超高效液相色谱-串联质谱法检测蜂蜜中 雷公藤甲素残留量

Determination of triptolide in honey by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  雷公藤甲素  分散固相萃取  高效液相色谱-串联质谱法  蜂蜜

英文关键词:triptolide  dispersive solid-phase extraction  ultra performance liquid chromatography-tandem mass spectrometry  honey

中文摘要:

      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 C18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10~200 μg/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0.3 μg/kg, 在20、50和100 μg/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。

英文摘要:

      Objective To establish a method for the determination of triptolide in honey by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (QuEChERS-UPLC-MS/MS). Methods Honey samples were extracted with ethyl acetate, adsorbed and purified with QuEChERS powder, separated by an Agilent Eclipse plus C18 column with the mobile phase of acetonitrile:0.1%formic acid (1:1, V:V), and then triptolide was detected by mass spectrometry under multiple reaction monitoring (MRM) mode. Results Triptolide had a good linearity in the range of 10~200 μg/L with the correlation coefficient of 0.998, and the limit of detection was 0.3 μg/kg. The average recoveries spiked at 3 levels of 20, 50 and 100 μg/kg were 88.1%~107.0% with the relative standard deviations (RSDs) no more than 13.4%. Conclusion The established method is rapid and accurate, which can meet the requirements of determination of triptolide in honey samples.