UPLC-ESI-MS-MS结合QuEChERS同时测定柑橘中的4 种真菌毒素

doi:10.7506/spkx1002-6630-201420034

食品科学

UPLC-ESI-MS-MS结合QuEChERS同时测定柑橘中的4 种真菌毒素

史文景1,2，赵其阳1，焦必宁1,2,3,*

1.农业部柑桔产品质量安全风险评估实验室（重庆），西南大学柑桔研究所，重庆 400712；
2.西南大学园艺园林学院，重庆 400715；3.国家柑桔工程技术研究中心，中国农业科学院柑桔研究所，重庆 400712

出版日期:2014-10-25 发布日期:2014-11-07
基金资助:
国家现代农业（柑桔）产业技术体系建设专项（CARS-27）；
“十一五”国家科技支撑计划项目（2007BAD47B07；2007BADB7B04）；
2014年国家柑桔产品质量安全风险评估项目（GJFP2014003）；农业部无公害农产品质量安全监测项目

Simultaneous Determination of Four Mycotoxins in Citrus Fruits by Ultra Performance Liquid Chromatography- Electrospray Ionization Tandem Mass Spectrometry Combined with Modified QuEChERS

SHI Wen-jing1,2, ZHAO Qi-yang1, JIAO Bi-ning1,2,3,*

1. Laboratory of Quality and Safety Risk Assessment for Citrus Products, Ministry of Agriculture, Citrus Research Institute,
Southwest University, Chongqing 400712, China; 2. College of Horticulture and Landscape Architecture, Southwest University,
Chongqing 400715, China; 3. National Citrus Engineering Research Center, Citrus Research Institute,
Chinese Academy of Agricultural Sciences, Chongqing 400712, China

Online:2014-10-25 Published:2014-11-07

摘要/Abstract

摘要：

建立同时检测柑橘中链格孢酚甲基乙醚、交链孢酚、腾毒素和橘青霉素4 种真菌毒素的QuEChERS-超高效液相色谱-质谱分析方法。待测样品经乙腈提取，无水MgSO4和NaCl脱水盐析，C18键合相分散萃取净化，以ACQUITY UPLC BEH C18液相色谱柱为分离柱，以0.1%甲酸溶液和乙腈作为流动相梯度洗脱，在电喷雾离子源电离、多反应监测模式条件下进行测定，外标法定量。该方法在5.0～200 μg/L范围内线性关系良好，相关系数（R2）不小于0.992 7，检出限为0.2～0.7 μg/kg。3 个不同加标水平的平均回收率为78.0%～103.3%，相对标准偏差为2.6%～10.6%。结果表明，该方法快速、准确、灵敏，适用于柑橘中4 种真菌毒素残留的快速确证检测。

关键词: 超高效液相色谱-电喷雾质谱, QuEChERS, 柑橘, 真菌毒素

Abstract:

A method was developed for simultaneous determination of four mycotoxins (aletrnariol monomethyl ether,
tentoxin, alternariol, and citrinin) in citrus fruits using ultra-performance liquid chromatography-tandem mass spectrometry
combined with optimized QuEChERS. Samples were extracted with acetonitrile, salted out with anhydrous MgSO4 and
NaCl, cleaned up with C18 and then analyzed using UPLC-MS-MS in multiple reaction monitoring (MRM) mode with
electrospray ionization. The separation of the target mycotoxins was performed on an ACQUITY UPLC BEH C18 liquid
chromatography column through gradient elution using a mobile phase consisting of acetonitrile and 0.1% formic acid
aqueous solution and the matrix-matched external standard calibration was used for quantitation. This method had a good
linearity in the concentration range of 5.0–200 μg/L with correlation coefficients (R2) more than 0.992 7, and the limit of
detection of the established method was in the range of 0.2–0.7 μg/kg. The average recoveries of the four mycotoxins in
different matrixes (citrus pulp, peel and whole fruit) at three spiked levels ranged from 78.0% to 103.3%, with relative
standard deviations (RSDs) of 2.6%–10.6%. This method is simple, quick, accurate, sensitive, and suitable for the quick
confirmation and quantitative determination of the four mycotoxins in citrus fruits.

Key words: ultra-high liquid chromatography-electrospray ionization tandem mass spectrometry, QuEChERS, citrus, mycotoxins

中图分类号:

TS207.3

史文景1,2，赵其阳1，焦必宁1,2,3,*. UPLC-ESI-MS-MS结合QuEChERS同时测定柑橘中的4 种真菌毒素[J]. 食品科学, doi: 10.7506/spkx1002-6630-201420034.

SHI Wen-jing1,2, ZHAO Qi-yang1, JIAO Bi-ning1,2,3,*. Simultaneous Determination of Four Mycotoxins in Citrus Fruits by Ultra Performance Liquid Chromatography- Electrospray Ionization Tandem Mass Spectrometry Combined with Modified QuEChERS[J]. FOOD SCIENCE, doi: 10.7506/spkx1002-6630-201420034.

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UPLC-ESI-MS-MS结合QuEChERS同时测定柑橘中的4 种真菌毒素

Simultaneous Determination of Four Mycotoxins in Citrus Fruits by Ultra Performance Liquid Chromatography- Electrospray Ionization Tandem Mass Spectrometry Combined with Modified QuEChERS

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