利用酰胺型手性固定相高效液相色谱法对格列美脲顺反异构体的分离与测定

Direct Separation and Quantitative Determination of Transglimepiride by High Performance Liquid Chromatography Using an Amide Type Chiral Stationary Phase

利用高效液相色谱法在一种酰胺型手性固定相上直接分离了格列美脲顺反异构体。讨论了流动相组成、柱温度和流速等色谱条件对分离的影响。优化的实验条件为 :流动相组成正己烷 :1 ,2 二氯乙烷∶甲醇(88∶8∶4 ,V/V/V) ;柱温 :2 5℃ ;流速 :1 .8mL/min。得到的分离度和选择性因子分别为 1 .86和 1 .1 2。在 2 88～ 32 0mg/L的浓度范围内建立了反式格列美脲的标准曲线 ,线性系数为 0 .99998;检出限为 0 .4 7mg/L。方法简单 ,可靠 。

Trans- and cis-glimepiride were directly separated by a new established high performance chromatographic method, which involved the use of Chirex 3005 column. Several parameters were studied. Simple and reliable separation was achieved, with the separation factor (alpha) 1.12 and the resolution factor (R-s) 1. 86, when using the optimized mobile phase composed of n-hexane: 1,2-dicholoethane: methanol (88/8/4 by vol) at 25degreesC and 1.8 mL/min. Standard linear calibration curve was established for trans-glimepiride, over the range of 3 similar to 320 mg/L, with the correlation coefficient of 1. 0000. The minimum limit of detection was 0. 47 mg/L. Precision of the assay was gratifying and the method has been used to monitor and identify quantitatively the products of glimepiride.