Black R M, Read R W
Chemical Defence Establishment, Porton Down, Salisbury, U.K.
J Chromatogr. 1988 Sep 30;449(1):261-70. doi: 10.1016/s0021-9673(00)94385-1.
A sensitive method has been developed for the detection and quantitative determination of thiodiglycol in blood, plasma and urine. Samples were extracted from Clin Elut columns and cleaned up on C18 Sep-Pak cartridges (blood, plasma) or Florisil Sep-Pak cartridges (urine). Tetradeuterothiodiglycol was added to the sample prior to extraction as internal standard. Thiodiglycol was converted to its bis-(pentafluorobenzoate) derivative and analysed by capillary gas chromatography-electron-capture negative-ion chemical ionisation mass spectrometry using selected ion monitoring. Levels of thiodiglycol down to 1 ng/ml (1 ppb) could be detected in 1-ml spiked blood and urine samples; calibration curves were linear over the range 5- or 10-100 ng/ml. Blood and urine samples from a number of control subjects were analysed for background levels of thiodiglycol. Concentrations up to 16 ng/ml were found in blood, but urine levels were below 1 ng/ml.
已开发出一种灵敏的方法，用于检测和定量测定血液、血浆及尿液中的硫二甘醇。样品从Clin Elut柱中提取，并在C18 Sep-Pak柱（血液、血浆）或弗罗里硅土Sep-Pak柱（尿液）上进行净化处理。在提取前，将四氘代硫二甘醇作为内标加入样品中。硫二甘醇被转化为其双（五氟苯甲酸酯）衍生物，并通过毛细管气相色谱-电子捕获负离子化学电离质谱法，采用选择离子监测进行分析。在1 ml加标的血液和尿液样品中，可检测到低至1 ng/ml（1 ppb）的硫二甘醇水平；校准曲线在5或10 - 100 ng/ml范围内呈线性。分析了许多对照受试者的血液和尿液样品中硫二甘醇的背景水平。血液中发现的浓度高达16 ng/ml，但尿液水平低于1 ng/ml。
