Siegel David, Rasenko Tatjana, Koch Matthias, Nehls Irene
Federal Institute for Materials Research and Testing, Division I.2, Berlin, Germany.
J Chromatogr A. 2009 May 22;1216(21):4582-8. doi: 10.1016/j.chroma.2009.03.063. Epub 2009 Mar 27.
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).
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)。