四种三唑类杀菌剂的超临界色谱手性分离  

Chiral separation of four triazole fungicides by supercritical fluid chromatography

作　　者：林春绵[1] 郑夏琼[1] 俞游 杨雪[1] 

机构地区：[1]浙江工业大学生物与环境工程学院,浙江杭州310032

出　　处：《浙江工业大学学报》2013年第5期473-477,共5页Journal of Zhejiang University of Technology

基　　金：浙江省自然科学基金资助项目(Y506264)

摘　　要：单一异构体对于研究手性药物的活性及毒性有着重要意义.以二氧化碳为流动相,使用超临界流体色谱,对四种三唑类杀菌剂在Chiralcel OD-H柱上进行对映体分离研究,考察了不同改性剂(甲醇、乙醇、异丙醇)种类及浓度对其对映体分离的影响并获得了最佳改性剂条件,且与Chiralpak IB柱上的分离效果做了比较.随着改性剂浓度的增加,容量因子逐渐减小,分离度总体上逐渐减小,分离因子的变化较为复杂.改性剂洗脱能力大小顺序为:异丙醇<乙醇<甲醇.硅氟唑、戊菌唑、烯效唑的最佳改性剂条件均为9%乙醇(体积分数),而多效唑则为5%甲醇(体积分数).以Chiralpak IB柱为手性固定相时拆分时间短,但是分离度降低.Obtaining single-enantiomers is essential for investigating the activity and toxicity of chiral medications. Enantiomeric separation of four triazole fungicides on Chiralcel OD-H column by supercritical fluid chromatography （SFC） was studied using CO2 as mobile phase. The effects of different types and concentrations of modifier （methanol, ethanol or 2-propanol） were investigated to obtain the best modifier condition for each compound. The results of two different columns, Chiralcel OD-H column and Chiralpak IB column, were compared. With higher modifier proportions, the capacity factor gradually decreased and the resolution basically decreased, but the change of separation factor was complicated. The ability of eluting enantiomers was in the order of 2-propanol〈ethanol〈methanol. The best modifier condition was 9 （ % ethanol （volume fraction） for Simeconazole, Penconazole and Uniconazole, and 5% volume fraction） for Paclobutrazol. The retention time was shorter and the resolution methanol decreasedwhen using Chiralpak IB column as chiral stationary phase.

关 键 词：三唑类杀菌剂 超临界色谱 对映体分离 手性固定性 

分 类 号：TQ455.4[化学工程—农药化工]