title: A validated stability-indicating normal phase LC method for clopidogrel bisulfate and its impurities in bulk drug and pharmaceutical dosage form.
abstract: A novel stability-indicating normal phase liquid chromatographic (NP-LC) method was developed for the determination of purity of clopidogrel drug substance and drug products in bulk samples and pharmaceutical dosage forms in the presence of its impurities and degradation products. This method is capable of separating all the related substances of clopidogrel along with the chiral impurities. This method can be also be used for the estimation of assay of clopidogrel in drug substance as well as in drug product. The method was developed using Chiralcel OJ-H (250mmx4.6mm, 5microm) column. n-Hexane, ethanol and diethyl amine in 95:5:0.05 (v/v/v) ratio was used as a mobile phase. The eluted compounds were monitored at 240nm. Clopidogrel bisulfate was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. The degradation products were well resolved from main peak and its impurities, proving the stability-indicating power of the method. The developed method was validated as per International Conference on Harmonization (ICH) guidelines with respect to specificity, limit of detection, limit of quantification, precision, linearity, accuracy, robustness and system suitability.
authors.affiliation: Dr. Reddy's Laboratories Ltd., IPDO, Bachupally, Hyderabad 500072, AP, India. dantu_durga@yahoo.com
authors.forename: Dantu
authors.initials: D
authors.lastname: Durga Rao
authors.forename: L
authors.initials: L
authors.lastname: Kalyanaraman
authors.forename: Shakil S
authors.initials: SS
authors.lastname: Sait
authors.forename: P
authors.initials: P
authors.lastname: Venkata Rao
mesh_terms: D002138:Calibration; D002853:Chromatography, Liquid / Q000592:standards; D000077144:Clopidogrel; D004340:Drug Contamination; D004355:Drug Stability; D005343:Fibrinolytic Agents / Q000032:analysis*; D017408:Guidelines as Topic; D006863:Hydrogen-Ion Concentration; D006868:Hydrolysis; D007536:Isomerism; D010084:Oxidation-Reduction; D010782:Photolysis; D010975:Platelet Aggregation Inhibitors / Q000032:analysis*; D015203:Reproducibility of Results; D013607:Tablets; D013678:Technology, Pharmaceutical / Q000379:methods* / Q000592:standards; D013696:Temperature; D013988:Ticlopidine / Q000031:analogs & derivatives* / Q000032:analysis
chemical_list: D005343:Fibrinolytic Agents; D010975:Platelet Aggregation Inhibitors; D013607:Tablets; D000077144:Clopidogrel; D013988:Ticlopidine