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目的建立分散固相萃取-超高效液相色谱-串联质谱法(dispersive solid-phase extraction-ultra performance liquid chromatography-tandem mass spectrometry,DSPE-UPLC-MS/MS)测定蜂蜜中雷公藤甲素的方法。方法蜂蜜样品经乙酸乙酯提取,QuEChERS粉包吸附净化后,以等体积比的乙腈和0.1%甲酸水溶液为流动相,经Agilent Eclipse plus C_(18)色谱柱分离后以多反应监测模式进行质谱测定。结果雷公藤甲素在10~200μg/L线性范围内具有良好的线性关系,线性相关系数为0.998;检出限为0.3μg/kg,在20、50和100μg/kg 3个添加水平下加标的平均回收率为88.1%~107.0%,相对标准偏差≤13.4%。结论本方法快速准确,可适用于蜂蜜中雷公藤甲素的定性和定量分析。
Objective To establish a method for the determination of triptolide in honey by dispersive solid-phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (DSPE-UPLC-MS / MS) Methods The honey samples were extracted with ethyl acetate and purified with QuEChERS powder. The mobile phases were eluted with acetonitrile and 0.1% formic acid in an equal volume. The mobile phases were separated by Agilent Eclipse plus C_ (18) Determination. Results Triptolide had good linearity in the range of 10 ~ 200μg / L with a linear correlation coefficient of 0.998. The detection limit was 0.3μg / kg, and the spiked samples were spiked at the three addition levels of 20, 50 and 100μg / kg The average recovery was 88.1% ~ 107.0%, the relative standard deviation ≤ 13.4%. Conclusion The method is rapid and accurate and can be applied to qualitative and quantitative analysis of triptolide in honey.