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
李玉芳 1焦洁 1黄铮 1肖锋 2黄远飞 2王青 1柳利龙 3张环1
作者信息
- 1. 甘肃省农业科学院畜草与绿色农业研究所,甘肃 兰州 730070;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
- 2. 文山三七数字本草检验中心有限公司,云南 文山 663000
- 3. 甘肃省农业科学院小麦研究所,甘肃 兰州 730070
- 折叠
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(R2>0.995 0),方法的检出限 0.04～1.43 μg/kg,定量限 0.12～4.75 μg/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B1(AFTB1)、黄曲霉毒素B2(AFTB2)、黄曲霉毒素G1(AFTG1).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.
Abstract
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(R2>0.995).The detection limits were 0.04 to1.43 μg/kg,and the quantification limits were 0.12 to 4.75 μg/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 AFTB1,AFTB2 and AFTG1.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Key words
Angelica sinensis/Chinese medicinal material/Mycotoxin/Ultra high performance liquid chromatography-tan-dem mass spectrometry/Method validation引用本文复制引用
基金项目
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)
出版年
2024
国家科技期刊平台
NSTL
万方数据