Current Issue : July- September Volume : 2012 Issue Number : 3 Articles : 51 Articles
Simultaneous and forced degradation studies for antidepressant analytes require knowledge of chemical, physicochemical and instrumental methods like High Performance Liquid Chromatography (HPLC), High Performance Thin Layer Chromatography (HPTLC) etc. There have been different experimental and empirical approaches reported in the literature for determination of antidepressant analytes where different approximations were applied. One of the most applied approach is HPLC. Therefore, the objective of this study is to review the literature and optimizing methodologies for simultaneous determination of antidepressant analytes. HPLC, alone or in combination with other methods such as mass, Gas Chromatography (GC) has proven to be key methods for identifying compounds....
A simple, rapid, and reliable HPTLC method has been established for simultaneous estimation of Nebivolol and Hydrochlorothiazide in combined dosage form. Chromatographic separation was performed on aluminum Precoated with silica gel 60 F254 using Ethyl Acetate: Methanol: Formic acid (8:0.5:0.5 v/v/v) as Mobile Phase. Calibration curves were linear in the range of 600-1400 ng /spot for nebivolol (R2=0.997) and 1500-3500 ng/spot for Hydrochlorothiazide (R2=0.993). Detection was carried out densitometrically at 280 nm. The suitability of this HPTLC method for quantitative determination of the compounds was proved by validation in accordance with the requirements of the ICH guidelines. The method was used for routine analysis of Nebivolol and Hydrochlorothiazide in Tablet dosage form....
The combination of Ofloxacin (OFL) and Cefpodoxime proxetil (CPD) is used in the treatment of upper and lower respiratory tract infection and typhoid fever. A simple, precise and accurate isocratic RP-HPLC method was developed and validated for determination of OFL and CPD in tablets. Isocratic RP-HPLC separation was achieved on a ACE C18 column (150 × 4.6 mm id, 5 µm particle size) using the mobile phase 0.2% triethyl amine in 20mM Ammoniun acetate buffer-Acetonitrile (65:35 v/v, pH 7.0) at a flow rate of 1.0 mL/min. The retention time of Ofloxacin and two isomer of Cefpodoxime Proxetil was 3.45, 9.95 and 11.15 min, respectively. The detection was performed at 272 nm. The method was validated for linearity, precision, accuracy, robustness, solution stability and specificity. The method was linear in the concentration range of 2-20 µg/mL with a correlation coefficient of 0.9995 for both drugs. OFL and CPD were subjected to forced degradation studies. The degradation products obtained were well resolved from the pure drugs with significantly different Rt values. As the method could effectively separate the drugs from its degradation products, it can be used for stability-indicating analysis....
Amlodipine is a long-acting calcium channel blocker (dihydropyridine (DHP) class) used as an anti-hypertensive and in the treatment of angina. Like other calcium channel blockers, amlodipine acts by relaxing the smooth muscle in the arterial wall, decreasing total peripheral resistance and hence reducing blood pressure; in angina it increases blood flow to the heart muscle . The clinical and pharmaceutical analysis of this drug requires effective analytical procedures for quality control and pharmacodynamic and pharmacokinetic studies as well as stability study. 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 amlodipine as single or combination with other drugs in bulk drugs, formulations and biological fluids have been reviewed. this review covers the time period from 1998 to 2011 during which 42 analytical methods including spectrophotometric methods like uv and derivative; visible which is based on formation of metal complexation, ion pair formation, charge-transfer complexation, IR spectroscopy, diffuse reflectance spectroscopy, spectrofluorometric methods and chromatographic method including HPLC, HPTLC, LC-MSMS and miscellaneous method like differential-pulse voltammetry, potentiometric method were reported. The application of these methods for the determination of amlodipine in pharmaceutical formulations and biological samples has also been discussed....
A simple high performance thin layer chromatography method is developed. The determination was carried on silica gel 60 gf254 hptlc plates using a mobile phase of Toluene : Ethyl Acetate : Methanol : Acetic acid (6:3:1:0.1 v/v/v/v). The absorbance of the spots was measured by densitometry at 289 nm. The retention Factor (Rf) For omeprazolewas 0.75,and for cinitapride hydrogen tartrate 0.48. Omeprazole and Cinitapride hydrogen tartrate showed a linear response in the concentrarion range 100-600ng and 15-90ng/band respectively. The correlation co-efficient (R2 value) for Omeprazole and Cinitapride hydrogen tartrate was 0.996 and 0.995 for both drug. The result of analysis have been validated statistically and by recovery studies. The percentage recoveries obtained for Omeprazole and Cinitapride hydrogen tartrate ranges from 97.86 To 99.20....
A Simple High Performance Thin Layer Chromatography Method For The Simulateneous Estimation Of Aspirin And Rosuvastatin calcuim In Bulk Drug And Marketed Formulation Is Developed.The Determination Was Carried On Silica Gel 60 GF254 HPTLC Plates Using A Mobile Phase Of Ethyl Acetate:Toluene:Acetone:Glacial Acetic Acid(4:4:2:0.1). The Absorbance Of The Spots Was Measured By Densitometry At 254 Nm.The Retention Factor (Rf) For Rosuvastatin calcuim Was 0.36, And For Aspirin 0.60. Aspirin And Rosuvastatin calcium Showed A Linear Response In The Concentrarion Range 300ng-750ng And 40ng-100ng/Band Respectively. The Correlation Co-Efficient (R2 Value) For Aspirin And Rosuvastatin calcuim Was 0.9965 And 0.9992 For Both Grug.The Result Of Analysis Have Been Validated Statistically And By Recovery Studies. The Percentage Recoveries Obtained For Aspirin And Rosuvastatin calcuim Ranges From 99.100 To 101.94....
