色谱 ›› 2017, Vol. 35 ›› Issue (6): 601-607.DOI: 10.3724/SP.J.1123.2016.12028

• 研究论文 • 上一篇    下一篇

同位素内标-液相色谱-串联质谱法同时测定粮食及其制品中的5种真菌毒素

高蓓, 姜德铭, 杨永坛   

  1. 中粮营养健康研究院, 营养健康与食品安全北京市重点实验室, 北京 102209
  • 收稿日期:2016-12-23 出版日期:2017-06-08 发布日期:2013-09-29
  • 通讯作者: 杨永坛,E-mail:yangyongtan@cofco.com.

Simultaneous determination of five mycotoxins in various grains and their products by liquid chromatography-tandem mass spectrometry with isotope internal standard

GAO Bei, JIANG Deming, YANG Yongtan   

  1. Chinese Oil & Foodstuffs Corporation (COFCO) Nutrition and Health Research Institute, Beijing Key Laboratory of Nutrition Health and Food Safety, Beijing 102209, China
  • Received:2016-12-23 Online:2017-06-08 Published:2013-09-29

摘要:

建立了同位素内标-液相色谱-串联质谱快速测定粮食及其制品中玉米赤霉烯酮(ZON)、雪腐镰刀菌烯醇(NIV)、脱氧雪腐镰刀菌烯醇(DON)及其衍生物3-乙酰基脱氧雪腐镰刀菌烯醇(3-ACDON)和15-乙酰基脱氧雪腐镰刀菌烯醇(15-ACDON)5种真菌毒素的分析方法。以乙腈-水(84:16,v/v)为提取液,采用多功能净化柱净化,同位素内标法定量。5种真菌毒素在各自的线性范围内线性关系良好,相关系数(r2)均大于0.99,检出限(LOD,S/N=3)为5~20 μg/kg。大麦、小麦、燕麦、玉米等9种代表性粮食及其制品在3个不同添加水平下的加标回收率为84.2%~114.5%,相对标准偏差(RSD)为0.4%~9.9%(n=6)。该法操作简单,成本低,准确可靠,灵敏度高,可同时检测粮食及其制品中的5种真菌毒素。

关键词: 粮食及其制品, 同位素内标, 液相色谱-串联质谱法, 真菌毒素

Abstract:

A rapid method was established for the determination of zearalenone (ZON), nivalenol (NIV), deoxynivalenol (DON), 3-acetyl-deoxynivalenol (3-ACDON) and 15-acetyl-deoxynivalenol (15-ACDON) in various grains and their products by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted by acetonitrile-water (84:16, v/v), and cleaned-up by multifunctional column without any further step. The separation was carried out on an Acquity UPLC® BEH C18 column (100 mm×2.1 mm, 1.7 μm) with gradient elution using acetonitrile-water as mobile phases. The analytes were quantified by isotope internal standard method. The correlation coefficients (r2) were all above 0.99. The limits of detection (LODs, S/N=3) ranged from 5 μg/kg to 20 μg/kg. The recoveries of the five mycotoxins spiked in blank grain and its product samples varied from 84.2% to 114.5%, with the relative standard deviations (RSDs) of 0.4%-9.9% (n=6). The method is accurate, efficient, sensitive and practical.

Key words: grains and their products, isotope internal standard, liquid chromatography-tandem mass spectrometry (LC-MS/MS), mycotoxins

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