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采用多段中心切割二维液相色谱串联质谱法测定啤酒中的真菌毒素。

Determination of mycotoxins in beer by multi heart-cutting two-dimensional liquid chromatography tandem mass spectrometry method.

机构信息

Department of Biotechnology and Biosciences, University of Milano-Bicocca, Piazza Della Scienza 2, I-20126 Milano, Italy; Dipartimento di Farmacia, Università degli studi di Salerno, Via Giovanni Paolo II, 84084 Fisciano, SA, Italy.

Dipartimento di Farmacia, Università degli studi di Salerno, Via Giovanni Paolo II, 84084 Fisciano, SA, Italy.

出版信息

Food Chem. 2020 Jul 15;318:126496. doi: 10.1016/j.foodchem.2020.126496. Epub 2020 Feb 26.

Abstract

Beer is one the most consumed alcoholic beverage in the world and its contamination with mycotoxins is of public health concern. This study reports a fast and automated analytical procedure based on a multi-heart-cutting two-dimensional liquid chromatography tandem mass spectrometry method using electrospray ionization for the determination of seven mycotoxins (aflatoxins B1, B2, G2 and G1, ochratoxin A, fumonisins B1 and B2) in beers. The developed method was based on the heart-cutting 2D- HPLC technique in which only the specific portions of the first dimension, in the retention time of analytes, were transferred into the second dimension for the further separation and successive determination. The method uses two different chromatographic columns; in the first dimension, 50 μL of sample was injected on first column, and mycotoxins elution regions were collected in a loop and transferred into the second column for the separation of analytes. Each column operated in gradient elution mode in order to eliminate interfering compounds and improve separation and peak shape. After the optimization, the method has been validated according to EU regulation and finally applied for the analysis of forty beer samples collected from Italian supermarkets. Among all mycotoxins studied, fumonisins B1 was the most widely distributed in analysed beers (>21%) in the range from 0.6 to 12.3 ng mL. The automated methodology developed was able to determine accurately and simultaneously seven mycotoxins in beer. This provided a significant reduction of sample handle and, consequently of analysis time.

摘要

啤酒是世界上消费最多的酒精饮料之一,其被真菌毒素污染引起了公众健康关注。本研究报告了一种快速自动化的分析方法,基于多中心切割二维液相色谱串联质谱法,采用电喷雾电离,用于测定啤酒中的七种真菌毒素(黄曲霉毒素 B1、B2、G2 和 G1、赭曲霉毒素 A、伏马菌素 B1 和 B2)。该方法基于中心切割二维 HPLC 技术,仅在第一个维度中分析物的保留时间内将特定部分转移到第二个维度进行进一步分离和连续测定。该方法使用了两种不同的色谱柱;在第一个维度中,将 50μL 的样品注入第一根色谱柱,真菌毒素洗脱区域被收集在一个环中并转移到第二根色谱柱进行分离。每根柱子都以梯度洗脱模式运行,以消除干扰化合物,提高分离度和峰形。经过优化后,该方法根据欧盟法规进行了验证,最后应用于分析从意大利超市采集的四十个啤酒样本。在所研究的所有真菌毒素中,伏马菌素 B1 在分析的啤酒中分布最广(>21%),范围从 0.6 到 12.3ng/mL。开发的自动化方法能够准确且同时测定啤酒中的七种真菌毒素。这大大减少了样品处理量,从而缩短了分析时间。

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