Kumazawa T, Sato K, Seno H, Ishii A, Suzuki O
Department of Legal Medicine, Showa University School of Medicine, Tokyo, Japan.
J Anal Toxicol. 1995 Mar-Apr;19(2):95-8. doi: 10.1093/jat/19.2.95.
A simple and rapid method for extraction of seven dinitroaniline herbicides from human whole blood and urine using Sep-Pak C18 cartridges is presented. After mixing with distilled water, whole blood and urine samples containing the herbicides were loaded on Sep-Pak C18 cartridges and eluted with chloroform-methanol (9:1). The recovery of the seven compounds that were added to whole blood and urine was more than 91%. The herbicides were detected by capillary gas chromatography (GC) with electron-capture detection (ECD), surface-ionization detection (SID), nitrogen-phosphorus detection (NPD), and flame-ionization detection (FID). GC-ECD generally gave the highest sensitivity for all herbicides, whereas GC-FID gave the lowest sensitivity. Isopropalin could be detected by GC-SID with a sensitivity comparable with that of GC-ECD; high sensitivity could also be obtained for isopropalin, pendimethalin, and nitralin using GC-NPD. The calibration curve for the seven herbicides measured by GC-ECD showed linearity in the range of 0.047-3.0 pmol on-column. The detection limits of the herbicides were 24-45 fmol on-column for whole blood and 19-40 fmol on-column for urine.
介绍了一种使用Sep-Pak C18柱从人全血和尿液中提取7种二硝基苯胺类除草剂的简单快速方法。将含有除草剂的全血和尿液样本与蒸馏水混合后,加载到Sep-Pak C18柱上,并用氯仿-甲醇(9:1)洗脱。添加到全血和尿液中的7种化合物的回收率超过91%。通过带有电子捕获检测(ECD)、表面电离检测(SID)、氮磷检测(NPD)和火焰离子化检测(FID)的毛细管气相色谱(GC)对除草剂进行检测。GC-ECD通常对所有除草剂具有最高的灵敏度,而GC-FID的灵敏度最低。异丙乐灵可通过GC-SID检测,其灵敏度与GC-ECD相当;使用GC-NPD对异丙乐灵、二甲戊灵和仲丁灵也可获得高灵敏度。通过GC-ECD测定的7种除草剂的校准曲线在柱上0.047-3.0 pmol范围内呈线性。全血中除草剂的柱上检测限为24-45 fmol,尿液中为19-40 fmol。