Cancer is the major lethal disease all around the world, despite huge progress in the understanding, treatment and prevention, the oncology diseases remain leading mortality-rate reason in the well-developed countries. Since FTIR- spectroscopy can distinguish normal and tumor cells as well as different levels of malignancy, in principle can be calculated the dissemination level of tumor premalignant status through biopsy in definite space of tumor heart and to be analyzed resection frames for individual patient. Exact tumor/ premalignant classification are significant for successful therapy determination, where incorrect definition can lead to wrong prognosis. Infrared spectroscopy is a potentially new method for cancer diagnosis, due to the sensitivity of the technique to alterations in cellular biochemistry which accompany disease stages. Infrared radiation is absorbed by tissues, fluids and cells to promote vibration of the covalent bonds of molecules within the sample. The wavelength of infrared radiation which is absorbed depends upon the nature of the covalent bond and the strength of any intermolecular interactions. The infrared spectrum of a sample is therefore a biochemical fingerprint. As the biochemistry of cells, tissues and fluids must change during disease (there can be no disease without abnormal biochemistry) then the biochemical fingerprint of the cells, tissues and fluids should be altered when a disease is present....
A sensitive, selective, precise, accurate high-performance thin layer chromatography (HPTLC) method was developed and validated for analysis of Flupentixol and Melitracen both as a bulk drug and in formulations. The analyte was separated on aluminium plates precoated with silica gel 60 F254. The mobile phase was consisted of ethyl acetate : methanol : ammonia in a proportion of (7.0:3.0:0.1) (v/v/v). Densitometric analysis of Flupentixol and Melitracen was carried out in the absorbance mode at 265 nm.This system was found to give compact spots for Flupentixol and Melitracen RF value of (0.73 ± 0.01 and 0.59 ± 0.01 for six replicates). The method was validated for linearity, precision, accuracy, specificity, LOD, LOQ, robustness, and ruggedness. Response was a linear function of Flupentixol concentration in the range of 20–120 ng/spot with significantly high value of correlation coefficient r2 = 0.99945 and Melitracen 100-600 ng/spot with significantly high value of correlation coefficient r2 = 0.99931. The limit of detection and quantification for Flupentixol were 7.04 and 21.22 ng/spot, respectively and for Melitracen limit of detection and quantification were 9.3 and 28.38 ng/spot respectively. The drug content for marketed formulation was found to be 98.3 % for Melitracen & 101.36 % Flupentixol for six replicate determinations. The established method enabled accurate, precise, and rapid analysis of Flupentixol and Melitracen in bulk as well as pharmaceutical formulation....
A simple, rapid, precise and accurate HPLC method for differentiating aspirin from the derivatives of Aspirin synthesized. The instrument used for carrying out HPLC was Shimadzu LCVP2010C integrated system equipped with quaternary gradient pump, Column utilized Kromasil C18 (180 X 4.6 mm), 5 µm, and the detection made possible using UV-Vis detector at a wavelength of 277 nm and the mobile phase employed was acetonitrile: methanol 60:40 (v/v). The Rt (Retention time) of aspirin was found to be 4.303 and that of derivatives as SR01- 2.543, SR02 -3.797, SR03-4.133, SR05-2.553, SR06-3.277, SR07-2.903. Proving the fact that the aspirin and its derivatives synthesized are pure....
Low back pain and spasticity is a leading reason for primary care visits. Many treatment options are available, but some lack scientific support. The aim of this review was to discuss potential therapies available to treat spasticity and low back pain which is the most common muscle skeletal disorders along with review of various chromatographic method available for their detection form various pharmaceutical formulations and from biological samples. It also suggest about the other alternate potential therapy to treat spasticity and low back pain and benefits of muscle relaxants commonly prescribed for the management of back pain and spasticity....
The purpose of research is to develop a new UV method for Simvastatin in bulk drugs and pharmaceutical formulations(tablets). The assays were linear over the concentration range of 2.5-15 µg/ml and reproducible. Linear relationship with good correlation coefficients 0.999 were found between absorbance and corresponding concentrations of drug. The reliability and performance of proposed methods was validated statistically the percentage recovery ranged from 98.21-101.34% respectively. This new method has been successfully applied in the assay of Simvastatin tablets and has the advantages of speed, high sensitivity, lower limit of detection and can be automated....