Simple sensitive accurate uv spectroscopic methods was developed for the simultaneous estimation of Sildenafil Citrate And Dapoxetine Hydrochloride in pharmaceutical dosage form. In this communication absorbance ratio method (Q value) was reported for the assay of both the drugs in the pharmaceutical dosage form. In absorbance ratio method (Q value) the absorbance were measured at wavelengths 237 nm and 293 nm. The proposed method was validated statistically for specificity, linearity, accuracy and precision. Recoveries of methods were carried out by standard addition method. The low values of standard deviation and percentage RSD indicated high precision of methods. These methods were successfully used for routine analysis of Sildenafil Citrate and Dapoxetine Hydrochloride in combination dosage form with good recoveries....
A reverse phase HPLC method is developed for the determination of Cinitapride and pantoprazole in pharmaceutical dosage forms. Chromatography was carried out on a C18 column [4.6 x 150mm, 5m, Make: 10AT SHIMADZU – SPD 10A Detector] using a mixture of sodium dihydrogen phosphate dihydrate buffer and acetonitrile (60:40 v/v) as the mobile phase at a flow rate of 1ml/min. Detection was carried out at 264 nm .The retention time of the drug Cinitapride and Pantoprazole was 2.51 min and 4.92 min. The method produced linear responses in the concentration range of 20 to 120μg/ml of Cinitapride and Pantoprazole. The LOD values for HPLC method for Cinitapride and Pantoprazole were found to be 0.17 and 0.61ng/ml. The LOQ for Cinitapride and Pantoprazole were foud to be 0.53 and 1.87 ng/ml respectively. The method was found to be applicable for determination of the drug in tablets....
The present research work describes not only simple and rapid but also sensitive, accurate, precise, and reliable absorbance ratio (Q – ratio) method for the simultaneous estimation of Rabeprazole sodium and Levosulpiride in combined pharmaceutical formulation. Absorbance ratio method uses the ratio of absorbances at two selected wavelengths, one which is an isoabsorptive point and other being the λmax of one of the two components. Rabeprazole sodium and Levosulpiride show an isoabsorptive point at 260.57 nm in methanol. The second wavelength used is 284 nm, which is the λmax of rabeprazole sodium in methanol. The linearity was obtained in the concentration range of 5 - 25 μg/ml for Rabeprazole sodium and 19 - 95 μg/ml Levosulpiride. The concentrations of both the drugs were determined by using ratio of absorbances at isoabsorptive point and at the λmax of Rabeprazole sodium. The method was successfully applied to pharmaceutical dosage form because no interference from the tablet excipients was found. The results of analysis have been validated statistically for linearity, LOD, LOQ, accuracy, precision, robustness and ruggedness of the proposed method. Present method is economical in the means of both time & cost....
Chromophore is the part of a molecule or chemical group which is responsible for its colour. The colour arises when a molecule absorbs certain and transmits or reflects others. Chromophore is the moiety that causes a conformational change of the molecule when hit by light. The visible spectrum constitutes but a small part of the total radiation spectrum. Most of the radiation that surrounds us cannot be seen, but can be detected by dedicated sensing instruments. This electromagnetic spectrum ranges from very short wavelengths (including gamma and x-rays) to very long wavelengths (including microwaves and broadcast radio waves). When light passes through the compound, energy from the light is used to promote an electron from a bonding or non-bonding orbital into one of the empty anti-bonding orbitals. A chromophore is a region in a molecule where the energy difference between 2 different molecular orbitals falls within the range of the visible spectrum. The present review is an attempt to provide detail knowledge and informations about cuurent status of chromophore utilization in the field of UV analysis....
A new, precise, accurate and selective TLC-Densitometry method has been developed for simultaneous determination of Tamsulosin Hydrochloride and Finasteride in tablet dosage form. Chromatographic separation was performed on aluminum Precoated with silica gel 60 F254 using Ethyl Acetate: Chloroform: Triethylamine (9.5:1.5:0.15v/v/v) as Mobile Phase. Detection was carried out densitometrically at 279 nm. The Rf values of Tamsulosin Hydrochloride and Finasteride are 0.189±0.02 and 0.344±0.03 respectively. The reliability of method was assessed by evaluation of Linearity which was found to be 400-1360ng per spot for Tamsulosin Hydrochloride and 5000-17000ng per spot for Finasteride. Accuracy of method was assessed by % Recovery which was found to be 99.06-99.82% and 99.59-99.80% for Tamsulosin Hydrochloride and Finasteride respectively. Thus, this method can be used for routine analysis of Tamsulosin hydrochloride and Finasteride in combined tablet dosage form....
Since methylcobalamin is the only form of vitamin B12 that can cross the blood brain barrier so it is also important in formulation .From literature survey it was found that there is no single method for the estimation of methylcobalamin in formulation containing multiple vitamin and minerals. Therefore a simple precise and accurate method was developed for the detection and estimation of methylcobalamin by RP-HPLC.The linearity value was found to be 0.9960. The % RSD for precision 0.8 ,0.4 &0.4 for retention time, area and amount. The accuracy studies were done for 80-120% sample and the results were 1.3,1.5 , 1.1 1.8 & 2.0 respectively. . The method passed the validation parameters and had the LOD & LOQ value as0.00195 %0.006519 respectively ....
A simple, precise, accurate and reproducible spectrophotometric method has been developed for simultaneous estimation of Aspirin and Esomeprazole Magnesium by employing first order derivative zero crossing method in methanol. The first order derivative absorption at 313 nm (zero cross point of aspirin) was used for quantification of Esomeprazole Magnesium and 236 nm (zero cross point of Esomeprazole Magnesium) for quantification of aspirin. The linearity was established over the concentration range of 10-60 μg/ml and 10-60 μg/ml for Esomeprazole Magnesium and Aspirin with correlation coefficient r 2 0.9974 and 0.9977, respectively. The mean % recoveries were found to be in the range of 99.7 – 99.9 % and 99.6 – 100.10 % for Esomeprazole Magnesium and aspirin, respectively. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of Esomeprazole Magnesium and aspirin in their combined Tablet dosage form....
