Next Article in Journal
Development and Validation of a Gas Chromatography Method for the Trace Level Determination of Allylamine in Sevelamer Hydrochloride and Sevelamer Carbonate Drug Substances
Previous Article in Journal
Isolation and Evaluation of the Enantiospecific Antitubercular Activity of a Novel Triazole Compound
 
 
Scientia Pharmaceutica is published by MDPI from Volume 84 Issue 3 (2016). Previous articles were published by another publisher in Open Access under a CC-BY (or CC-BY-NC-ND) licence, and they are hosted by MDPI on mdpi.com as a courtesy and upon agreement with Austrian Pharmaceutical Society (Österreichische Pharmazeutische Gesellschaft, ÖPhG).
Font Type:
Arial Georgia Verdana
Font Size:
Aa Aa Aa
Line Spacing:
Column Width:
Background:
Article

Development and Validation of a Stability-Indicating RP-HPLC Method for the Estimation of Drotaverine Impurities in API and Pharmaceutical Formulation

*
Author to whom correspondence should be addressed.
Sci. Pharm. 2014, 82(1), 99-116; https://doi.org/10.3797/scipharm.1309-06
Submission received: 16 September 2013 / Accepted: 21 October 2013 / Published: 21 October 2013

Abstract

A sensitive, stability-indicating gradient RP-HPLC method with PDA detection has been developed for the simultaneous analysis of drotaverine impurities in active pharmaceutical ingredient (API) and pharmaceutical formulations. Efficient chromatographic separation was achieved on an XTerra RP18, 150 × 4.6 mm, 5 μm column using gradient elution at 230 nm detection wavelength. The optimized mobile phase consisted of a 0.02 M potassium dihydrogen ortho-phosphate buffer of pH 3.0 as solvent A and acetonitrile as solvent B. The flow rate of the mobile phase was 1.0 mL min−1 with a column temperature of 25°C. The method showed linearity over the range of 0.251–10.033 μg/mL, 0.231–9.995 μg/mL, 0.230–10.089 μg/mL, 0.334–10.011 μg/mL, and 0.324–10.050 μg/mL for impurities 1, 2, 3, 4, and drotaverine, respectively, with a correlation coefficient greater than 0.999. The relative retention times and relative response factors of impurities 1, 2, 3, 4 were 0.36, 0.90, 1.42, 1.55 and 1.04, 0.84, 1.10, 1.30, respectively. The drotaverine formulation sample was subjected to the stress conditions of acid, base, oxidative, thermal, humidity, and photolytic degradation. Drotaverine was found to degrade significantly in peroxide, base, and heat stress conditions. The degradation products were well-resolved from drotaverine and its impurities. The peak purity test results confirmed that the drotaverine peak was homogenous and pure in all stress samples and the mass balance was found to be more than 98%, thus proving the stability-indicating power of the method. The developed method was validated according to ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, and robustness.
Keywords: Drotaverine; RP-HPLC; Stability-indicating; Impurities; ICH guidelines Drotaverine; RP-HPLC; Stability-indicating; Impurities; ICH guidelines

Share and Cite

MDPI and ACS Style

THUMMALA, V.R.R.; THARLAPU, S.S.J.M.; REKULAPALLI, V.K.; IVATURI, M.R.; NITTALA, S.R. Development and Validation of a Stability-Indicating RP-HPLC Method for the Estimation of Drotaverine Impurities in API and Pharmaceutical Formulation. Sci. Pharm. 2014, 82, 99-116. https://doi.org/10.3797/scipharm.1309-06

AMA Style

THUMMALA VRR, THARLAPU SSJM, REKULAPALLI VK, IVATURI MR, NITTALA SR. Development and Validation of a Stability-Indicating RP-HPLC Method for the Estimation of Drotaverine Impurities in API and Pharmaceutical Formulation. Scientia Pharmaceutica. 2014; 82(1):99-116. https://doi.org/10.3797/scipharm.1309-06

Chicago/Turabian Style

THUMMALA, Veera Raghava Raju, Satya Sankarsana Jagan Mohan THARLAPU, Vijay Kumar REKULAPALLI, Mrutyunjaya Rao IVATURI, and Someswara Rao NITTALA. 2014. "Development and Validation of a Stability-Indicating RP-HPLC Method for the Estimation of Drotaverine Impurities in API and Pharmaceutical Formulation" Scientia Pharmaceutica 82, no. 1: 99-116. https://doi.org/10.3797/scipharm.1309-06

Article Metrics

Back to TopTop