超高效液相色谱-串联质谱法同时测定当归9种真菌毒素  

Simultaneous Determination of 9 Mycotoxins in Angelica sinensis by Ultra High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：李玉芳[1,2] 焦洁[1,2] 黄铮[1,2] 肖锋 黄远飞 王青[1,2] 柳利龙 张环[1,2] LI Yufang;JIAO Jie;HUANG Zheng;XIAO Feng;HUANG Yuanfei;WANG Qing;LIU Lilong;ZHANG Huan(Institute of Animal Husbandry,Pasture and Green Agriculture,Gansu Academy of Agricultural Sciences,Lanzhou Gansu 730070,China;Institute of Agricultural Quality Standards and Testing Technology,Gansu Academy of Agricultural Sciences,Lanzhou Gansu 730070,China;Wenshan Sanqi Digital Materia Medica Inspection Centre Co.,Ltd.,Wenshan Yunnan 663000,China;Wheat Research Institute,Gansu Academy of Agricultural Sciences,Lanzhou Gansu 730070,China)

机构地区：[1]甘肃省农业科学院畜草与绿色农业研究所,甘肃兰州730070 [2]甘肃省农业科学院农业质量标准与检测技术研究所,甘肃兰州730070 [3]文山三七数字本草检验中心有限公司,云南文山663000 [4]甘肃省农业科学院小麦研究所,甘肃兰州730070

出　　处：《寒旱农业科学》2024年第10期974-980,共7页Journal of Cold-Arid Agricultural Sciences

基　　金：甘肃省农业科学院农业科技创新专项(2020GAAS15);甘肃省自然科学基金计划项目(22JR5RA764)。

摘　　要：通过优化液相色谱条件和质谱条件等,建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定当归中药材中9种真菌毒素的检测方法。样品经70%甲醇溶液超声提取,经固相萃取柱净化;采用流动相A:2 mmol/L甲酸铵0.1%甲酸水溶液;流动相B:甲醇,经C18色谱柱分离后注入质谱仪,电喷雾电离源(ESI)和多反应监测模式(MRM)进行检测,基质外标法定量。经方法学验证,9种真菌毒素标准曲线线性关系良好(R^(2)>0.9950),方法的检出限0.04~1.43μg/kg,定量限0.12~4.75μg/kg,高、中、低3个浓度加标回收率为77.8%~113.6%,测定结果的相对标准偏差为0.2%~17.7%。该检测方法应用于72批当归样品9种真菌毒素同时检测,2批当归样品检出真菌毒素,检出率为2.8%,样品中主要的污染真菌毒素为黄曲霉毒素B_(1)(AFTB_(1))、黄曲霉毒素B2(AFTB_(2))、黄曲霉毒素G_(1)(AFTG_(1))。本研究建立的方法具有预处理简便、经济等优点,适用于当归样品9种真菌毒素的快速检测。An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of 9 mycotoxins in Angelica sinensis was established by optimizing the conditions of liquid chromatography and mass spectrometry.The samples were extracted by ultrasonic extraction of 70%methanol solution and purified by solid phase extraction column.Using mobile phase A,i.e.,0.1%formic acid solution(containing 2 mmol/L ammonium formate),and mobile phase B,i.e.,methanol,samples were separated by a C18 column and injected into a mass spectrometer,detected by ESI and multiple reaction monitoring mode(MRM),and quantified by matrix external standard.The linear relationship between the standard curves of the nine mycotoxins was good(R^(2)>0.995).The detection limits were 0.04 to1.43μg/kg,and the quantification limits were 0.12 to 4.75μg/kg.The recoveries of high,medium and low concentrations were 77.8%to 113.6%.The relative standard deviation of the results was 0.2%to17.7%.The method was applied to the simultaneous detection of mycotoxins in 72 batches of Angelica sinensis samples.Mycotoxins were detected in 2 batches of Angelica sinensis samples,with a detection rate of 2.8%.The main mycotoxins in Angelica sinensis samples were AFTB_(1),AFTB_(2) and AFTG_(1).The method established in this study has the advantages of simple pretreatment and economy,and is suitable for the rapid detection of 9 mycotoxins in Angelica sinensis samples.

关 键 词：当归 中药材 真菌毒素 超高效液相色谱-串联质谱法 方法验证 

分 类 号：S567.23[农业科学—中草药栽培]