Novel combination of Fexofenadine hydrochloride (FEXO) and Montelukast Sodium (MONT) is available as tablet dosage form in the ratio of 12:1 and no spectrophotometric method has been reported yet. The present research work aims to develop a simple, sensitive, accurate and reproducible method for the simultaneous estimation of both drugs by the first derivative spectrophotometric method, using methanol: water (20:80) as a solvent. The Method was performed at 297.10(zero crossing point of montelukast sodium) and 340.60(zero crossing point of fexofenadine hydrochloride) for Fexofenadine hydrochloride and Montelukast sodium respectively. The regression analysis data for the calibration plot showed good linear relationship in the concentration range of 12‐60 μg/ml (R2 = 0.9993) for Fexofenadine hydrochloride and 1‐5 μg/ml (R2 = 0.9988) for Montelukast sodium. The average percentage recovery of Fexofenadine hydrochloride and Montelukast sodium combination was found to be 100.20% and 99.28% respectively. The LODs for Fexofenadine hydrochloride and Montelukast sodium were 2.7862 μg/ml and 3.0657 μg/ml and LOQs were found to be 8.4432 μg/ml and 9.2902 μg/ml respectively. Statistical analysis proves that the method is reproducible and selective for the simultaneous determination of Fexofenadine hydrochloride and Montelukast sodium. The Results were found to be within acceptance criteria according to ICH Q2 R1 guidelines....
A simple, precise, accurate and reproducible spectrophotometric method has been developed for simultaneous estimation of Naproxen and Esomeprazole Magnesium trihydrate by employing first order derivative zero crossing method in methanol. The first order derivative absorption at 318 nm (zero cross point of Naproxen) was used for quantification of Esomeprazole Magnesium trihydrate and 276 nm (zero cross point of Esomeprazole Magnesium trihydrate) for quantification of Naproxen. The linearity was established over the concentration range of 1-11 μg/ml and 10-35 μg/ml for Esomeprazole Magnesium trihydrate and Naproxen with correlation coefficient r 2 0.999 and 0.999, respectively. The mean % recoveries were found to be in the range of 98.88 – 99.33 % and 99.11 – 99.55 % for Esomeprazole Magnesium trihydrate and Naproxen, respectively. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of Esomeprazole Magnesium trihydrate and Naproxen in their combined Tablet dosage form....
A simple, specific, accurate, precise and reproducible first order derivative spectrophotometric method has been developed and validated for the simultaneous estimation of Sulbactam Sodium (SUL) and Cefixime Trihydrate (CEF) in their combined dosage form. The principle advantage of this method is to get an even order spectrum of narrower spectral bandwidth than its fundamental spectrum, Therefore method shows better resolution of overlapping band. Methanol was selected as a common solvent for Sulbactam Sodium and Cefixime Trihydrate for determination at 255 nm and 275 nm over the Linearity range of 50-300 and 5-30 μg/ml respectively. 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 Sulbactam Sodium and Cefixime Trihydrate was proved by validation and recovery studies. The % recoveries of the both the drugs were found to be 99.31% – 99.72 % and 99.24– 99.63 % respectively. Limit of Detection and Quantitation were found to be 2.49μg/ml and 1.01μg/ml for SUL and 7.56μg/ml and 3.06μg/ml for CEF. The method was validated as per International Conference on Harmonization (ICH) guideline....
A simple, rapid, precise, stable and accurate liquid chromatographic method (HPLC) was developed for the simultaneous estimation of Clindamycin phosphate (CLI), Clotrimazole (CLO) and Tinidazole (TIN) in pharmaceutical dosage form. A Kromasil C18 column (150 MM ×4.6 MM, 5 µm) in isocratic mode using ph 2.5 ±0.01 phosphate buffer and methanol in the ratio of 40:60 as a mobile phase was used. The flow rate was maintained at 1 mL/min. The detection was carried out at 210 nm. The column temperature was maintained at 40 oC. The retention time was found to be 2.7 min, 3.9 min and 8.5 min TIN, CLI and CLO respectively. The method was validated for linearity, accuracy, precision and robustness. The assay was linear over the range of 75-350 µg/ml. The average recovery of TIN, CLI and CLO was found to be 99.87±0.64 %, 100.61±1.02 % and 100.03±0.84 % respectively. The percentage relative standard deviation (%RSD) was found to be less than 2 % in precision study for each drug. The proposed method was successfully applied for the quantitative determination of CLI, CLO and TIN in pharmaceutical dosage form....
An accurate, simple, reproducible, and sensitive HPLC method was developed and validated for the estimation of Propranolol hydrochloride (PRH) and Flunarizine dihydrochloride (FLZ) in solid dosage form. The analyses were performed on a kromasil C18 column, 250 × 4.60 mm id, 5 μm particle size. The mobile phase methanol: buffer (20 mM phosphate buffer, pH-3): TEA (80: 20: 0.4 v/v/v), was pumped at a constant flow rate of 1.0 mL/min. UV detection was performed at 240 nm. Retention times of Propranolol hydrochloride and Flunarizine dihydrochloride were found to be 2.90 and 4.10 min, respectively. The LOD & LOQ is 1.09ug/ml & 3.33ug/ml for PRH & 0.34ug/ml & 1.02ug/ml for FLZ. The method was validated in terms of linearity, precision, accuracy, LOD, LOQ, and robustness. The response was linear in the range 10-50 μg/mL (r2 = 0.995) for Propranolol hydrochloride, 2.5-12.5 μg/mL (r2 = 0.996) for Flunarizine dihydrochloride....
A simple, specific, accurate, precise and reproducible spectrophotometric method has been developed and validated for the simultaneous estimation of Aliskiren Hemifumarate (ALK) and Valsartan in their combined tablet dosage form. Methanol was selected as a common solvent for Aliskiren Hemifumarate and Valsartan for determination at 275 nm and 250 nm over the Linearity range of 30-80 and 5-25 μg/ml respectively. 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 Aliskiren Hemifumarate and Valsartan was proved by validation and recovery studies. The % recoveries of Aliskiren Hemifumarate and Valsartan were found to be 99.32 -99.89% and 99.12 - 99.71% respectively. Limit of Detection and Quantitation were found to be 4.0749μg/ml and 12.3482μg/ml for Aliskiren hemifumarate and 3.51μg/ml and 10.6551μg/ml for Valsartan. The method was validated as per International Conference on Harmonization (ICH) guideline....
