Validated chiral chromatographic methods for clopidogrel bisulphate and its related substances in bulk drug and pharmaceutical dosage forms
-
Eman S. Elzanfaly
and
Maissa Y. Salem
Abstract
Two validated chromatographic methods developed for the analysis of S clopidogrel bisulphate in the presence of its related substances listed in the United States and British Pharmacopoeias including its inactive R enantiomer are described. The first method is a simple thin layer chromatographic (TLC) method where separation is performed on pre-coated silica gel 60 F254 plates using methanol/diethylamine/heptanes/water containing 20 mg vancomycin hydrochloride (7 : 7 : 1.5 : 0.5 vol. %) as a mobile phase. Rf values were found to be 0.69, 0.74, 0.78, 0.84 and 0.88 for R clopidogrel, S clopidogrel, related substances A, B1 and B2, respectively. The second method depends on the separation by HPLC on a Lux polysaccharide chiral column with UV detection at 220 nm using 0.1 vol. % diethyl amine in methanol pumped at a rate of 1 mL min−1. Retention times were found to be 1.90 min, 2.82 min, 3.00 min, 3.27 min and 3.71 min for the related substances A, B1, C which are clopidogrel R enantiomer, B2, and S clopidogrel, respectively. The proposed methods were validated in accordance with the ICH guidelines and successfully applied to the determination of S clopidogrel bisulphate in pure powder and dosage forms without interference from the excipients and to affirm the dosage form to be pure S clopidogrel and devoid of the R enantiomer, which is inactive.
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Institute of Chemistry, Slovak Academy of Sciences
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- A rapid LC-MS/MS method for determination of urinary EtG and application to a cut-off limit study
- Validated chiral chromatographic methods for clopidogrel bisulphate and its related substances in bulk drug and pharmaceutical dosage forms
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- Polyphenols, radical scavenger activity, short-chain organic acids and heavy metals of several plants extracts from “Bucharest Delta”
- Reaction of anhydrous zinc chloride with 2,3-thiophenedicarbaldehyde bis(semicarbazone) (2,3BSTCH2) and bis(thiosemicarbazone) (2,3BTSTCH2): Crystal structure of {[C6H5N2S]+[ZnCl3(C6H4N2S)]−} complex
- Synthesis and evaluation of a novel hydrophobically associating polymer based on acrylamide for enhanced oil recovery
- Synthesis of cardanol-based photo-active SET-LRP initiator and its application to preparation of UV-cured resin
- Preparation, characterization and ion adsorption properties of functionalized polystyrene modified with 1,4-phenylene diisocyanate and diethylenetriamine
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