THE COMPARISON OF TWO VALIDATED HPLC METHODS FOR THE DETERMINATION OF (+)-CLOPIDOGREL HYDROGENSULFATE PURITY WITH THE USP METHOD.

Anna Bielejewska 1,2Wioleta Maruszak 1Lidia Rozmarynowska 1Hanna M. Beczkowicz 1

1. Pharmaceutical Research Institute (IF), Rydygiera 8, Warszawa 01-793, Poland
2. Polish Academy of Sciences, Institute of Physical Chemistry, Kasprzaka 52/56, Warszawa 01-224, Poland

Abstract

The comparison of two validated high performance liquid chromatography (HPLC) methods for the determination of chemical impurities and enantiomeric purity of (+)-clopidogrel hydrogensulfate with the USP method is presented.

The determination using the developed methods were performed on Nova-Pak Phenyl and Chiral AGP columns. The selectivity of the method of chemical impurities determination was demonstrated for 6 analytes: impurity A (RRT 0.5), D (RRT 0.7), B (RRT 1.3), E (RRT 1.7), substrate Cl-5 (RRT 0.4) and clopidogrel. Method for chemical impurities determination and method for chiral analysis are linear with R2 = 0.999 and R2 = 0.996 and precise with RSD 1.4 % and 2.3, respectively. The LOQ and LOD were calculated respectively on the 0.02 % and 0.006 % for chemical impurities and LOQ = 0.3 % for (-)-clopidogrel determination. Both methods are not affected by broad range of changes of chromatographic parameters, thus proving their robustness.

The developed method for chiral analysis allows to obtain the results as good as using USP method. However, concerning the chemical impurities determination the developed method presents much better selectivity than USP method.

 

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Presentation: Poster at V Multidyscyplinarna Konferencja Nauki o Leku, by Wioleta Maruszak
See On-line Journal of V Multidyscyplinarna Konferencja Nauki o Leku

Submitted: 2006-01-11 07:04
Revised:   2009-06-07 00:44