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Separation Enantiomers Of Dihydropyridine Calcium Antagonists By High Performance Liquid Chromatography As Pre-Column Derivatizing Reagent And Quantitative Analysis Of Clofencet Methyl Ester By High Performance Liquid Chromatography

Posted on:2011-03-30Degree:MasterType:Thesis
Country:ChinaCandidate:L LuFull Text:PDF
GTID:2154330338977971Subject:Drug analysis
Abstract/Summary:PDF Full Text Request
Many chiral drugs may differ in vivo pharmacokinetics and pharmacodynamics due to the difference of stereochemistry. Therefore,a rapid and sensitive method for enantiomers separated is of great importance. Currently, high performance liquid chromatography method has been widely used in optical resolution of enantiomers, and has been become a practical and useful method not only for determining optical purity but also for obtaining optical isomers. In this paper the enantiomeric separation of 1,4 Dihydropyridine Calcium Antagonists has been investigated by high performance liquid chromatography as non chiral pre column derivatizing reagent.In part one, gives a general review about dihydropyridine calcium antagonists with the clinical application, mechanism, structure activity relationship,and the main reseaches on enantiomeric separation of dihydropyridine calcium Antagonists at home and abroad. Basically, the commonly methods used in enantiomer separation and types of CSP were introduced.In part two, dihydropyridine calcium antagonists enantiomeric separation with Chiralcel OD-H by high performance liquid chromatography were presented. Enantiomers of five Dihydropyridine Calcium Antagonists were separated on Chiralcel OD-H in degrees. Cilnidipine and manidipine hydrochloride were completely separated, nimodipine, nisoldipine and nicardipine hydrochloride were partially separated. Then, dihydropyridine calcium antagonists were non chiral pre column derivatizated. The derivatives with Chiralcel OD-H by high performance liquid chromatography were presented. Some of derivatives were completely separated, such as Amlodlpine Cilnidipine and Manidipine. A part of derivatives were partially separated, such as nimodipines, nisoldipine and nicardipine. Preliminary discussed chiral recognition mechanism of dihydropyridine calcium antagonists on the Chiralcel OD-H.In part three, a method for quantitative analysis of clofencet methyl ester, was established by high performance liquid chromatography. Kromasil C8 column was used with UV detection at 274 nm and with a mobile phase consisting of acetonitrile and water (50:50, by vol) at a flow rate of 1.0 mL min-1. The linear range of the method was 30.0 70.0 mg L-1 (liner correlation coefficient 0.9998), the limit of detection was 0.09 mg L-1, the limit of quantitative was 0.3 mg L-1, the average recovery of clofencet methyl ester was 98.0 100%, with RSD of 0.37 1.56%. This method is simple, specific, sensitive. It is suitable for investigating clofencet methyl ester.
Keywords/Search Tags:Dihydropyridine Calcium Antagonists, Enantiomer separation, pre column derivatization, Clofencet methyl ester
PDF Full Text Request
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