柱前手性衍生化反相高效液色谱分离酮洛芬对映体

 目的：建立柱前手性衍生化反相高效液相色谱法分离酮洛芬对映体的方法。方法：分别以二氯亚砜和1，l′-羰基二咪唑为酰化剂，R-(+)-a-甲基苄胺作为柱前手性衍生化试剂，甲醇-0.025 mol·L〈sup〉-1〈/sup〉，磷酸二氢钾溶液(70：30)作流动相，在Shim-Pack LC-ODS柱上反相色谱分离酮洛芬对映体衍生物，柱温，室温。结果：在选定的条件下，酮洛芬的对映体衍生物得到分离，并确认了R-(一)-和S-(+)-两个衍生物的色谱峰。结论：通过统化，再以R-(+)-a-甲基苄胺为柱前手性衍生化试剂，用反相色谱法，实现了对酮洛芬对映体的分离。

Separation of enantiomeric ketoprofen by pre-column chiral derivatization reversed-phase HPLC

OBJECTIVE:To establish a pre column chiral derivatization reversed phase high performance liquid chromatographic method for the separation of ketoprofen enantiomers.METHODS:Thionyl chloride and 1,1′carbonyldiimidazole were chosen as the reagents for acylation,respectively.R(+)αmethylbenzylamine as the reagent for pre column chiral derivation to give two diastereomeric acylamide derivatives.These derivatives were separated on a Shim Pack CLC-ODS column using MeOH 0.025 mol·L_-1KH2PO4(70∶30) as the mobile phase and detected by UV detector at a wavelength of 254 nm.RESULTS:Two diastereomeric acylamide derivatives were effectively separated under the chosen conditions,and two peaks were determined.CONCLUSION:A simple highly sensitive method for the separation of ketoprofen was established.It may be a suitable analysis method for ketoprofen enantiomers pharmacology studies.It may also be a purity detective method for ketoprofen eanantiomers.