模拟移动床（ SMB）色谱作为一种精确、高效的制备色谱技术引起研究者的极大关注。本文以 EnantioPak OD填料为手性固定相，正己烷-乙醇（70：30，v／v）为流动相，在四区模拟移动床上手性拆分甲霜灵外消旋体。采用旋光检测器研究甲霜灵异构体在手性柱上的洗脱顺序；探讨进样浓度、进样流速、各区流速和切换时间等条件对手性分离甲霜灵外消旋体的影响，并与制备色谱进行比较。结果表明：S-（+）-甲霜灵先于 R-（-）-甲霜灵被流动相洗脱，R-（-）-甲霜灵在色谱柱上的保留强于 S-（+）-甲霜灵；在线性和非线性条件下，模拟移动床都能很好地拆分甲霜灵外消旋体，在优化 SMB工艺条件下，S-（+）-甲霜灵和 R-（-）-甲霜灵的光学纯度都大于99％；在样品质量浓度为15 mg／mL的条件下，模拟移动床色谱分离的样品量显著高于制备色谱，而流动相消耗仅为后者的1／9。这对于发展大规模色谱拆分甲霜灵工艺具有良好的指导意义。
Due to some advantages such as high precision,high efficiency and low consump-tion of organic solvents, chromatographic separation technique by simulated moving bed ( SMB)has attracted considerable attention in the past decades. Herein,the enantioseparation of metalaxyl racemate on EnantioPak OD columns has been carried out by SMB chromatogra-phy with the mixture of hexane-ethanol(70:30,v/v). The elution order of two metalaxyl enan-tiomers under current chromatographic conditions was determined by HPLC with the optical rotation detector. Then,the influence of running parameters,such as the concentration,flow rate and switch time on the resolution of metalaxyl racemate has been studied in detail. In addi-tion,the separation results from SMB and the preparative chromatography have been compared under the same concentrations. The results showed that the retention of S-(+)-metalaxyl was weaker than R-(-)-metalaxyl and S-(+)-metalaxyl was eluted first. Most importantly,metalax-yl racemate was well separated by SMB chromatography under linear or non-linear conditions, and the purity of each enantiomer product was over 99%. Furthermore,the amount separated by SMB was much more than by the preparative chromatography with racemate concentration of 15 mg/mL,and the mobile phase consumption was one-ninth of the latter. In brief,these results provide us important information for the future development of large-scale
chromatographic separation of metalaxyl enantiomers.
参考文献
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