The present manuscript describes simple, sensitive, rapid, accurate, precise and economical spectrophotometric method for the simultaneous determination of Escitalopram oxalate and Etizolam in combined tablet dosage form. The method is based on the simultaneous equations for analysis of both the drugs using 0.01 N HCl as solvent. Escitalopram oxalate has absorbance maxima at 238 nm and Etizolam has absorbance maxima at 249 nm in 0.01 N HCl. The method was validated for linearity, precision, accuracy, LOD, LOQ and solution stability. The method was linear in the concentration range of 4-40µg/ml for ESC and 1-32 µg/ml for ETI with a correlation coefficient of 0.9999 and 0.9998 for respective drugs. The percent recovery was found in the range of 98.39-101.13% and 98.07-101.83 % for ESC and ETI, respectively. The proposed method was successfully applied for quantitative determination of Escitalopram oxalate and Etizolam in combined tablet dosage form for routine analysis....
A simple UV spectrophotometric method was developed and validated for quantitative determination of cinitapride and omeprazole, at their respective analytical wavelengths in fixed dose combination (FDCS) products. Method involve formation and solving of simultaneous equation by the measurement of absorbances at two wavelength 263.0 nm (max for cinitapride) and 302.0 nm (max for omeprazole). The different analytical performance parameters such as linearity, accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ) were determined according to International Conference on Harmonization ICH Q2 (R1) guidelines. Method obeyed the beer’s law and Calibration cures for both omeprazole and cinitapride were linear over concentration range of 2-10 µg/mL with correlation coefficients 0.9994 and 0.9998, respectively. The recovery of omeprazole and cinitapride was found to be in range of 98.15 to 101.92% and from 99.56 to 100.18%, respectively. The limit of determination for omeprazole and cinitapride was 0.09µg/ml and 0.03µg/ml, respectively. The limit of quantification for omeprazole and cinitapride was 0.29µg/ml and 0.11µg/ml, respectively. This developed method is simple, rapid, precise and accurate and was successfully employed for quantifying both drugs containing pharmaceutical formulations....
This study describes the development and validation for the simultaneous estimation of Etodolac (ETO) And Thiocolchicoside (THIO) by the Simultaneous equation and Absorption ratio method of UV spectroscopy methods. The quantification was achieved at 280 nm (ETO) and 257 nm (THIO) over the concentration range of 1-12 µg/ml for Etodolac (r2=0.9998) and 1-12 µg/ml for Thiocolchicoside (r2=0.9998) by the Simultaneous equation method. Procedure does not require prior separation of components from the sample. LOD values for ETO and THIO were found to be 0.06 μg/ml and 0.04 μg/ml, respectively. LOQ values for ETO and THIO are found to be 0.17 μg/ml and 0.13 μg/ml respectively. The other method involved Q-absorption analysis based on the measurement of absorbance at two wavelengths, i.e λmax of Etodolac (280 nm) and Iso-absorptive point of both drugs (269.2 nm). Beer’s law was obeyed in the concentration range between 1-12μg for both Etodolac and Thiocolchicoside. 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 relative standard deviation was found to be <2.0 % in both the methods. The present result shows that the proposed methods can be successfully used for simultaneous determination of the drug content in marketed formulations....
A simple, precise, accurate and reproducible spectrophotometric method has been developed for simultaneous estimation of Amlodipine besylate and Indapamide by employing first order derivative zero crossing method in methanol. The first order derivative absorption at 224 nm (zero cross point of Indapamide) was used for quantification of Amlodipine besylate and 237 nm (zero cross point of Amlodipine besylate) for quantification of Indapamide. The Linearity range 10-60 and 5-30 μg/ml for both Amlodipine besylate and Indapamide. The % recoveries of the both the drugs were found to be 98.8 – 102.2 % and 100 – 102.5 % Amlodipine besylate and Indapamide respectively. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of Amlodipine besylate and Indapamide in their combined Tablet dosage form....
A simple, precise and economical Zero-order (Method A), Area Under Curve [AUC] (Method B) UV-Spectropotometric methods have been developed and validated for the estimation of Mitiglinide calcium hydrate in bulk and its formulation. The solutions of standard and sample were prepared in methanol. Mitiglinide calcium hydrate was estimated at 259 nm for the zero order UV-Spectrophotometric method, while area under the zero order spectrum of Mitiglinide calcium hydrate was measured in between 254 nm to 264 nm for AUC method. Beer’s law was obeyed in the concentration range of 100 - 600 μg / ml with r2 value 0.999 for zero order method. Similarly in AUC method, Beer’s law was obeyed in the concentration range of 100-600 μg / ml with r2 value 0.999. The precision expressed as relative standard deviation, which was within 2.0 % for the above two methods. The proposed methods were successfully applied for the determination of Mitiglinide calcium hydrate in Oral formulations. In addition, the proposed methods are simple, easy to apply, low-cost, and requires relatively inexpensive instruments....
Spectrophotometric method has been developed for simultaneous estimation of Doxofylline and Terbutaline sulphate in combined dosage form. The method employed simultaneous equation method for analysis using 0.1N NaOH as a solvent. The two wavelengths 274nm and 296nm were selected for estimation of Doxofylline and Terbutaline sulphate respectively. Linearity was observed in the concentration range of 5–25μg/mL for both drugs Doxofylline and Terbutaline sulpahte. The method was validated as per ICH guidelines. The method can be employed for estimation of pharmaceutical formulations....
Camptothecin (CPT), a pentacyclic monoterpene indole alkaloid, is a potent anticancer molecule. A simple and reproducible UV-visible spectrophotometric method for the quantitative determination of Camptothecin (CPT) from Nothapodytes nimmoniana was developed and validated as per ICH guidelines. The parameters linearity, precision, accuracy, limit of detection, limit of quantitation were studied. The concentration of CPT present in stem bark of Nothapodytes nimmoniana was found to be 1.654±0.04 % w/w. Recovery studies were carried out by standard addition method. Recovery of camptothecin at all the level was found to be in the range of 98.76%-99.88%. The developed method was found to be accurate, simple, precise and rapid and can effectively applied for routine analysis....
