Development and validation of an accurate and rapid LC-ESI-MS/MS method for the simultaneous quantification of aflatoxin B1, B2, G1 and G2 in lotus seeds
Development and validation of an accurate and rapid LC-ESI-MS/MS method for the simultaneous quantification of aflatoxin B1, B2, G1 and G2 in lotus seeds
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开发并验证一种准确快速的 LC-ESI-MS/MS 方法，用于同时定量莲子中的黄曲霉毒素 B1、B2、G1 和 G2
DOI：
10.1016/j.foodcont.2012.05.069
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发表时间：
2013-01-01
期刊：
影响因子：
6
通讯作者：
Yang, Meihua
中科院分区：
文献类型：
--
作者：
Liu, Shuyu;Qiu, Feng;Yang, Meihua
建立并验证了一种准确、快速的液相色谱 - 电喷雾电离串联质谱（LC - ESI - MS/MS）分析方法，用于同时测定莲子中的黄曲霉毒素B - 1、B - 2、G₁和G₂。样品首先用甲醇 - 水溶液（80 : 20，v/v）提取，然后用免疫亲和柱净化。质谱仪采用正离子电喷雾（ESI⁺）模式，使用多反应监测（MRM）分析四种黄曲霉毒素。分别使用质荷比m/z 313 → 285（黄曲霉毒素B₁，碰撞能量33 eV）、m/z 315 → 259（黄曲霉毒素B₂，碰撞能量37 eV）、m/z 329 → 243（黄曲霉毒素G₁，碰撞能量37 eV）和m/z 331 → 257（黄曲霉毒素G₂，碰撞能量37 eV）对这四种黄曲霉毒素进行定量。基于3 : 1的信噪比，黄曲霉毒素B - 1、B - 2、G₁和G₂的检测限（LODs）分别为0.007、0.005、0.003和0.005μg/kg。基于10 : 1的信噪比，黄曲霉毒素B - 1、B - 2、G₁和G₂的定量限（LOQs）分别为0.02、0.015、0.01和0.015μg/kg。在添加标准品的莲子样品中，所有化合物的回收率均在66%以上，相对标准偏差均在15%以下。从中国不同药店或市场收集的20批莲子中有19批被发现受到不同程度的黄曲霉毒素污染，含量范围从0.02到688.4μg/kg。英国皇家版权所有（C）2012，由爱思唯尔有限公司出版。保留所有权利。
An accurate and rapid LC-ESI-MS/MS analytical method was developed and validated for the simultaneous determination of aflatoxin B-1, B-2, G(1) and G(2) in lotus seeds. The samples were firstly extracted with methanol-water solution (80:20, v/v), and then cleaned up by immunoaffinity columns. The mass spectrometer was operated in the positive ionization electrospray (ESI+) mode using multiple reaction monitoring (MRM) for analysis of four aflatoxins. The transitions of m/z 313 -> 285 (AFB(1), CE 33 eV), m/z 315 -> 259 (AFB(2), CE 37 eV), m/z 329 -> 243 (AFG(1), CE 37 eV) and m/z 331 -> 257 (AFG(2), CE 37 eV) were used to quantify these four aflatoxins, respectively. The limits of detection (LODs) of aflatoxin B-1, B-2, G(1) and G(2) were 0.007, 0.005, 0.003 and 0.005 mu g kg(-1) based on a signal-to-noise ratio of 3:1, respectively. The limits of quantification (LOQs) of aflatoxin B-1, B-2, G(1) and G(2) were 0.02, 0.015, 0.01 and 0.015 pg kg(-1) based on a signal-to-noise ratio of 10:1, respectively. Recoveries for samples of spiked lotus seeds were all above 66% with relative standard deviation all below 15% for all compounds. Nineteen out of twenty batches of lotus seeds collected from different drug stores or markets in China were found to be contaminated with aflatoxins at different levels ranging from 0.02 to 688.4 mu g kg(-1). Crown Copyright (C) 2012 Published by Elsevier Ltd. All rights reserved.