Stability-Indicating Micellar Liquid Chromatographic Method for the Determination of Clopidogrel. Application to Tablets and Content Uniformity Testing

Abstract

A simple, stability-indicating, reversed-phase micellar liquid chromatographic method was developed for the analysis of the antiplatelet drug clopidogrel. Clopidogrel was determined in presence of its carboxylic acid degradation product, namely; SR26334. The analysis was carried out using a 150 mm × 4.6 mm i.d., 5 µm particle size Nucleodur MN-C18 column. The Mobile phase used was a solution containing 0.15 M sodium dodecyl sulphate and 10% n-propanol and 0.3% triethylamine in 0.02 M phosphoric acid at pH = 3.0 pumped at a flow rate of 1 mL/min with UV-detection at 235 nm. The method showed good linearity in the range of 1-20 µg/mL with limit of detection (S/N = 3) 0.06 µg/mL (1.86 × 10⁻⁷ M). The suggested method was successfully applied for the analysis of clopidogrel in bulk and in commercial tablets with average recoveries of 99.67% ± 0.94%, and 100.27 ± 0.89%, respectively. The results were favorably compared to those obtained by a reference method. The proposed method was successfully applied to the content uniformity testing of tablets. The proposed method was also applied for the determination of clopidogrel in the presence of its co-administered drug, acetyl salicylic acid, with application to synthetic mixtures and prepared tablets.

Keywords:

• Clopidogrel
• Content uniformity testing
• Degradation
• Micellar liquid chromatography
• Stability-indicating
• Tablets

Notes

∗Cp is Clopidogrel.

∗∗Dg is the degradation product.

N.B. Each result is the average of three separate determinations.

∗Intra-day: within the day.

Inter-day: consecutive days.

Tabulated t- and F-values at p=0.05 are: 1.782 and 3.838, respectively [25].

Tabulated t- and F-values at p=0.05 are 1.943 and 9.277, respectively.