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超高效液相色谱-串联质谱法同时测定花生及其衍生产品中的黄曲霉毒素 B1、B2、G1、G2、M1 和 M2

Simultaneous determination of aflatoxins B1, B2, G1, G2, M1 and M2 in peanuts and their derivative products by ultra-high-performance liquid chromatography-tandem mass spectrometry.

机构信息

Zhejiang Provincial Center for Disease Prevention and Control, Hangzhou 310051, Zhejiang Province, China.

出版信息

Anal Chim Acta. 2010 Mar 3;662(1):62-8. doi: 10.1016/j.aca.2010.01.002. Epub 2010 Jan 11.

Abstract

A reliable ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for simultaneous determination of aflatoxins B1, B2, G1, G2, M1 and M2 in peanuts and their derivative products was developed. The sample was extracted by 84% of acetonitrile aqueous solution and the extract was purified by a reliable solid phase extraction-based clean-up method. Then, the analytes were separated on Acquity UPLC HSS T3 column (100 mm x 2.1 mm, 1.8 microm particle size), and eluted with a mobile phase consisting of (A) water containing 0.1% formic acid and (B) acetonitrile/methanol (50/50, v/v). The separated compounds were detected with a Waters Micromass Quattro Ultima Pt tandem quadrupole mass spectrometer operating in positive electro-spray ionization using multiple reaction monitoring mode. The established method was extensively validated by determining the linearity (R(2) > or = 0.9990), average recovery (74.7-86.8%) and precision (relative standard deviation < or = 10.9%). It was shown to be a suitable method for simultaneous determination of the six aflatoxins in peanuts and their derivative products. Finally, a total of 73 samples randomly collected from different areas in Zhejiang province were screened for aflatoxins with the proposed method. The results showed that 31 samples of peanut butter, 14 samples of fresh peanut and 5 samples of musty peanut were contaminated with aflatoxins. Meanwhile, this was the first report on aflatoxins M1 and M2, which were found in unprocessed peanuts and their derivative products.

摘要

建立了一种可靠的超高效液相色谱-串联质谱(UHPLC-MS/MS)法,用于同时测定花生及其衍生产品中黄曲霉毒素 B1、B2、G1、G2、M1 和 M2。样品用 84%的乙腈水溶液提取,用可靠的基于固相萃取的净化方法净化提取液。然后,在 Acquity UPLC HSS T3 柱(100mm×2.1mm,1.8μm 粒径)上分离分析物,用由(A)含 0.1%甲酸的水和(B)乙腈/甲醇(50/50,v/v)组成的流动相洗脱。分离的化合物在 Waters Micromass Quattro Ultima Pt 串联四极杆质谱仪上以正电喷雾电离模式,采用多反应监测模式进行检测。该方法通过测定线性(R(2)≥0.9990)、平均回收率(74.7-86.8%)和精密度(相对标准偏差≤10.9%)进行了广泛验证。结果表明,该方法适用于同时测定花生及其衍生产品中的六种黄曲霉毒素。最后,采用所建立的方法对浙江省不同地区随机采集的 73 份花生样品进行了黄曲霉毒素筛查。结果显示,31 份花生酱、14 份鲜花生和 5 份霉花生样品受到黄曲霉毒素污染。同时,这是首次在未经加工的花生及其衍生产品中发现黄曲霉毒素 M1 和 M2。

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