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目的以纤维素氨基甲酸脂作为手性固定相,研究佐米曲普坦的高效液相色谱手性拆分方法。方法对流动相的比例、柱温以及流速等进行了优化。采用ChiralcelOD柱(250mm×4.6mm,5μm),以正已烷-异丙醇-三乙胺(85:15:0.2,v/v)为流动相,流速为0.7ml·min-1,检测波长280nm,柱温30℃。结果用ChiralcelOD手性柱在拟定的色谱条件下可实现佐米曲普坦对映体的完全分离,分离度为1.6。R-(-)型先于S-(+)型出峰。结论流动相中异丙醇的含量由低向高变化时,有降低分离度的趋势;在流动相中增大三乙胺的比例对拆分较为有利;温度较高时,有利于对映体的分离;较低的流速可改善分离度,但会延长对映体的出峰时间。
OBJECTIVE To study the chiral separation method of zolmitriptan by HPLC using cellulose carbamate as chiral stationary phase. The method was optimized for the mobile phase ratio, column temperature and flow rate. Using a Chiralcel OD column (250 mm × 4.6 mm, 5 μm) with n-hexane-isopropanol-triethylamine (85:15: 0.2, v / v) as the mobile phase at a flow rate of 0.7 ml · min -1, 280nm, column temperature 30 ℃. Results The complete separation of the Zolmitriptan enantiomer was achieved with a Chiralcel OD chiral column under the proposed chromatographic conditions with a resolution of 1.6. The R - (-) type precedes the S - (+) type peak. Conclusion The isopropanol content in the mobile phase tends to decrease the resolution when the isopropanol content changes from low to high. Increasing the proportion of triethylamine in the mobile phase is more favorable for the resolution. At higher temperatures, ; Lower flow rates improve resolution but extend the enantiomer peak time.