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Sathish Kumar Konidala ¹, Pampana V. V. Suresh Babu ¹, Ranj ¹, K. S. D. Ranjitha ¹

Affiliations
1 Department of Pharmaceutical Analysis, Aditya College of Pharmacy Surampalem, Kakinada, East Godavari, A.P-533437, IN

Abstract

Analytical methods are required to characterize drug substance and drug product composition during all phases of pharmaceutical development. Early phase methods must support changes in synthetic routes and dosage form and elucidate the structures and levels of impurities. In later phases, goals change to the development of rapid and robust methods for release and stability evaluation. Hence we attempt to develop a simple accurate RPHPLC method for the simultaneous estimation of Simvastatin a hypo-lipidemic drug and Sitagliptin an oral antihyperglycemic drug in pharmaceutical formulations. The quantification was carried out on Prontosil ODS C18 Column (250 x 4.6 mm and 5μm) in isocratic mode, with mobile phase consisting of Methanol: Water: Acetonitile in the ratio of 50:30:20 (v/v/v).The mobile phase was pumped at a rate of 0.80ml/min and the detection was carried out at 261nm and the linearity was found to be in the range of 2 to 12μg/ml for Simvastatin and 5-30μg/ml for Sitagliptin. The regression equation was found to be y = 25876x + 41754 (r²=0.999) for Simvastatin and y = 18801x + 12921 (r² = 0.998) for Sitagliptin. The % recovery values were found to be in the range of 98-102% for both the drugs. LOD and LOQ value was found to be 0.005μg/ml, 0.016μg/ml for Sitagliptin and 0.025μg/ml, 0.08μg/ml for Simvastatin respectively. The proposed method was validated for accuracy and precision. Statistical analysis proves that the method was found to be simple, precise, accurate, rapid and reproducible and can be used for the routine simultaneous determination of Simvastatin and Sitagliptin in bulk drug and in pharmaceutical formulations.

Keywords

RP-HPLC, Simultaneous Estimation, Simavastatin and Sitagliptin, Method Validation.

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Yamini Mangalagiri ¹, Siva Sreelakshmi Mamidala ¹, Sathish Kumar Konidala ¹

Affiliations
1 Department of Pharmaceutical Analysis and Quality Assurance, Aditya Institute of Pharmaceutical Sciences and Research, Surampalem, Kakinada, EG, AP - 533 437, IN

Abstract

A reverse phase high performance liquid chromatographic method was developed for the simultaneous determination of Ezetimibe and Fenofibrate in bulk and pharmaceutical dosage forms. The determination was performed by using Waters Symmetry Inertsil ODS (250×4.6mm×5μ) as stationary phase and Methanol: Acetonitrile: Water in the ratio of (80:10: 10 %v/v/v) as mobile phase. The flow rate of mobile phase was optimized as 1mL/min and effluents were monitored at 251nm. The retention time of Ezetimibe and Fenofibrate were found as 3.23min and 6.48min respectively. The method shows linearity in the concentration range of 6-14 μg/mL and 87-203 μg/mL respectively. The developed method was validated for specificity, precision, linearity, accuracy, robustness, Ruggedness, LOD and LOQ. Recovery of Ezetimibe and Fenofibrate in formulations was found to be in the range of 98.07-101.94% and 98.45-101.40% respectively conforms the non-interferences of the excepients in the formulation. Due to its simplicity, rapidness and high precision, the proposed RP- HPLC method can be used for the simultaneous determination of these two drugs in Quality control department for regular analysis.

Keywords

RP-HPLC, Ezetimibe and Fenofibrate.

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Sathish Kumar Konidala ¹, Adinarayana Penumala ¹, Vinod Kumar Mugada ¹, Govinda Rao Kamala ¹

Affiliations
1 Aditya Institute of Pharmaceutical Scienecs and Research, Surampalem, Kakinada, East Godawary, Andhra Pradesh – 533 437, IN

Abstract

A simple, validated RP-HPLC method for the simultaneous estimation of Paracetamol and Flupirtine maleate in pharmaceutical dosage form was developed and validated. This method was developed by selecting Inertsil, C18, (250 x 4.6mm, 5μ) column as stationary phase and Methanol: O-Phosporic acid (85: 15 v/v) as mobile phase. Flow rate of mobile phase was maintained at 1 ml/min at ambient temperature throughout the experiment. Quantification was achieved with ultraviolet (DAD) detection at 239 nm. The retention times of Paracetamol and Flupirtine maleate were found as 2.78 min and 3.47 min respectively. The detector response was linear in the concentration range of 65-190 μg/ml and 20-60 μg/ml for Paracetamol and Flupirtine maleate respectively, and the regression coefficients found as 0.998 and 0.999 for Paracetamol and Flupirtine maleate respectively. From recovery studies we concluded that the recovery of Paracetamol and Flupirtine maleate has no interference with any excepients in the formulation. This method has been validated according to ICH guidelines and shown to be Specific, Sensitive, Precise, Accurate, Rugged and Robust. Hence, this method can be applied for routine quality control of Paracetamol and Flupirtine maleate in dosage forms as well as in bulk drug.

Keywords

Paracetamol And Flupirtine Maleate, RP-HPLC, Analytical Method Validation, Lupirtine- P Tablets.

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Sravani Koralla ¹, Sathish Kumar Konidala ², K. Govinda Rao ¹, Sheik Mobina Begum ²

Affiliations
1 Department of Pharmaceutical Chemistry, Aditya Pharmacy College, Surampalem, E.G., A.P., 533347, IN
2 Department of Pharmaceutical Analysis and Quality Control, Aditya Pharmacy College, Surampalem, E.G., A.P., 533347, IN

Abstract

A simple and accurate stability indicating RP-HPLC method for the simultaneous estimation of Ramipril and amlodipine besylate in pharmaceutical dosage form was developed and validated. The separation of selected drugs was done by using, X-Bridge C18 (150 x 4.6 mm, 5μ) column as stationary phase and a mixture of 5 mM Ammonium acetate(45): ACN(55): 0.1%formic acid(0.5) as mobile phase. Flow rate of mobile phase was maintained at 1 ml/min at ambient temperature throughout the experiment. Quantification was achieved with ultraviolet (DAD) detection at 240 nm. The retention times of Ramipril and amlodipine besylate were found as 5.653minutes and 6.944 minutes respectively. The detector response was linear in the concentration range of 4- 12μg/ml for both drugs and the regression coefficients found as 0.9999 and 0.9998 for Ramipril and amlodipine respectively. This method was found free of any interference from any excipients. The percentage recovery values for Ramipril and amlodipine was found to be in the range of 98.83-101.09% and 98.40-100.13%. The Ramipril and amlodipine subjected to stress conditions including acidic, alkaline, oxidation, photolysis and thermal degradation. Ramipril and amlodipine besylate were more sensitive towards alkali and oxidative degradation. The developed method has been optimized and validated according to ICH guidelines and shown to be Specific, Sensitive, Precise, Accurate, Rugged and Robust. Hence, this method can be applied for routine quality control of Ramipril and amlodipine besylate in dosage forms as well as in bulk drug.

Keywords

Ramipril, Amlodipine Besylate, Simultaneous Estimation, RP-HPLC, Stability Indicating, Validation.

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