A simple and sensitive spectrophotometric method has been developed for simultaneous determination of Meropenem and Sulbactam in a binary mixture. In the proposed method, the absorbances were measured at 296.0 nm and 258.0 nm corresponding to the absorbance maxima of Meropenem and Sulbactam in 0.05 N Sodium Hydroxide respectively. Linearity range was observed in the concentration range of 5-25 μg/ml for Meropenem and 2.5-12.5 μg/ml for Sulbactam. Concentration of each drug was obtained by using the absorptivity values calculated for both drugs at two wavelengths, 296.0 nm and 258.0 nm and solving the simultaneous equation. Developed method was applied to laboratory mixture. The method was validated statistically and recovery study was performed to confirm the accuracy of the method. The method was found to be rapid, simple, accurate and precise....
To survive in demanding market and still to be successful, it is necessary to achieve high level product quality. It is derived from careful attention to a process design, control of the process, and in-process and end-product testing. Due to the complexity of today''s medical products, routine end-product testing alone often is not sufficient to assure product quality, So for this, the manufacturing process need to be controlled as integrated level and a good understanding of the processes and their performance is important. The process breaking down each individual steps, determine critical and non-critical steps. Every critical step should be scientifically planned and executed and documented appropriately in order to have effective and efficient. So here we go on the Prospective type of process validation of Loperamide Hydrochloride B.P 2 mg tablets, Initial three consecutive process batches of same size method, equipment and validation criteria were taken. The feedback indicated that this process is implemented as intended to use and data provide high degree of phenomenal assurance that the manufacturing process produce product that meet its predetermined specification and quality attributes....
A simple, accurate and economical UV-Spectrophotometric method has been developed for routine analysis of Moxifloxacin Hydrochloride (MOX) in ophthalmic solution. In saline phosphate buffer (PBS) pH 7.4 and simulated tear fluid (STF) pH 7.4, MOX showed maximum absorbance at 287.0 nm. In this method MOX obeyed linearity in the concentration range of 2 - 20 μg/mL (r2 > 0.99). Proposed methods were applied for ophthalmic solution and amounts of MOX estimated by this method were 99.93 ± 1, 99.36 ± 1 in phosphate buffer and in simulated tear fluid respectively. Methods were validated statistically....
A simple, rapid and precise reverse phase high performance liquid chromatography method was developed for the analysis of Almotriptan. Chromatographic separation of Almotriptan was performed by using a waters C18 column (250 x 4.6 mm, 5 µm) as stationary phase with a mobile phase comprising of Methanol, ACN, Acetic acid 75:20:5 (v/v/v) at a flow rate of 1.0 ml/min and UV detection at 231 nm. The linearity of Almotriptan is in the range of 20 ppm to 120 ppm. The limit of detection for Almotriptan was found to be 0.2 ppm. The proposed method was found to be accurate, precise and rapid for the analysis of Almotriptan. Degradation test was also performed....
A new, simple and rapid spectrophotometric method was developed for determination of Acebutolol Hydrochloride (ACE) in pure and pharmaceutical formulations. The solvent and wavelength of detection were optimized in order to maximize the sensitivity of the proposed method. Parameters such as linearity, precision, accuracy, limit of detection, limit of quantification and content uniformity were studied according to the International Conference on Harmonization (ICH) Guidelines. The linearity was established between the concentration ranges of 2 – 12 µg/ml. The intra- and inter-day relative standard deviation (RSD) was less than 2 %. Limits of detection and quantification were determined as 0.23 and 0.69 µg/ml, respectively. The mean recovery value of Acebutolol HCl was 99.50% for pharmaceutical preparation. The method was applied for the quality control of commercial Acebutolol HCl dosage form to quantify the drug and to check the formulation content uniformity....
A simple, economical, accurate, and, and reproducible spectrophotometric method for the simultaneous estimation of Nebivolol and Hydrochlorothiazide in combined dosage forms. The method was based on dual wavelength data processing program (dual wavelength Spectrophotometry or DW Spectrophotometry). In the proposed method, Absorbance spectrum of pure NEB was scanned in the spectrum basic mode. NEB showed some absorbance value at 286.0 nm while it does not show any absorbance value at 315.5 nm. The absorbance value at 315.5 nm is due to HTZ only in the combined mixture of both drugs. Wavelength 315.5 nm was selected for the measurement of HTZ and 286.0 nm for NEB. Linearity range was observed in the concentration range of 4-24 μg/ml for Nebivolol and 10-60 μg/ml for Hydrochlorothiazide. Developed method was successfully applied for simultaneous determination of NEB and HTZ in combined dosage forms that are available in the market. The method was validated statistically and recovery study was performed to confirm the accuracy of the method. The method was found to be rapid, simple, accurate and precise....
