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Characterization of (13C24) T-2 toxin and its use as an internal standard for the quantification of T-2 toxin in cereals with HPLC–MS/MS

机译:(13 C24 )T-2毒素的表征及其作为内部标准品通过HPLC-MS / MS定量测定谷物中T-2毒素的用途

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摘要

In this paper, the structure and the identity of fully 13C-substituted T-2 toxin were confirmed using high-resolution mass spectrometry, 1H-NMR, 13C-NMR, tandem mass spectrometry and HPLC–DAD. The purity of this compound was estimated to be at least 98.8% according to UV data. The isotopic distribution of (13C24) T-2 toxin indicated a total isotopic enrichment of 98.2 ± 1.0 atom% 13C, and the application of different MS measurement modes revealed the MS/MS fragmentation pattern of T-2 toxin. Furthermore, a stable isotope dilution mass spectrometry method for the quantification of T-2 toxin was developed using (13C24) T-2 toxin as internal standard. The method was evaluated with and without conventional clean-up and validated for maize and oats. Both cereals showed strong matrix enhancement effects, which could be compensated for through the application of the isotope-substituted internal standard.
机译:本文通过高分辨率质谱,1 H-NMR,13 C-NMR,13 C-NMR证实了完全被13 C-取代的T-2毒素的结构和身份。串联质谱和HPLC–DAD。根据UV数据,该化合物的纯度估计为至少98.8%。 (13 C24 )T-2毒素的同位素分布表明13同位素总同位素富集为98.2±1.0原子%13 ,不同质谱测量模式的应用揭示了MS / T-2毒素的MS片段化模式。并以(13 C24 )T-2毒素为内标,建立了稳定的同位素稀释质谱法定量T-2毒素。在有和没有常规清理的情况下对该方法进行了评估,并针对玉米和燕麦进行了验证。两种谷物均显示出强大的基质增强作用,这可以通过应用同位素取代的内标物来弥补。

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