Collins G J, Rosen J D
J Assoc Off Anal Chem. 1979 Nov;62(6):1274-80.
A method for the analysis of T-2 toxin in milk is presented. Ethyl acetate extracts of milk samples which had been spiked with T-2 toxin were purified by thin layer chromatography and derivatized with N,O-bis(trimethylsilyl)acetamide to produce the T-2 toxin trimethylsilyl ether (T-2 toxin-TMS). N,O-bis(trimethylsilyl-d9)acetamide was used to make T-2 toxin d9-trimethylsilyl ether (T-2 toxin-d9 TMS) which was added to the derivatized milk extract as an internal standard. Samples were analyzed by combined gas-liquid chromatography/mass spectrometry using either electron impact ionization or chemical ionization mass spectrometry. In electron impact ionization analyses, simultaneous monitoring of the T-2 toxin-TMS fragment ion at m/z 436 and the T-2 toxin-d9TMS fragment ion at m/z 445 gave a T-2 toxin-TMS detectability estimated at 6 microgram/kg. In chemical ionization analyses, the T-2 toxin-TMS fragment ion at m/z 377 and the T-2 toxin-d9TMS fragment ion at m/z 386 were simultaneously monitored to give a T-2 toxin-TMS detectability estimated at 3 microgram/kg. Average recovery was 85% at 200 microgram/kg and 65% at 20 microgram/kg.
本文介绍了一种牛奶中T-2毒素的分析方法。用T-2毒素加标的牛奶样品的乙酸乙酯提取物通过薄层色谱法进行纯化，并用N,O-双（三甲基硅基）乙酰胺进行衍生化，以生成T-2毒素三甲基硅基醚（T-2毒素-TMS）。使用N,O-双（三甲基硅基-d9）乙酰胺制备T-2毒素d9-三甲基硅基醚（T-2毒素-d9 TMS），并将其作为内标添加到衍生化的牛奶提取物中。采用电子轰击电离或化学电离质谱联用的气相色谱/质谱法对样品进行分析。在电子轰击电离分析中，同时监测质荷比为436的T-2毒素-TMS碎片离子和质荷比为445的T-2毒素-d9TMS碎片离子，得出T-2毒素-TMS的检测限估计为6微克/千克。在化学电离分析中，同时监测质荷比为377的T-2毒素-TMS碎片离子和质荷比为386的T-2毒素-d9TMS碎片离子，得出T-2毒素-TMS的检测限估计为3微克/千克。在200微克/千克时平均回收率为85%，在20微克/千克时为65%。
