色谱

色谱 ›› 2014, Vol. 32 ›› Issue (2): 133-138.DOI: 10.3724/SP.J.1123.2013.10014

• 研究论文 • 上一篇    下一篇

基于QuEChERS提取的快速液相色谱-串联质谱法测定婴幼儿谷基辅助食品中的9种真菌毒素

胡文彦, 许磊, 杨军, 凌睿   

  1. 南京市产品质量监督检验院, 江苏 南京 210000
  • 收稿日期:2013-10-16 修回日期:2013-11-27 出版日期:2014-02-08 发布日期:2014-01-25
  • 通讯作者: 胡文彦
  • 基金资助:

    国家科技支撑计划项目(2011BAK21B05).

QuEChERS-based extraction procedure and rapid resolution liquid chromatography coupled to triple quadrupole mass spectrometry for the determination of nine mycotoxins in cereal-based complementary foods for infants and young children

HU Wenyan, XU Lei, YANG Jun, LING Rui   

  1. Nanjing Bureau of Quality and Technical Supervision, Nanjing 210000, China
  • Received:2013-10-16 Revised:2013-11-27 Online:2014-02-08 Published:2014-01-25

PDF

525

被引次数

56

摘要：

建立了婴幼儿谷基辅助食品中黄曲霉毒素B1、B2、G1、G2、赭曲霉毒素A、玉米赤霉烯酮、T-2毒素、脱氧雪腐镰刀菌烯醇、伏马毒素B1共9种真菌毒素的快速测定方法。试样用改良的QuEChERS方法进行提取，无需进一步净化，直接用液相色谱-串联质谱仪进行测定，基质外标法定量。在较宽的线性范围内，9种毒素的线性相关系数(r2)均不小于0.98，检出限为0.1~15.8 μg/kg，在3个不同添加水平下的加标回收率为77.6%~105.7%，RSD为2.5%~13.7%。采用建立的方法对市面上销售的41批次婴幼儿谷基辅助食品中的9种真菌毒素进行了筛查，数批产品检出不同含量的毒素。该方法准确、灵敏，可适用于婴幼儿谷基辅助食品中多种真菌毒素的快速分析。

关键词: QuEChERS, 快速液相色谱-串联质谱, 婴幼儿谷基食品, 真菌毒素

Abstract:

A rapid method has been developed for the determination of aflatoxins B1, B2, G1 and G2, ochratoxin A, zearalenone, T-2 toxin, deoxynivalenol and fumonisin B1 in cereal-based complementary foods for infants and young children. The mycotoxins were extracted from the samples using a modified QuEChERS-based extraction procedure without any further clean-up step. The separation of the analytes was carried out on an Agilent XDB C18 column (50 mm×2.1 mm, 1.8 μm) using the mobile phases of acetonitrile and 5 mmol/L ammonium acetate-0.1% (volume percentage) formic acid aqueous solution with gradient elution. The extract was determined by rapid resolution liquid chromatography-tandem mass spectrometry. Matrix-matched calibration was used for the quantification. The proposed method showed good linear correlation with the correlation coefficients all above 0.98. The blank samples were fortified at three levels, and the recoveries ranged from 77.6% to 105.7% with the RSDs from 2.5% to 13.7%. The limits of detection ranged from 0.1 μg/kg to 15.8 μg/kg. The developed method was successfully applied for mycotoxin analysis in 41 samples bought from markets. The method shows advantages in both accuracy and sensitivity, and is suitable for the rapid multi-aflatoxin screening in cereal-based complementary foods for infants and young children.

Key words: cereal-based foods for infants and young children, mycotoxins, QuEChERS, rapid resolution liquid chromatography-tandem mass spectrometry (RRLC-MS/MS)

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