A Simple, accurate, precise and economical procedure for simultaneous estimation of Amlodipine besylate and Indapamide in combined tablet dosage form by UV spectrophotometry, using Multicomponent mode of analysis. The method is based upon determination of Amlodipine besylate at 238 nm and Indapamide at 242 nm in methanol at their respective λmax. Developed method was validated according to ICH guidelines. The calibration graph follows Beer’s law in the range of 5 to 25 μg/ml for Amlodipine besylate and 2 to 8 μg/ml for Indapamide with R square value greater than 0.999. Accuracy of all methods was determined by recovery studies and showed % recovery between 99 to 103 %. Intraday and interday precision was checked for all methods and mean %RSD was found to be less than 2 for all the methods. The methods were successfully applied for estimation of Amlodipine besylate and Indapamide in marketed formulation....
A simple, precise and accurate UV Spectrophotometric method have been developed for the simultaneous estimation of Cefixime and Ornidazole in tablet dosage form. The solvent used is 0.1N NaOH. The λmax of Cefixime and Ornidazole was found to be 287 and 318nm. Various validation parameters such as linearity, accuracy, precision were determined as per ICH guidelines. The linearity range was found to be 5-25µg/ml and 5-25µg/ml for Cefixime and Ornidazole respectively. Recovery studies were also carried out and the percent recovery was found to be in the range of 98-102%.Therefore the proposed method can be successfully applied to the routine analysis of both the drugs in quality control laboratories....
Area under curve and dual wavelength Spectrophotometric methods have been developed for simultaneous estimation of Cetrizine hydrochloride and Phenyelphrine hydrochloride in bulk drug and in pharmaceutical formulation. All these methods utilizes water as a solvent. In Area Under Curve the wavelength ranges of 225-235nm and 267-277nm were selected as analytical wavelength ranges for the determination of area of both the drugs in pure and in combined formulation. In Dual wavelength method, the absorbance difference was determined within 233nm and 254nm for the the determination of Cetrizine hydrochloride, and absorbance difference within 250nm and 265nm for the determination of Phenylephrine hydrochloride. The results of analysis of all methods have been validated statistically. Lower value of % RSD indicates that these methods were simple, rapid and accurate, hence can be used for routine simultaneous estimation of these drugs in formulations. The results were found to be within acceptance criteria according to ICH Q2 R1 guideline....
Zero order, Area under curve and dual wavelength Spectrophotometric methods has been developed for simultaneous estimation of Pantoprazole sodium and Levosulpiride in bulk drug and in pharmaceutical formulation. All these methods utilizes methanol as a solvent. In Zero order spectroscopy 291nm and 289nm were selected as analytical wavelength for determination of both the drugs simultaneously. In Area Under Curve the wavelength ranges of 283–298 nm and 282–297 nm were selected as analytical wavelength ranges for the determination of area of both the drugs in pure and in combined formulation. In Dual wavelength method, the absorbance difference was determined within 287nm and 295nm for the the determination of Pantoprazole, and absorbance difference within 286 nm and 292 nm for the determination of Leveosulpiride. The results of analysis of all methods have been validated statistically. Lower value of % RSD indicates that these methods were simple, rapid and accurate, hence can be used for routine simultaneous estimation of these drugs in formulations. The results were found to be within acceptance criteria according to ICH Q2 R1 guideline....
First order, Area under curve and dual wavelength Spectrophotometric methods has been developed for simultaneous estimation of Montelukast sodium and Acebrophylline in bulk drug and in pharmaceutical formulation. All these methods utilizes methanol as a solvent. In First order spectroscopy 236.4 nm and 334.4 nm were selected as ZCP (zero crossing point) for determination of both the drugs simultaneously. In Area Under Curve the wavelength ranges of 277-287 nm and 270-280 nm were selected as analytical wavelength ranges for the determination of area of both the drugs in pure and in combined formulation. In Dual wavelength method, the absorbance difference was determined within 244 nm and 254 nm for the determination of Montelukast sodium, and absorbance difference within 265 nm and 285 nm for the determination of Acebrophylline. The results of analysis of all methods have been validated statistically. Lower value of % RSD indicates that these methods were simple, rapid and accurate, hence can be used for routine simultaneous estimation of these drugs in formulations. The results were found to be within acceptance criteria according to ICH Q2 R1 guideline....
