超高效液相色谱-串联质谱法同时测定陈年老茶中16 种真菌毒素残留

doi:10.7506/spkx1002-6630-20200611-157

食品科学 ›› 2021, Vol. 42 ›› Issue (2): 299-305.doi: 10.7506/spkx1002-6630-20200611-157

超高效液相色谱-串联质谱法同时测定陈年老茶中16 种真菌毒素残留

刘文静，黄彪，傅建炜，韦航，黄财标

（福建省农业科学院农业质量标准与检测技术研究所，福建省农产品质量安全重点实验室，福建省茶叶质量检测与技术推广中心，福建福州 350003）

出版日期:2021-01-18 发布日期:2021-01-27
基金资助:
福建省公益类项目（2017R1018-1）；福建省农业科学院杰出青年人才科技创新基金项目（JC2017-1）；福建省农科院农产品质量安全创新团队项目（STIT2017-1-12）

Simultaneous Determination of 16 Mycotoxin Residues in Aged Tea by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

LIU Wenjing, HUANG Biao, FU Jianwei, WEI Hang, HUANG Caibiao

(Fujian Key Laboratory of Agro-products Qualitiy & Safety, Fujian Provincial Center of Tea Quality Inspection and Technology Promotion, Institute of Quality Standards and Testing Technology of Agro-products, Fujian Academy of Agricultural Sciences, Fuzhou 350003, China)

Online:2021-01-18 Published:2021-01-27

摘要/Abstract

摘要： 建立一种超高效液相色谱-串联质谱法测定不同种类陈年老茶中16 种真菌毒素的方法。样品经甲酸-乙腈（10∶90，V/V）溶液提取，提取液加入QuEChERS盐包振摇离心，过OASIS PRIME HLB小柱和dSPE净化管处理，以ACQUITY UPLC HSS T3 C18色谱柱分离，采用电喷雾正离子的多反应离子监测模式，茶叶基质匹配标准溶液。结果显示：16 种真菌毒素在各自浓度范围内呈良好线性关系（R＞0.999）；在茶叶基质中3 个不同添加水平下的加标回收率在63.4%～109.7%之间，相对标准偏差为1.7%～11.3%，方法检出限为0.03～7.00 μg/kg。选取了121 份陈年老茶样品进行检测，1 份乌龙茶样品检出黄曲霉毒素B1，含量为34.0 μg/kg，1 份红茶样品检出赭曲霉毒素A，含量为1.6 μg/kg。本方法稳定、准确、灵敏、快速，能够满足各种茶叶样品中多毒素残留分析的需求。

关键词: 超高效液相色谱-串联质谱法；陈年老茶；真菌毒素

Abstract: An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of 16 mycotoxins from different types of aged tea. The sample was extracted with formic acid-acetonitrile (10:90, V/V), added with a blend of QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction salts, shaken and centrifuged; the extract was cleaned up by passing through an OASIS PRIME HLB cartridge and a dispersive solid-phase extraction (dSPE) purification tube, separated on an ACQUITY UPLC HSS T3 C18 column, detected using an electrospray ionization source in the positive ion multiple reaction monitoring (MRM) mode, and quantified using tea matrix matching standard solution. The 16 mycotoxins showed a good linear relationship within their respective concentration ranges with correlation coefficients > 0.999. The average recoveries from tea matrix spiked at three different levels ranged between 63.4% and 109.7%, with relative standard deviations (RSDs) between 1.7% and 11.3%. The method limits of detection (LODs) ranged from 0.03 to 7.00 μg/kg. Among 121 aged tea samples selected for analysis, aflatoxin B1 was detected from one oolong tea sample at a concentration of 34.0 μg/kg, and ochratoxin A was also detected from one black tea sample at a concentration of 1.6 μg/kg. The method proved to be stable, accurate, sensitive and fast, and could meet the requirements for the analysis of multiple toxic residues in a variety of tea samples.

Key words: ultra-high performance liquid chromatography-tandem mass spectrometry; aged tea; mycotoxins

中图分类号:

TS207.7

刘文静，黄彪，傅建炜，韦航，黄财标. 超高效液相色谱-串联质谱法同时测定陈年老茶中16 种真菌毒素残留[J]. 食品科学, 2021, 42(2): 299-305.

LIU Wenjing, HUANG Biao, FU Jianwei, WEI Hang, HUANG Caibiao. Simultaneous Determination of 16 Mycotoxin Residues in Aged Tea by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. FOOD SCIENCE, 2021, 42(2): 299-305.

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超高效液相色谱-串联质谱法同时测定陈年老茶中16 种真菌毒素残留

Simultaneous Determination of 16 Mycotoxin Residues in Aged Tea by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

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