hplc―elsd同时测定酸枣仁中6种成分的含量.docVIP

HPLC―ELSD同时测定酸枣仁中6种成分的含量 　　[摘要] 目的 建立同时测定酸枣仁中6种成分含量的高效液相色谱-蒸发光检测器（HPLC-ELSD）法。 方法 经70%乙醇超声提取80 min，采用Kromasil C18（250 mm×4.6 mm，5.0 μm）色谱柱进行分离，以乙腈-0.1%乙酸为流动相，梯度洗脱，流速为1.0 mL/min，柱温35℃；ELSD检测，载气流速为2.9 mL/min，漂移管温度为100℃，测定酸枣仁中斯皮诺素、酸枣仁皂苷A、酸枣仁皂苷D、酸枣仁皂苷B、酸枣仁皂苷B1和白桦脂酸6种成分的含量。回收率计算采用外标法，按峰面积计算。 结果 斯皮诺素、酸枣仁皂苷A、酸枣仁皂苷D、酸枣仁皂苷B、酸枣仁皂苷B1和白桦脂酸在各自质量浓度范围内与峰面积呈良好的线性关系（R20.9991）；平均加样回收率为94.91%～99.35%，RSD为0.78%～1.23%。不同产地酸枣仁中6种成分的含量差异较大，斯皮诺素和白桦脂酸的含量最高，3批样品中检测到酸枣仁皂苷B1。 结论 该方法简便、准确、重现性好，适用于酸枣仁中多成分的同时快速检测。 　　[关键词] 酸枣仁；多成分测定；高效液相色谱-蒸发光检测器 　　[中图分类号] R917 [文献标识码] A [文章编号] 1673-7210（2016）12（c）-0149-05 　　[Abstract] Objective To establish a HPLC-ELSD method for simultaneous determination of six compounds in ZiziphiSpinosae Semen. Methods The sample was extracted by ultrasonication for 80 min using 70% ethanol and the target compounds were separated on a Kromasil C18 chromatographic column （250 mm×4.6 mm， 5.0 μm）. A mixture of acetonitrile-water containing 0.1% acetic acid was utilized as the mobile phase at the flow rate of 1.0 mL/min， and the column temperature was set 35℃. The drift tube temperature of ELSD was 100℃ with carrier gas flow rate of 2.9 mL/min. The contents of spinosin， jujuboside A， juboside D， jujuboside B， jujuboside B1 and betulinic acid were determined on the above conditions. External standard method was used to measure recovery based on the peak areas. Results The six target analytes （spinosin， jujuboside A， jujuboside D， jujuboside B， jujuboside B1， betulinic acid） all exhibited good linear relationships （R2 0.9991） in their relatively wide concentration ranges. The average recoveries varied between 94.91% and 99.35% with RSD of 0.78%-1.23%. The contents of the six components in ZiziphiSpinosae Semen collected from different locations in China exhibited great variations. Spinosin and betulinic acid had the highest contents in all samples， and jujuboside B1 was only detected in three samples. Conclusion This established HPLC-ELSD method is simple， quick and accurate，