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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 high performance liquid chromatographic method for the separation of fumaric acid (R, R) -pentanil and its three optical isomers to control the optical purity. Methods The chromatographic column was C18 (4.6 mm × 250 mm, 5 μm) with acetonitrile-0.05 mol·L-1 potassium dihydrogen phosphate (containing 0.6% triethylamine and 0.015 mol·L-1β-cyclodextrin ) As the mobile phase, the column temperature was 25 ℃, the detection wavelength was 206 nm and the flow rate was 1.0 mL.min-1. Results The detection sensitivity of the three optical isomers was 9.0 ng. This method can detect the optical isomer impurities with the limit of 0.09%. Conclusion This method can effectively separate fumaric acid (R, R) - Penehyclidine and its three optical isomers and can be used to control the optical purity of this product.