液相色谱-串联质谱法同时测定动物血浆中21种霉菌毒素或其代谢物残留

引用本文: 王瑞国, 苏晓鸥, 王培龙, 张维, 薛岩, 李玉. 液相色谱-串联质谱法同时测定动物血浆中21种霉菌毒素或其代谢物残留[J]. 分析化学, 2017, 45(2): 231-237. doi: 10.11895/j.issn.0253-3820.160526 shu

Citation: WANG Rui-Guo, SU Xiao-Ou, WANG Pei-Long, ZHANG Wei, XUE Yan, LI Yu. Simultaneous Detection of 21 Kinds of Mycotoxins and Their Metabolites in Animal Plasma with Impurity Adsorption Purification Followed by Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2017, 45(2): 231-237. doi: 10.11895/j.issn.0253-3820.160526 shu

液相色谱-串联质谱法同时测定动物血浆中21种霉菌毒素或其代谢物残留

王瑞国 ^1, ,
苏晓鸥 ^1, ,
王培龙 ^1, ,
张维 ^1, ,
薛岩 ^2, ,
李玉 ^2,

1.
中国农业科学院农业质量标准与检测技术研究所, 农业部农产品质量安全研究重点实验室, 北京 100081;
2.
奥特奇生物制品(中国)有限公司, 北京 100600
基金项目:
本文系“十二五”农村领域国家科技计划（No.2011BAD26B0405）和公益性行业（农业）科研专项经费（No.201203088-01）资助

摘要: 建立了同时检测动物血浆中黄曲霉毒素B₁等21种霉菌毒素或其代谢物残留的液相色谱-串联质谱方法。动物血浆样品中加入0.1%甲酸-乙腈溶液、NaCl和无水MgSO₄进行萃取，无水MgSO₄和C₁₈，PSA，A-AL对提取液进行脱水净化，经浓缩、复溶和离心后，再进行测定。采用反相C₁₈色谱柱分离，以0.1%甲酸-0.5 mmol/L乙酸铵溶液和0.1%甲酸-甲醇溶液作为流动相进行梯度洗脱，采用电喷雾离子源（ESI）多反应监测离子模式（MRM）进行检测，基质标准曲线外标法进行定量分析，线性范围在0.05~100 ng/mL之间，方法的定量限为0.05~0.5 ng/mL。在高、中、低3个添加浓度水平下，21种霉菌毒素的平均回收率为62.0%~116.4%，相对标准偏差小于19%。

关键词:

English

Simultaneous Detection of 21 Kinds of Mycotoxins and Their Metabolites in Animal Plasma with Impurity Adsorption Purification Followed by Liquid Chromatography-Tandem Mass Spectrometry

1.
Institute of Quality Standards and Testing Technology for Agricultural Products, Chinese Academy of Agricultural Science, Key Laboratory of Agrifood Safety and Quality, Ministry of Agriculture, Beijing 100081, China;
2.
Alltech Biological Products(China) Co., LTD, Beijing 100600, China
Received Date: 09 July 2016
Revised Date: 19 September 2016
Fund Project:
This work was supported by the Planning Subject of the Twelfth Five-Plan National Science and Technology for the Rural Development in China (No.2011BAD26B0405)

Abstract: A novel method for simultaneous detection of mycotoxins (e.g., aflatoxin B₁) or their metabolic residues in animal plasma with impurity adsorption purification followed ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. Extraction of mycotoxins and their metabolites from animal plasma sample was performed with 0.1% formic acid-acetonitrile solution after addition of sodium chloride and hydrous magnesium sulfate. The extract was then dehydrated and purified with hydrous magnesium sulfate, C₁₈, primary secondary amine, and alumina-A. 3 mL of the supernatant was evaporated and re-dissolved with 0.5 mL of 0.1% formic acid aqueous solution/acetonitrile (70:30, V/V) for UPLC-MS/MS detection. The analytes were separated by a C₁₈ column utilizing gradient elution with 0.1% formic acid aqueous solution containing 0.5 mmol of ammonium acetate and 0.1% formic acid-methanol solution, and finally detected by tandem mass spectrometry in positive/negative ESI mode. Identification and quantification were achieved by LC-MS/MS with multi-reaction monitoring (MRM). Good linearity in response was obtained in the analytes concentration range of 0.05-100 ng/mL with correlation coefficients larger than 0.99. The limits of quantification (S/N=10) were around 0.05-0.5 ng/mL. The recoveries of mycotoxins and their metabolites spiked in blank plasma samples were in the range of 62.0%-116.4%, with relative standard deviations (RSDs) less than 19.0%.

Key words:

Liquid chromatography-tandem mass spectrometry
/ Plasma
/ Mycotoxins
/ Residue

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沈阳化工大学材料科学与工程学院沈阳 110142

液相色谱-串联质谱法同时测定动物血浆中21种霉菌毒素或其代谢物残留

English

Simultaneous Detection of 21 Kinds of Mycotoxins and Their Metabolites in Animal Plasma with Impurity Adsorption Purification Followed by Liquid Chromatography-Tandem Mass Spectrometry

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

液相色谱-串联质谱法同时测定动物血浆中21种霉菌毒素或其代谢物残留

English

Simultaneous Detection of 21 Kinds of Mycotoxins and Their Metabolites in Animal Plasma with Impurity Adsorption Purification Followed by Liquid Chromatography-Tandem Mass Spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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