First order derivative spectroscopy method involves the measurement of absorbances at zero crossing point of other drug. A newsimple, accurate, economic and sensitive first order derivative spectrophotometric method is proposed for the simultaneous estimation of Sildenafil Citrate and Dapoxetine Hydrochloride in their combined dosage form. Due to mutual interference, quantitation was carried out by the proposed methods namely first order derivative spectroscopy. The drugs obeyed the Beer’s law in the concentration range of 5-30μg//ml (r2 = 0.9984 and r2 = 0.9992) for Sildenafil Citrate and Dapoxetine Hydrochloride both. In the proposed method, absorbance was measured at 265.8 nm (Zero Crossing Point of Sildenafil Citrate) and 250.3 nm (Zero Crossing Point of Dapoxetine Hydrochloride). The percent recoveries were found near to 100% for both the drugs indicated that method is precise and reproducible. LOD for Sildenafil Citrate and Dapoxetine Hydrochloride was found to be 0.566 μg/ml and 1.65 μg/ respectively. LOQ was found to be 1.71 μg/ml and 5.0 μg/ml respectively....
A Simple High Performance Thin Layer Chromatography Method for the Simulateneous Estimation of Ibuprofen and Famotidine in marketed formulation was developed. The Determination was carried on Silica Gel 60 GF254 HPTLC Plates using a Mobile Phase of Toluene: MeOH: Ethyl acetate: Glacial Acetic Acid (5.5:3.2:1:0.3 v/v/v/v). The absorbance of the spots was measured by Densitometry at 271 nm. The Retention Factor (Rf) was found to be 0.71 for Ibuprofen and 0.22 for Famotidine. Ibuprofen and Famotidine showed a linear response in the Concentrarion Range 1000-5000 ng/band and 40-150 ng/band respectively. The Correlation Co-efficient (r2 Value) for Ibuprofen and Famotidine was found to be 0.998 and 0.997 respectively. The result of analysis has been validated statistically and by Recovery Studies. The percentage recoveries obtained for Ibuprofen and Famotidine ranges from 99.26 to 100.61....
A simple, sensitive, and precise high performance liquid chromatographic method has been developed for the simultaneous determination of esomeprazole magnesium (ESO) and domperidone (DOM) from combined capsule dosage form. The compounds were well separated on a ODS hypersil C-18 (4.6mm×250mm) column. The mobile phase consisting of (methanol: acetonitrile: 1% triethylamine solution = 60:30:10 v/v/v) at a flow rate of 0.8 mL/min with detection wavelength at 280 nm. The retention times for esomeprazole magnesium and domperidone were found to be 2.833 and 3.765 min, respectively .The linearity range and recovery amount were found to be 20-100 μg /ml and in between 99-101% respectively for both the drugs. The method was validated for specificity, linearity, accuracy, precision, LOD, LOQ. The method herein described can be employed for quality control and routine analysis of esomeprazole magnesium and domperidone in pharmaceutical dosage form....
A simple and sensitive HPTLC method has been developed for determination of Ambroxol and roxithromycin in its pharmaceutical dosage forms. The method employed HPTLC aluminium plates precoated with silica gel 60F-254 as the stationary phase. Benzene: Chloroform: TEA (5:4:1v/v) as a mobile phase then spray with sulfuric acid and dry the plate at ahe room temperature. After that saturation time is optimized for the better separation The Rf value of Ambroxol HCl is 0.59±0.02 and of Roxithromycin is 0.39±0.02 were found. The linearity for both the drugs were in the range of 120-360 μg/ml and 300-900 μg/ml. The % recoveries of ambroxol hydrochloride and cetirizine hydrochloride were found to be in the range of 99.37-99.42 and 99.27-99.3, respectively. The proposed method was validated and successfully applied to the estimation of ambroxol hydrochloride and roxithromycin in combined dosage form....
A simple Reverse phase liquid chromatography method has been also developed and subsequently validated for the tablet dosage form. Here mobile phase consisting Methanol 25mM Triethylamine pH set to 3.6 with O-Phosphoric acid gave resolution of peaks and satisfied retention time in HPLC. C-18(250mm × 4.6mm i.d with particle size of 5 µm used with flow rate 0.6ml/min using UV detection at 254nm. The retention time of Amlodipine Besylate and Clopidogrel bisulphate were found at 4.6 and 6.2 respectively. In Which Linearity for AML and CLOP was found to be y = 6720x-16231, R2 = 0.998 in concentration range of 5-25µg/ml and 984.04+ 948780, R2 + 0.998 for 75-375µg/ml respectively. Recovery studies were found to be 99.16-100.5% for AML and 99.72-100.86% for CLOP. Other all the data (Precision, LOD and LOQ, Assay, Robustness) are within the specified criteria of ICH guideline. The proposed method was validated and successfully applied to the estimation of Amlodipine besylate and Clopidogrel bisulphate in combined dosage form....
In UV Spectrophotometry Method, Methanol use as Solvent and λmax of Amlodipine besylate and Clopidogrel bisulphate selected for analysis were found to be 361nm and 264nm. A simple Reverse phase liquid chromatography method has been also developed and subsequently validated for the tablet dosage form. New UV Spectrophotometric (UV method) have been developed and subsequently validated for the tablet dosage form. The Linear regression equations for Amlodipine Besylate and Clopidogrel bisulphate was found to be 0.019x-0.017, R2 = 0.998 and 0.001x + 0.022, R2 = 0.998 (in µg/ml) measured at 361nm and 264nm respectively in concentration range of 5-25µg/ml and 75-375µg/ml and Recovery studies was found to be 100.05-100.34% for AML and 99.80- 100.25% of CLOP. Other all the data (Precision, LOD and LOQ, Assay, Robustness) are within the specified criteria of ICH guideline....
