Begley P, Foulger B E, Jeffery P D, Black R M, Read R W
J Chromatogr. 1986 Sep 26;367(1):87-101. doi: 10.1016/s0021-9673(00)94819-2.
A sensitive and selective method has been developed for the simultaneous detection in blood of eleven trichothecenes of widely varying polarity. The procedure involved precipitation of blood proteins with acetone followed by a clean-up using reversed-phase Sep-Pak C18 cartridges. The extracted trichothecenes were derivatised as their pentafluoropropionyl esters, separated using capillary gas chromatography and detected using electron-capture negative ion chemical ionisation with methane reagent gas and selected-ion monitoring. Optimum sensitivity and selectivity were obtained using low source temperatures (60 degrees C indicated) and high source pressures (1 Torr indicated). Detection limits on 1-ml blood samples were in the range 0.1-5 ppb. The method was readily adaptable to the detection of other trichothecenes. A protocol was used which minimised the risk of cross-contamination. The method was validated in collaborative studies by the successful analysis of 42 blood samples spiked and submitted blind by two independent laboratories for analysis.
已开发出一种灵敏且具选择性的方法，用于同时检测血液中极性差异很大的11种单端孢霉烯族毒素。该程序包括用丙酮沉淀血液蛋白，然后使用反相Sep-Pak C18柱进行净化。提取的单端孢霉烯族毒素被衍生化为其五氟丙酰酯，用毛细管气相色谱法分离，并用甲烷反应气和选择离子监测的电子捕获负离子化学电离进行检测。使用低源温度（指示为60摄氏度）和高源压力（指示为1托）可获得最佳灵敏度和选择性。1毫升血液样本的检测限在0.1 - 5 ppb范围内。该方法易于适用于其他单端孢霉烯族毒素的检测。使用了一种将交叉污染风险降至最低的方案。该方法在合作研究中通过成功分析两个独立实验室加标并盲样提交的42份血液样本而得到验证。
