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目的:建立用于测定有机相中脂肪酶促进布洛芬与正辛醇立体选择性酯化反应转化率及对映体过量值的手性高效液相色谱方法。方法:通过变更流动相组成与配比,找到在Chiralcel OD手性柱上拆分外消旋布洛芬及其正辛酯对映体的最佳色谱条件,建立各自对映体峰面积与浓度之间的校正关系。结果:以100％正己烷作流动相,布洛芬正辛酯的一对对映体可以分开,布洛芬则滞留在柱子上;当在正己烷中添加1％冰醋酸后,布洛芬对映体可以分开,但此时酯的对映体分不开。峰面积-浓度校正曲线表明,布洛芬及其正辛酯各对映体响应因子值相等。结论:可以用峰面积代替浓度,按有关公式算出布洛芬立体选择性酯化反应的转化率及对映体过量值。鉴于冰醋酸对柱子有害等原因,实际样品分析中直跟踪酯。
OBJECTIVE: To establish a chiral HPLC method for the determination of the conversion and enantiomeric excess of stereoselective esterification of ibuprofen and n-octanol by lipase in organic phase. Methods: The optimum chromatographic conditions for the separation of enantiomers of racemic ibuprofen and n-octyl ester from Chiralcel OD chiral column were found by changing the composition and proportion of mobile phases. The peak area and concentration Correction between the relationship. Results: With 100% n-hexane as the mobile phase, one pair of enantiomers of n-octyl ester of ibuprofen could be separated and ibuprofen was retained on the column. After adding 1% glacial acetic acid to n-hexane, Enantiomers can be separated, but the ester enantiomer can not be separated at this time. The peak area-concentration calibration curve shows that the enantiomer response factors for ibuprofen and n-octyl ester are equal. Conclusion: The peak area can be used in place of the concentration, and the conversion and enantiomeric excess of the stereoselective esterification of ibuprofen can be calculated according to the formula. In view of the glacial acetic acid is harmful to the column and other reasons, the actual sample analysis straight trace esters.