A simple, rapid, sensitive and accurate RP-HPLC method has been developed for estimation of Fluconazole and Ivermectin in bulk drug and in pharmaceutical formulation. Linearity was observed in the concentration range of 100-300 μg/ml and 4-12 μg/ml for Fluconazole (r2 =0.998) and Ivermectin (r2 =0.997) respectively. Amounts of drug estimated from tablet formulation were in good agreement with label claim. The method was validated statistically and by recovery studies. The proposed method is economical and sensitive for the estimation of Fluconazole and Ivermectin in bulk and tablet dosage form....
Metoprolol Succinate (MS) is B1 -Blocker acting as a adrenoreceptor antagonist agent and Clopidogrel bisulphate (CLOP) is an antiplatelet agent so, the combination is used in the treatment of Hypertension who need antiplatelet therapy. MS and CLOP were estimated at 254 nm by densitometry using silica gel 60/UV254 as stationary phase and a premix of Hexane: Toluene: Methanol: TEA (5: 3: 1.2: 0.5 /v/v/v) as mobile phase. Rf value of MS and CLOP were 0.23±0.02 and 0.68±0.02 respectively, with a Linearity range 1000-3500 ng/band and 1500-5250 ng/band and R2 value was found to 0.999 for MS and CLOP both. The developed high performance thin layer chromatography method was found to be specific, precise and reproducible and can be used for the routine estimation of MS and CLOP in the combined tablet dosage form....
Metoprolol Succinate (MS) is B1 -Blocker acting as a adrenoreceptor antagonist agent and Olmesartan medoxomil (OM) is an AT1- receptor blocking property so, the combination is used in the treatment of Hypertension. MS and OM were estimated at 254nm by densitometry using silica gel 60/UV254 as stationary phase and a premix of Toluene: Methanol: Acetonitrile: Triethylamine (4:2:4:0.2 v/v) as mobile phase. Rf value of MS and OM were 0.39±0.02 and 0.66±0.02 respectively, with a Linearity range 500-3000 ng/band and 200-1200 ng/band and R2 value was found to be 0.997 and 0.999 for MS and OM respectively. The developed high performance thin layer chromatography method was found to be specific, precise and reproducible and can be used for the routine estimation of MS and OM in the combined tablet dosage form, available in market...
A reverse phase high performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of Metoprolol succinate (MS) and Olmeartan medoxomil (OM) in marketed formulation is developed. The determination was carried out on a Hibar 250-4.6 RP18 (5um) column using a mobile phase of Methanol: Water: Acetonitrile (70:20:10) pH-3.4 with ortho phosphoric acid. The flow rate was 1.0 ml/min with detection at 231 nm.The retention time for Metoprolol succinate 2.1 min and Olmeartan medoxomil 3.0 min. Metoprolol succinate and Olmeartan medoxomil showed a linear response in the concentration range of 5-30µg/ml and 2-12 µg/ml respectively. The correlation co-efficient (r2) 0.997 for Metoprolol succinate and 0.999 for Omesartan medoxomil.The results of analysis have been validated statistically and by recovery studies.The percentage recoveries obtained for Metoprolol succinate and Omesartan medoxomil ranges from 99.05-101.28%....
Simultaneous quantification of Racemethionine and Taurine in Capsules by HPTLC method was developed and validated. The method was based on separation of drugs followed by post chromatographic derivatization with Ninhydrine and densitometric measurement of their spots at 500 nm. The chromatograms were developed using a mobile phase of n - butanol: acetic acid: water (6:2:2, v/v/v) on pre-coated plate of silica gel GF245 aluminum TLC plate. The Rf values for Racemethionine and Taurine were found to be 0.49 ± 0.03 and 0.34 ± 0.03 respectively. The calibration curves were linear in range of 160 – 560 ng/band and 400 - 1400 ng/band for Racemethionine and Taurine respectively. The % recoveries for Racemethionine and Taurine were found to be in the range of 99.05-100.52 and 98.07-99.48 respectively....
An accurate, precise and ecofriendly spectrophotometric method is presented for the determination of Cefixime based on the formation of a yellow colour product with ninhydrin in the presence of bicarbonate with an absorption maximum at 438 nm. The reaction proceeds quantitatively at 97 ± 1°C in 15 min. The calibration curve is linear over the range of 45-65 μg/ml and is described by the regression equation A = (-) 0.858 + 0.021 C with a regression coefficient (r) of 0.9987 (n = 5). The calculated molar absorptivity and Sandell sensitivity values are 4.1536 x 10 3 L/mol/cm and 0.0072 μg/cm2, respectively. The limits of detection (LOD) and quantification (LOQ) calculated as per ICH guidelines are 1.13 and 3.40 μg/ml, respectively. The within-day accuracy expressed as relative error was better than 2.5% with precision (RSD) ranging from 1.02 to 1.93%. The between-day accuracy ranged from 1.5-3.0% with a precision less than 4%. Accuracy was also checked by placebo blank and synthetic mixture analyses besides a recovery study via standard addition procedure....
A simple, reproducible and efficient reverse phase high performance liquid chromatography (RP-HPLC) method has been developed for estimation of rupatadine fumarate in its tablet dosage form. The separation was performed on a Hypersil BDS -C18 (250 mm×4.6 mm, 5 μm) column, the mobile phase was composed of 1% triethylamine (pH 3.0 using o-phosphoric acid)-acetonitrile (30∶70) and the flow rate was 1.0 mL•min-1 with UV detection at 252 nm and the retention time for rupatadine fumarate is 5 min. The linear dynamic response was found to be in the concentration of 50 μg-150 μg/ml. The correlation coefficient was found to be 0.9996. The %RSD of % recovery of rupatadine fumarate was found to be 0.899, 0.267, and 0.421 for 50%, 100% and 150% respectively. Proposed methods were found to be simple, accurate, precise and rapid and could be used for routine analysis. This condition is applied only for tablet dosage form. The statistical parameters and recovery studies were carried out and reported.was also checked by placebo blank and synthetic mixture analyses besides a recovery study via standard addition procedure....
