A validated chiral LC method for the enantiomeric separation of repaglinide on immobilized amylose based stationary phase

摘要

A simple, rapid, isocratic, normal phase chiral HPLC method was developed and validated for the enantiomeric separation of repaglinide, (S)-(+)-2-ethoxy-4-N [1-(2-piperidinophenyl)-3-methyl-1-butyl] aminocarbonylmethyl] benzoic acid, an antidiabetic drug substance. The enantiomers of repaglinide were resolved on a Chiralpak IA (immobilized amylose based stationary phase) column using a mobile phase consisting of n-hexane:ethanol:trifluoroacetic acid (80:20:0.2, v/v/v) at a flow rate of 1.0 mL min-1. The resolution between both enantiomers was greater than 2 in the optimized method. The developed method was extensively validated and proved to be robust, enantioselective, accurate, precise, and suitable for quantitative determination of (R)-enantiomer in bulk drug substance and product.