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作物学报 ›› 2014, Vol. 40 ›› Issue (04): 691-701.doi: 10.3724/SP.J.1006.2014.00691

• 耕作栽培·生理生化 • 上一篇    下一篇

用超高效液相色谱串联质谱法同时测定谷物中12种真菌毒素

孙娟,李为喜,张妍,孙丽娟,董晓丽,胡学旭,王步军*   

  1. 中国农业科学院作物科学研究所 / 农业部谷物品质监督检验测试中心，北京100081
  • 收稿日期:2013-08-28 修回日期:2014-01-12 出版日期:2014-04-12 网络出版日期:2014-02-14
  • 通讯作者: 王步军, E-mail: wangbujun@caas.cn
  • 基金资助:

    本研究由谷物产品(水稻、小麦)质量安全普查项目(农办质[2012]19号)资助。

Simultaneous Determination of Twelve Mycotoxins in Cereals by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

UN Juan,LI Wei-Xi,ZHANG Yan,SUN Li-Juan,DONG Xiao-Li,HU Xue-Xu,WANG Bu-Jun*   

  1. Institute of Crop Science, Chinese Academy of Agricultural Sciences / Cereal Quality Supercision and Testing Center, Ministry of Agriculture, Beijing 100081, China
  • Received:2013-08-28 Revised:2014-01-12 Published:2014-04-12 Published online:2014-02-14
  • Contact: 王步军, E-mail: wangbujun@caas.cn

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被引次数

40

摘要：

建立了简单、快速、同步测定谷物中12种常见真菌毒素的超高效液相色谱串联质谱分析方法。样品用80%乙腈水溶液振荡提取，多功能净化柱净化，Waters ACQUITY UPLCTMBEH C18色谱柱分离, 串联四极杆质谱多反应离子监测方式检测，并采用外标法定量。结果表明, 12种真菌毒素在各自的线性响应范围内线性关系良好, 相关系数均不低于0.998，12种真菌毒素的检出限为0.016~1.000 μg kg-1，低、中、高3个加标水平的平均回收率(n = 6)为60.0%~122.4%，相对标准偏差(RSD)为0.9%~20.3%。该方法具有前处理简单、净化效果好、灵敏度高和检测速度快的优点，适用于谷物样品中多组分真菌毒素残留的分离和定量检测。

关键词: 超高效液相色谱-串联质谱, 多功能净化, 谷物, 真菌毒素

Abstract:

A determination method was developed using ultra-high performance liquid chromatography-tendem mass spectrometry (UPLC-MS/MS). Samples were sequentially extracted with 80% acetonitrile, and then the extracts were pooled and cleaned up with multifunction cleaning column before being separating by a chromatographic column of Waters ACQUITY UPLCTMBEH C18. The Mass spectrometry was conducted by using positive (ESI+) electrospray ionization and Multi-reactions monitoring (MRM) models, with external standard method. The results indicated that contants of the 12 mycotoxins had good linear relationship with than peak areas. The detection limits for them ranged from 0.016 to 1.000 μg kg-1, and the average recovery rates at three levels of adding external standard were from 60.0% to 122.4%, with a relative standard deviation (RSD) varying from 0.9% to 20.3%. The method is simple, rapid, accurate and suitable for simultaneously by measuring 12 kinds of mycotoxins in cereals.

Key words: Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry (UPLC-MS/MS), Multifunction cleaning, Cereals, Mycotoxin

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