A reverse phase high performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of Metoprolol succinate and Clopidogrel bisuphate in marketed formulation is developed. The determination was carried out on a Hibar 250-4.6 RP18 (5um) column using a mobile phase of Methanol: Water: Acetonitrile (70:20:10) pH-3.4 with ortho phosphoric acid. The flow rate was 1.0 ml/min with detection at 222 nm.The retention time for Metoprolol succinate 2.1 min and Clopidogrel bisulphate 7.0 min. Metoprolol succinate and Clopidogrel bisulphate showed a linear response in the concentration range of 5-40µg/ml and 7.5-60µg/ml respectively.The correlation co-efficient (r2) 0.997 for Metoprolol succinate and 0.999 for Clopidogrel bisulphate.The results of analysis have been validated statistically and by recovery studies.The percentage recoveries obtained for Metoprolol succinate and Clopidogrel bisulphate ranges from 99.05-101.28%....
A new, simple, rapid and novel simultaneous equation method has been developed & validated for simultaneous estimation of Citicoline and Piracetam in their combined tablet dosage form. The method involves measurement of absorbance at two wavelengths, 216 nm and 275 nm λmaxof Piracetam and Citicoline respectively. Beer’s law obeyed in concentration range of 32-72 μg ml-1 and 40-90 μg ml-1 for Piracetam and Citicoline respectively. The method was found to be precise, accurate and specific by statistical parameters and recovery studies. The proposed method was successfully applied for Simultaneous estimation of Citicoline and Piracetam in combined solid dosage form....
A simple, specific, accurate, precise and reproducible method has been developed and validated for the simultaneous estimation of olmesartanmedoxomil andmetoprolol succinate in their combined tablet dosage form using simultaneous equation method.The wavelength for simultaneously detection were 256nm and 223 nm selected for olmesartanmedoxomil and metoprolol succinate, respectivelyin methanol.The method was found to be linear in concentration range of 5-25 μg/ml and 10-50 μg/ml for olmesartanmedoxomil and metoprolol succinate,respectively.The % recoveries were found to be 98.38% – 101.1 % and 98.3– 101.75 % for olmesartanmedoxomil and metoprolol succinate,respectively.LOD were found to be 1.275 μg/ml and 1.297 μg/ml for olmesartanmedoxomil at 256nm and 223 nm and 2.264 μg/ml and 2.692 μg/ml for metoprolol succinate at 256nm and 223 nm,respectively. Methods were statistically validated for accuracy, precision, specificity, LOD, LOQ, robustnessand ruggedness according to ICH guidelines and can be used for analysis of combined dosage form....
A simple, rapid reverse phase high performance liquid chromatographic method has been developed and validated for estimation of Tolperisone hydrochloride and paracetamol in pharmaceutical tablet dosage form. The estimation was carried out on Phenomenex C-18 column at 60 ºC having 250 x 4.6mm, 5µ size with a mixture of methanol: acetonitrile in the ratio of 65:35 :( v/v) as mobile phase. UV detection was performed at 254 nm. The method was validated for linearity, accuracy, precision and specificity as per ICH norms. The developed and validated method was successfully used for the quantitative analysis of commercially available dosage form. The retention time was 2.6 min. for Paracetamol and 4.2 min. for Tolperisone hydrochloride. Total run time was 10 min. at a flow rate of 1.0 ml/min. The calibration curve was linear over the concentration range of 50-150 µg/ml for paracetamol and 25-125 µg/ml for tolperisone. The LOD and LOQ values were found to be 0.48 and 1.46 µg/ml for paracetamol and 0.93and 2.84 µg/ml for tolperisone. The high percentage of recovery confirms the suitability of the method for the estimation of Tolperisone in pharmaceutical dosage form....
A simple, precise, accurate and rapid high performance thin layer chromatographic method has been developed and validated for the simultaneous estimation of Levocetrizine dihydrochloride, Montelukast sodium and Ambroxol hydrochloride. in a combined capsule dosage form. The method was based on separation of three drugs on Merck aluminium plates precoated with silica gel 60 F254 using chloroform: methanol 9.3:0.7(v/v) as mobile phase. Quantitative analysis was performed by densitometric scanning at 206 nm. The three drugs were satisfactorily resolved with Rf values of 0.05, 0.52 and 0.21 mins for levocetirizine ,Montelukast and Ambroxol, respectively. The developed method was validated as per the ICH guidelines (Q2 R1). The method was found to be linear over concentration ranges of 800ââ?¬â??2400 ng/spot for Levocetirizine dihydrochloride, 100-700 ng/spot for Montelukast sodium and 600-1400 ng/spot for Ambroxol hydrochloride. Percentage recovery was found to be 99.46, 87.83 and 97.57 for Levocetrizine dihydrochloride, Montelukast sodium and Ambroxol hydrochloride respectively. The HPTLC method was successfully applied to the analysis of all the three drugs in a pharmaceutical tablet formulation. No chromatographic interference from the tablet excipients was seen in this method. The method developed can be used for routine analysis in bulk drug and capsule dosage form....
Chemically Paracetamol is known as N-(4-hydroxyphenyl)ethanamideN-(4-hydroxyphenyl)acetamide (Acetaminophen)1which is a potent non-steroidal anti-inflammatory agent. Paracetamol is a widely use over the counter pain reliver and antipyretic drug. The present study describes a simple, sensitive and rapid colorimetric method for determination of paracetamol in bulk and tablet dosage form. The method is based on reaction of FC Reagent with phenolic compounds, which involves the oxidation of phenolic compounds by FC reagent in alkaline medium, producing a blue molybdo tungstate complex. The produced complex was measured using uv spectrophotometer at 648 nm. The developed method was validated in terms of precision, specificity, linearity and range. This method provides quick and cost effective quality control tool for routine analysis of paracetamol in bulk and tablet dosage form....