Four simple, sensitive, rapid, accurate and precise simultaneous UV-spectrophotometric methods have been developed and validated for the estimation of Cilnidipine and Telmisartan in combined tablet dosage form. The first method is based on simultaneous equation, 240 (λ max of Cilnidipine) and 296 (λ max of Telmisartan) were selected for the determination of Cilnidipine and Telmisartan respectively in methanol. The principle for second method, AUC curve method is “the area under two points on the mixture spectra is directly proportional to the concentration of the component of interest”. The area selected were 230 to 254 nm and 275.2 to 313 nm for determination of Cilnidipine and Telmisartan respectively. Third method is Dual wavelength in which Cilnidipine was determined by plotting the difference in absorbance at 244 and 291.4 nm (difference is zero for Telmisartan) against the concentration of Cilnidipine. Similarly for the determination of Telmisartan, the difference in absorbance at 284.2 and 346 nm (difference is zero for Cilnidipine) was plotted against the concentration of Telmisartan. The fourth method is based on first order derivative spectroscopy, wavelengths 272.4 nm (ZCP of Telmisartan) and 240.6 nm (ZCP of Cilnidipine) were selected for the estimation of the Cilnidipine and Telmisartan, respectively. All the methods were obeyed Beer’s law. The results of analysis have been validated statistically and by recovery studies. Statistical comparisons prove that there is no significant difference between all this methods. The proposed methods can be successfully applied in routine work for the determination of Cilnidipine and Telmisartan in combined dosage form....
A simple and precise visible spectrophotometric method was developed for the determination of lidocaine hydrochloride in bulk and pharmaceutical preparations based on the formation of green colored molecular complex with sodium nitroprusside in presence of hydroxyl amine hydrochloride under alkaline conditions and exhibiting λmax at 401 nm. The Regression analysis of Beer’s Law plot showed good correlation in a general concentration range of 10-50µg/ml with correlation coefficient (r = 0.998). The proposed method is validated with respect to accuracy, precision, and linearity, limit of quantification and limit of detection. The suggested procedure is successfully applied to the determination of the drug in pharmaceutical preparation, with high percentage recovery of 100%, 98.19%, 99.12%. The results of analysis have been validated according to ICH guidelines. The results are found satisfactory and reproducible. The method is applied successfully for the estimation lidocaine hydrochloride in tablet form without the interference of excipients....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical derivative spectroscopic method for the simultaneous determination of Eperisone hydrochloride (EPE) and Diclofenac sodium (DIC) in synthetic mixture. Derivative spectroscopy offers a useful approach for the analysis of drugs in mixtures. In this study a first-derivative spectroscopic method was used for simultaneous determination of Eperisone hydrochloride and diclofenac sodium using the zero-crossing technique. The measurements were carried out at wavelengths of 281 nm and 225 nm for Eperisone hydrochloride and Diclofenac sodium respectively. The method was found to be linear (r2>0.996) in the range of 2- 16 μg/ml for Eperisone hydrochloride at 281 nm. The linear correlation was obtained (r2>0.999) in the range of 2-16 μg/ml for Diclofenac sodium at 225 nm. The limit of determination was 0.3930 and 0.4095 μg/ml for Eperisone hydrochloride and Diclofenac sodium respectively. The limit of quantification was 1.1911 and 1.2409 μg/ml. The method was successfully applied for simultaneous determination of Eperisone hydrochloride and Diclofenac sodium in binary mixture....
Three-wavelength spectrophotometric method has been developed for the simultaneous estimation of Tramadol Hydrochloride (TRA) and Diclofenac Sodium (DIC) in pharmaceutical preparations. The absorbance value at 288nm was used for the estimation of DIC where TRA showed zero absorbance. The absorbance value for TRA was estimated by taking difference of absorbance at two wavelengths 283 nm and 268.9 nm. These method obeyed Beer’s law in the concentration range of 4-24 μg/ml for TRA and 6-36 μg/ml for DIC in 0.1N NaOH. The results of analysis have been validated statistically and recovery studies confirmed the accuracy of the proposed method. The method was found to be simple, rapid and accurate. Hence can be used for routine simultaneous estimation of these drugs in formulations....
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