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

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 QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry （QuEChERS-UPLC-MS/MS）.MethodsHoney 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.ResultsTriptolide had a good linearity in the range of 10~200μg/L with the correlation coefficient of 0.998, and the limit of detection was 0.3μg/kg. The average recoveries spiked at 3 levels of 20, 50 and 100μg/kg were 88.1%~107.0% with the relative standard deviations （RSDs） no more than 13.4%.ConclusionThe established method is rapid and accurate, which can meet the requirements of determination of triptolide in honey samples.