Simple, Precise, Accurate and Rapid methods for simultaneous estimation of Cinitapride Hydrogen Tartrate (CNT) and Omeprazole (OMP) in combined capsule dosage form have been developed. Method A is based on Ratio Spectra Derivative and Method B uses integrated area under curve (AUC), Methanol is used as a solvent for both the methods. In Method A, the amplitudes at 251 nm and 294 nm of the first derivative of ratio spectra were selected to determine CNT and OMP respectively by ratio derivative method. In Method B, the wavelength ranges of 260 – 270 nm and 296 – 306 nm were selected to determine CNT and OMP by AUC method in combined formulation. The linearity was found to be 1.5 - 4.5 µg/ml and 10 – 30 µg/ml for CNT and OMP respectively by both the methods. The % assay for CNT and OMP were found to be 99.66% and 99.89% by Method A & 100.83% and 99.74% by Method B respectively. The methods were validated with respect to linearity, precision and accuracy. The Average Percentage Mean Recovery was found to be 99.24% for CNT and 99.28% for OMP by ratio derivative method and 101.20% for CNT and 99.30% for OMP by AUC method. The developed methods are simple, economical, precise and accurate and can be used for routine quality control of analytes in combined formulations....
Cefpodoxime proxetil (CPD) and Ambroxol hydrochloride (AMB) are used in the treatment of respiratory tract infection, chronic bronchitis, COPD. A simple, precise and accurate isocratic RP-HPLC method was developed and validated for determination of CPD and AMB in tablets. Isocratic RP-HPLC separation was achieved on a ACE C18 column (150 × 4.6 mm id, 5 µm particle size) using the mobile phase Acetronitrile: Phosphate buffer (pH 6.0): Methanol (25:35:40v/v) at a flow rate of 0.8 mL/min. The retention time of Cefpodoxime Proxetil and Ambroxol hydrochloride was 3.5 and 6.5 min. The detection was performed at 248 nm. The method was validated for linearity, precision, accuracy, robustness, solution stability and specificity. The method was linear in the concentration range of 5-50 µg/mL for CPD and 3-30 µg/mL for AMB with a correlation coefficient of 0.999 for both drugs. The intraday precision was 0.17-0.47% and 0.15-0.59% and for interday precision were 0.25-0.37% and 0.22-0.58% for CPD and AMB respectively. The accuracy (recovery) was found to be in the range of 99.09-99.85% and 99.46-99.98% for CPD and AMB respectively....
A novel, simple, accurate, precise andreproducibleUV- Spectrometricmethod has been developed for simultaneous estimationof Clonazepam and Paroxetine hydrochloride hemihydrate in capsule formulation. Clonazepam and Paroxetine hydrochloride hemihydrate in combinedcapsule formulation were estimated using the Area Under Curve (AUC) method at 304 - 314 nm for Clonazepam and 290 - 300 nm for Paroxetine hydrochloride hemihydrate in their methanolic solution. The linearity was found in the concentration range of 0.4- 3.6 µg/ml for Clonazepam and 10- 90 µg/ml for Paroxetine hydrochloride hemihydrate. The method was validated bylinearity, LOD, LOQ, accuracy, precision, robustness and ruggedness for both Clonazepam and Paroxetine hydrochloride hemihydrate.This method can be used for the routine simultaneous estimation of Clonazepam and Paroxetine hydrochloride hemihydrate in industries and other analytical laboratories....
A new, rapid, precise, accurate and sensitive analytical method was developed for the UV spectrophotometric assay of Silodosin. The drug obeyed the Beer’s law and showed good correlation. It showed absorption maxima at 270 nm in Acetonitrile. The linearity was observed between 10-50 μg/ml. The results of analysis were validated by recovery studies. The recovery was more than 99%. The proposed method is the only method available for spectrophotometric determination of Silodosin. It is simple, precise, sensitive and reproducible and can be used for the routine quality control testing of the marketed formulations....
Present work describes UV Spectrophotometric methods for simultaneous estimation of Tolperisone Hydrochloride (TOL) and Paracetamol (PAR) in tablet dosage form. For simultaneous equation method (method-I) wavelengths selected were 260 nm and 242 nm and in first derivative zero crossing method (method-II) wavelengths were selected 242.20 nm for TOL and 260.30 nm for PAR. In both the methods linearity of TOL and PAR were found to be in concentration range of 3-10 µg/mL and 10-30 µg/mL respectively with correlation coefficient >0.998. Validation of the proposed methods was carried out for its accuracy and precision according to ICH guidelines. Percentage recoveries in method-I was found to be 99.16% (TOL) and 99.64% (PAR) and in method-II it was found to be 99.53% (TOL) and 100.23% (PAR). These methods are simple, accurate, precise and economical. There was no interference of any excipient in the determination of drugs in tablets. These methods can be applied for routine quality control analysis and dissolution study....
Diclofenac sodium is chemically known as 2-[(2, 6-dichlorophenyl)amino] phenyl acetic acid monosodium salt which is a potent non-steroidal anti-inflammatory agent. A novel, accurate and precise method developed and validated for estimation of Diclofenac sodium in its pure form & in their pharmaceutical formulation. The proposed developed method is based on reaction between Diclofenac Sodium and 2, 3-Dichloro-1, 4-napthaquinone (Dichlone) in methanol medium. This reaction was carried out by heating at 600C for 10 minutes which produce a charge transfer complex having a absorbance maxima at 535 nm. The values of optimal reaction conditions such as reagent concentration, heating time and stability of the reaction product were determined. In this work, Beer’s law was followed in a concentration range from of 7.4×10-4 to 1.9×10-3 mol l-1 with a correlation coefficient of 0.999 and molar absorptivity of 0.222×103 l mol-1 cm-1. The limit of detection (LOD) and the limit of quantification (LOQ) were found to be 4.77×10-5 mol l-1 & 1.4×10-4 mol l-1 respectively. In the presence of the common exicipients such as glucose, lactose, talc, starch, magnesium stearate, sodium sulphite, titanium dioxide, polyethylene glycol, polyvinyl pyrrolidone, mannitol and benzyl alcohol, no interferences were observed. Recoveries of Diclofenac sodium from various pharmaceutical preparations were found within range of 98.9 to 101.7%....
Loading....