填充柱超临界流体色谱手性拆分5-羟基-8-十一碳烯酸-δ-内酯(茉莉内酯)
Fine Chemicals(2013)
Abstract
研究了填充柱超临界CO2流体色谱手性拆分外消旋5-羟基-8-十一碳烯酸-δ-内酯(茉莉内酯)的方法。在筛选固定相种类及改性剂种类基础上,通过单因素及正交实验较为系统地考察了柱温、柱压、改性剂含量、流速等因素的影响,优化出较佳的分析型拆分条件:固定相Chiralcel OD-H,柱温31℃,柱压12 MPa,改性剂为乙腈-甲醇(体积比7∶3),在流动相中体积分数2.0%,流动相流速1.0 mL/min,分离度2.00。利用较佳条件,在流速8mL/min下进行制备规模放大,320 min内进样10 mg得6.6 mg两对映体产品,回收率66%,光学纯度(e.e%)均为100%,表明超临界流体色谱分离效率高,可作为茉莉内酯mg级对映体纯品快速制备的手段。
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Key words
Chiralcel OD,packed column supercritical fluid chromatography,chiral resolution,6-[(3E)-hexenyl]-2H-tetrahydro-pyran-2-one,flavor and fragrance,jasmolactone,5-hydroxy-8-undecenoic acid δ-lactone
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