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一种用于测定青贮牧草中霉菌毒素的超高效液相色谱-串联质谱法的开发与验证

Development and validation of an UHPLC-MS/MS method for the determination of mycotoxins in grass silages.

作者信息

McElhinney Cormac, O'Kiely Pádraig, Elliott Chris, Danaher Martin

机构信息

a Animal & Grassland Research and Innovation Centre, Teagasc, Grange, Dunsany, Co. Meath , Ireland.

b Institute for Global Food Security , Queen's University Belfast , Belfast , Northern Ireland.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2015;32(12):2101-12. doi: 10.1080/19440049.2015.1094830. Epub 2015 Oct 19.

Abstract

An ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) multi-mycotoxin analytical method was developed to simultaneously identify and quantify 20 mycotoxins in grass silages, inclusive of mycotoxins that are currently regulated in European Union feeds. Extraction of mycotoxins from dried grass silages was performed using of a modified QuEChERS extraction employing an acidified aqueous extraction (0.1 N HCl) with no further clean-up. Following chromatographic separation, analytes were detected using a fast polarity-switching MS/MS method that allowed both positive and negative ions to be analysed from a single injection, thus the reducing time and cost of analysis. The limits of detection and quantification ranged between 3 µg kg(-1) DM (aflatoxin B1, beauvericin and enniatin A and A1) and 200 µg kg(-1) DM (deoxynivalenol), and between 10 µg kg(-1) DM (aflatoxin B1, beauvericin and enniatin A1) and 500 µg kg(-1) DM (deoxynivalenol), respectively. Inter-assay accuracy and precision ranged between 90% and 107% and between 3.9% and 15.0% CV, respectively. The accuracy of the method was assessed through the application to a range of incurred samples in an inter-laboratory study.

摘要

建立了一种超高效液相色谱 - 串联质谱(UHPLC - MS/MS)多霉菌毒素分析方法,用于同时鉴定和定量青贮饲料中的20种霉菌毒素,包括目前欧盟饲料中受监管的霉菌毒素。从干青贮饲料中提取霉菌毒素采用改良的QuEChERS提取法,使用酸化水提取液(0.1 N HCl),无需进一步净化。色谱分离后,使用快速极性切换MS/MS方法检测分析物,该方法允许从一次进样中分析正离子和负离子,从而减少分析时间和成本。检测限和定量限分别在3 μg kg⁻¹ DM(黄曲霉毒素B1、白僵菌素和恩镰孢菌素A及A1)至200 μg kg⁻¹ DM(脱氧雪腐镰刀菌烯醇)之间,以及10 μg kg⁻¹ DM(黄曲霉毒素B1、白僵菌素和恩镰孢菌素A1)至500 μg kg⁻¹ DM(脱氧雪腐镰刀菌烯醇)之间。批间准确度和精密度分别在90%至107%之间和3.9%至15.0% CV之间。通过在一项实验室间研究中应用于一系列实际污染样品来评估该方法的准确度。

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