超高效液相色谱-串联质谱法同时测定蜂蜜中16种生物碱  

Simultaneous determination of 16 kinds of alkaloids in honey by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：刘先军[1] 冯家力[1] 曾栋[1] 陈东洋[1] 李帮锐[1] 张昊[1] 周丽平[1] 李谭瑶[1] LIU Xianjun;FENG Jiali;ZENG Dong;CHEN Dongyang;LI Bangrui;ZHANG Hao;ZHOU Liping;LI Tanyao(Hunan Provincial Center for Disease Control and Prevention,Changsha,Hunan 410003,China)

机构地区：[1]湖南省疾病预防控制中心,湖南长沙410003

出　　处：《实用预防医学》2023年第8期922-926,共5页Practical Preventive Medicine

基　　金：食物中毒诊断溯源技术北京市重点实验室开放基金(2018BZ0063-01)。

摘　　要：目的建立超高效液相色谱-串联质谱方法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定蜂蜜中吡咯里西啶类、雷公藤类、马桑内酯和异喹啉类共16种生物碱。方法样品加水超声提取过膜后,以苯基色谱柱分离,甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱,在电喷雾正离子(ESI+)模式下采用多反应监测模式(multiple reactions monitoring,MRM)进行测定。基质匹配标准曲线法定量。结果目标化合物在给定的线性范围内线性关系良好,r均≥0.99;方法的定量限为0.005~5μg/kg;3个不同浓度加标水平下,该方法平均回收率范围为60.5%~117.5%,相对标准偏差在0.8%~8.7%之间。采用该方法对40份蜂蜜样品进行检测,其中15份样品检出了小檗碱,含量为0.05~4.61μg/kg;三份样品检出千里光菲林,含量分别为14.3、17.6和17.8μg/kg。结论该方法操作简单,回收率高,重现性好,适用于蜂蜜中多种生物碱的同时测定。Objective To develop a method for simultaneous determination of 16 kinds of alkaloids including pyrrolizidine,Tripterygium wilfordii Hook.F.,coriaria lactone and isoquinoline in honey samples by using ultra performance liquidchromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The honey samples were extracted with 0.1%formic water,and then separated on a Waters Phenyl column by gradient elution methanol with 0.1%formic acid as mobile phase.The detection of alkaloids was performed by using electrospray ionization in positive ion mode(ESI+)with multiple reactions monitoring(MRM)mode.Quantification was performed using the matrix-matched calibration curves.Results The linearity of the calibration curves of all alkaloids was observed within a given linear range with good correlation coefficients(r≥0.99).The limits of quantification were 0.005-5μg/kg.The average recoveries for alkaloids in honey samples at three different spiked concentration levels ranged from 60.5%to 117.5%,with relative standard deviations of 0.8%-8.7%.The method established was used to determine 40 honey samples,and berberine was detected in 15 samples,with the concentrations ranging from 0.05-4.61μg/kg.Seneciophylline was contained in 3 samples,with the concentrations being 14.3μg/kg,17.6μg/kg and 17.8μg/kg respectively.Conclusion The method developed has the advantages of simple operation,high recoveries and good reproducibility,and it is suitable for simultaneous determination of alkaloids in honey.

关 键 词：蜂蜜 超高效液相色谱-串联质谱法 生物碱 吡咯里西啶 雷公藤 马桑内酯 异喹啉 

分 类 号：O657.63[理学—分析化学] R155.5[理学—化学]