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多毒素 LC-MS/MS 方法验证及其在匈牙利 54 种小麦粉中的应用。

Multi-mycotoxin LC-MS/MS method validation and its application to fifty-four wheat flours in Hungary.

机构信息

Department of Applied Chemistry, Faculty of Food Science, Szent István University, Budapest, Hungary.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2021 Apr;38(4):670-680. doi: 10.1080/19440049.2020.1862424. Epub 2021 Feb 10.

DOI:10.1080/19440049.2020.1862424
PMID:33566733
Abstract

In this study, fifty-four wheat flour and wheat-based products available on the Hungarian market were assessed for twelve mycotoxins. Prior to analysis, a multi-mycotoxin method using high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) was developed and validated for wheat and wheat-based products. A simple extraction with acetonitrile/water/formic acid (79/20/1 v/v%) was used for sample preparation. The limits of quantitation (LOQ) were between 0.02 and 161 μg kg. Good linearity (r > 0.995) was achieved for all mycotoxins investigated. Recoveries varied between 88 and 120% at three concentration levels. Based on the low relative matrix effect (RSD < 0.15%) of the different wheat flour samples, matrix-matched calibration was used, which also proved its suitability in proficiency testing (z-scores: -0.6 for DON; +1.5 for OTA; -0.5 for ZEA). DON was the predominant mycotoxin, which contaminated 84% of the investigated samples. Metabolised forms of DON were found in spelt, durum flour and some wheat-based products (D3G in 4 samples, 15Ac-DON in 7 samples). T-2 and HT-2 were the second most frequently detected mycotoxins. All investigated samples complied with current European/Hungarian legislation.

摘要

本研究评估了匈牙利市场上的 54 种小麦粉和以小麦为基础的产品中的 12 种真菌毒素。在分析之前,开发并验证了一种用于小麦和以小麦为基础的产品的高效液相色谱-串联质谱(HPLC-MS/MS)多真菌毒素方法。简单的乙腈/水/甲酸(79/20/1 v/v%)提取用于样品制备。定量限(LOQ)在 0.02 至 161 μg kg 之间。所有研究的真菌毒素均具有良好的线性(r>0.995)。在三个浓度水平下,回收率在 88%至 120%之间变化。基于不同小麦粉样品的相对基质效应(RSD <0.15%)较低,使用基质匹配校准,这也证明了其在能力验证中的适用性(DON 的 z 分数为-0.6;OTA 的 z 分数为+1.5;ZEA 的 z 分数为-0.5)。DON 是主要的真菌毒素,污染了 84%的调查样品。在斯佩尔特小麦粉、硬粒小麦粉和一些以小麦为基础的产品中发现了 DON 的代谢产物(D3G 在 4 个样品中,15Ac-DON 在 7 个样品中)。T-2 和 HT-2 是第二常见的真菌毒素。所有调查的样品均符合现行的欧洲/匈牙利法规。

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