Klötzel Marianna, Gutsche Birgit, Lauber Uwe, Humpf Hans-Ulrich
Chemisches und Veterinäruntersuchungsamt Stuttgart, Schaflandstrasse 3/2, 70736 Fellbach, Germany.
J Agric Food Chem. 2005 Nov 16;53(23):8904-10. doi: 10.1021/jf051501c.
A new sensitive method for the simultaneous determination of 12 trichothecenes (deoxynivalenol, nivalenol, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, fusarenon X, T-2 toxin, HT-2 toxin, neosolaniol, monoacetoxyscirpenol, diacetoxyscirpenol, T-2 triol, and T-2 tetraol) by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) is presented. The development of the method and investigations on the matrix influence on the MS signal are described in particular. The matrix effect was thereby minimized by using an internal standard, a special mobile phase, and specific fragmentation parameters. The sample was extracted with acetonitrile/water (84:16, v/v), and the extract was cleaned up with a MycoSep 227 column. Quantification was based on the internal standard de-epoxy-deoxynivalenol. Calibration curves were linear between 16 and 1600 ng/g, and the limits of detection ranged from 0.18 to 5.0 ng/g. The developed method was applied for the determination of trichothecenes in 120 naturally contaminated wheat and oat samples.
本文介绍了一种通过液相色谱 - 电喷雾电离串联质谱法（LC - ESI - MS/MS）同时测定12种单端孢霉烯族毒素（脱氧雪腐镰刀菌烯醇、雪腐镰刀菌烯醇、3 - 乙酰脱氧雪腐镰刀菌烯醇、15 - 乙酰脱氧雪腐镰刀菌烯醇、镰刀菌烯酮X、T - 2毒素、HT - 2毒素、新茄病镰刀菌烯醇、单乙酰氧基镰刀菌烯醇、二乙酰氧基镰刀菌烯醇、T - 2三醇和T - 2四醇）的新的灵敏方法。特别描述了该方法的开发以及基质对质谱信号影响的研究。通过使用内标、特殊流动相和特定的碎片参数，使基质效应最小化。样品用乙腈/水（84:16，v/v）萃取，萃取液用MycoSep 227柱净化。定量基于内标脱环氧脱氧雪腐镰刀菌烯醇。校准曲线在16至1600 ng/g之间呈线性，检测限范围为0.18至5.0 ng/g。所开发的方法用于测定120个天然污染小麦和燕麦样品中的单端孢霉烯族毒素。
