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

引用本文: 高蓓, 姜德铭, 杨永坛. 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[J]. 色谱, 2017, 35(6): 601-607. doi: 10.3724/SP.J.1123.2016.12028 shu

Citation: GAO Bei, JIANG Deming, YANG Yongtan. Simultaneous determination of five mycotoxins in various grains and their products by liquid chromatography-tandem mass spectrometry with isotope internal standard[J]. Chinese Journal of Chromatography, 2017, 35(6): 601-607. doi: 10.3724/SP.J.1123.2016.12028 shu

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

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

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:

English

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

Chinese Oil & Foodstuffs Corporation (COFCO) Nutrition and Health Research Institute, Beijing Key Laboratory of Nutrition Health and Food Safety, Beijing 102209, China
Received Date: 23 December 2016

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:

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

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沈阳化工大学材料科学与工程学院沈阳 110142

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

English

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

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

English

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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