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目的采用有机液体分散液相微萃取对五味子药材提取液进行纯化富集,建立分散液相微萃取结合HPLC测定五味子甲素和五味子酯甲的含量。方法分散液相微萃取以60μL四氯化碳为萃取剂,供相pH为1,萃取4 min,以转速1 500 r.min~(-1)离心2 min。在上述优化条件下,对五味子药材提取液进行萃取后,以C_(18)柱为固定相、甲醇-0.6%磷酸溶液(69︰31)为流动相、检测波长254 nm进行色谱分析。结果分散液相微萃取对五味子甲素和五味子酯甲的富集倍数分别为5 112和1 118,线性范围在0.10~19μg·m L~(-1)之间,回收率分别为100.1%和94.4%。结论本法灵敏度高、重现性好,简便、快速、环保,可用于五味子药材中五味子甲素和五味子酯甲的含量测定。
OBJECTIVE To purify and enrich the extracts of Schisandra chinensis by liquid-liquid phase microextraction and determine the contents of Schisandrin A and Schisandra ester A by means of dispersive liquid phase microextraction combined with HPLC. Methods Dispersive liquid-phase microextraction with 60μL of carbon tetrachloride as extractant for phase pH 1, extraction 4min, at a speed of 1500 r.min ~ (-1) centrifugation 2 min. Under the optimized conditions, the extract of Schisandra chinensis was extracted with C 18 column and methanol-0.6% phosphoric acid solution (69:31) as the mobile phase at a detection wavelength of 254 nm for chromatographic analysis. Results The enrichment ratios of schisandrin A and schisandrins A by liquid-liquid microextraction were 5 112 and 1 118, respectively. The linear range was 0.10-19 μg · m L -1 and the recoveries were 100.1% and 94.4%. Conclusion This method has high sensitivity, good reproducibility, simple, rapid, environmental protection, and can be used for the determination of schisandrin A and Schisandra ester A in Schisandra sp.