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用2,4-二硝基苯肼衍生化后,通过高效液相色谱-电喷雾电离离子阱多级质谱法测定谷物中的链格孢霉菌毒素细交链孢菌酮酸。

Determination of the Alternaria mycotoxin tenuazonic acid in cereals by high-performance liquid chromatography-electrospray ionization ion-trap multistage mass spectrometry after derivatization with 2,4-dinitrophenylhydrazine.

作者信息

Siegel David, Rasenko Tatjana, Koch Matthias, Nehls Irene

机构信息

Federal Institute for Materials Research and Testing, Division I.2, Berlin, Germany.

出版信息

J Chromatogr A. 2009 May 22;1216(21):4582-8. doi: 10.1016/j.chroma.2009.03.063. Epub 2009 Mar 27.

Abstract

Tenuazonic acid (TA) is a major Alternaria mycotoxin. In the present work a novel approach for the detection of TA in cereals by liquid chromatography-ion-trap multistage mass spectrometry after derivatization with 2,4-dinitrophenylhydrazine is described. The product of the derivatization reaction and its major MS(2) fragments were characterised by Fourier transform-ion cyclotron resonance tandem mass spectrometry. Without preconcentration, the established method features a limit of detection of 10 microg/kg using 2g of sample in a rapid workup procedure. Accuracy, precision and linearity were evaluated in the working range of 50-5000 microg/kg. TA was detected in 13 and quantified in 3 out of 27 cereal samples obtained from a local supermarket, the average content being 49 microg/kg (highest incidence: 851+/-41 microg/kg).

摘要

细交链孢菌酮酸(TA)是一种主要的链格孢属霉菌毒素。本文描述了一种新方法,即先用2,4-二硝基苯肼衍生化,然后通过液相色谱-离子阱多级质谱法检测谷物中的TA。衍生化反应产物及其主要的二级质谱(MS(2))碎片通过傅里叶变换离子回旋共振串联质谱进行了表征。在无需预浓缩的情况下,该既定方法在快速分析流程中使用2克样品时的检测限为10微克/千克。在50 - 5000微克/千克的工作范围内评估了准确度、精密度和线性度。从当地一家超市获取的27份谷物样品中,有13份检测出了TA,3份进行了定量分析,平均含量为49微克/千克(最高含量:851±41微克/千克)。

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