高效液相色谱手性流动相添加剂法测定富马酸(R,R)-戊乙奎醚中3个光学异构体杂质的含量

Determination of Three Optical Isomer Impurities in(R,R)-Penehyclidine Fumarate by Reversed Phase High Performance Liquid Chromatography with Cyclodetrin as a Moble Phase Additive

目的建立拆分富马酸(R,R)-戊乙奎醚与其3个光学异构体的高效液相色谱分离方法,控制光学纯度。方法选用C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-0.05 mol.L-1磷酸二氢钾(含0.6%三乙胺和0.015 mol.L-1β-环糊精,pH为2.3)为流动相,柱温25℃,检测波长206 nm,流速1.0 mL.min-1。结果 3个光学异构体的检测灵敏度为9.0 ng,本方法可检出限量为0.09%的光学异构体杂质。结论本法可有效分离富马酸(R,R)-戊乙奎醚及其3个光学异构体,可用于控制本品光学纯度。

OBJECTIVE To establish a reversed phase high performance liquid chromatography （RP-HPLC） method for the chiral separation and determination of （R,R）-penehyclidine fumarate and its optical isomer impurities. METHODS The chiral separation was performed on a C18 （4. 6 mm × 250 mm, 5 um） with mobile phase consisting of acetonitrile-0.05 mol . L-1 phosphates buffer （0. 015 mol . L -1 β-cyclodextrin, 0. 6% triethylamine, pH 2. 3） at flow rate of 1.0 mL . min-1. The column temperature was set at 25℃. UV Detection wavelength was set at 206 nm. RESULTS The limit of detection （LOD） of three optical isomers was 0. 09%. The established chiral HPLC method was used for the quality control of （R, R）-penehyclidine fumarate. CONCLUSION The method can be used to check and control the optical isomer impurities in the chiral drug, （R ,R）-penehyclidine fumarate.