Singh A K, Spassova D, White T
Department of Veterinary Diagnostic Medicine, College of Veterinary Medicine, University of Minnesota, St. Paul 55108, USA.
J Chromatogr B Biomed Sci Appl. 1998 Mar 20;706(2):231-44. doi: 10.1016/s0378-4347(97)00560-4.
A broad range of pollutants such as polycyclic aromatic hydrocarbons (PAHs), polychlorinated hydrocarbons (PCHs), polynitrohydrocarbons (PNHs), polychlorinated biphenyls (PCBs) and organochlorine (OCs) insecticides were simultaneously analyzed in spiked soil, water or plasma samples by using gas chromatography-mass spectrometry (GC-MS). Water and plasma samples containing the pollutants were extracted by a solid-phase extraction (SPE) method using florisil columns. The soil samples, fortified with the toxicants, were extracted with water, methanol or dichloromethane (DCM). The water extract was processed by the SPE method. The methanol and DCM samples were dried, dissolved in acetonitrile and subjected to the SPE extraction. The extracted samples were analyzed by GC-MS programmed to monitor selected ions. The deuterium labelled compounds were used as the internal standards. The chromatographic profile of total ions indicated complete separation of some compounds such as isophorone, naphthalene, all PCBs, most OC insecticides and PNHs; high Mr PAHs and some PCHs were partially or incompletely separated. The chromatographic profile of individual ion indicated good separation of each ion. The minimum detection limit ranged from 1 to 4 pg injected when 1 or 2 ions were monitored or from 20 to 200 pg injected when 20 ions were monitored. The SPE method that provided 60-105% recovery of pollutants from water samples, provided only 2-60% recovery from plasma samples. This may be due to the binding of pollutants to plasma proteins. Water recovered 1-30%, while methanol or DCM recovered 65-100% of the pollutants added to the soil samples. The use of internal standards corrected for the loss of pollutants from plasma or soil.
通过气相色谱 - 质谱联用仪（GC - MS），对加标土壤、水或血浆样品中的多种污染物进行了同时分析，这些污染物包括多环芳烃（PAHs）、多氯代烃（PCHs）、多硝基烃（PNHs）、多氯联苯（PCBs）和有机氯（OCs）杀虫剂。含有污染物的水和血浆样品采用弗罗里硅土柱固相萃取（SPE）法进行萃取。用毒物强化后的土壤样品用水、甲醇或二氯甲烷（DCM）进行萃取。水提取物采用SPE法处理。甲醇和DCM样品经干燥后，溶解于乙腈中并进行SPE萃取。萃取后的样品通过GC - MS进行程序控制监测选定离子的分析。氘代标记化合物用作内标。总离子色谱图表明，一些化合物如异佛尔酮、萘、所有多氯联苯、大多数有机氯杀虫剂和多硝基烃实现了完全分离；高分子量多环芳烃和一些多氯代烃部分或未完全分离。单个离子的色谱图表明每个离子实现了良好分离。当监测1个或2个离子时，最低检测限为进样1至4 pg；当监测20个离子时，最低检测限为进样20至200 pg。SPE法从水样中回收污染物的回收率为60 - 105%，而从血浆样品中回收的回收率仅为2 - 60%。这可能是由于污染物与血浆蛋白结合所致。水的回收率为1 - 30%，而甲醇或DCM从添加到土壤样品中的污染物中回收的回收率为65 - 100%。内标的使用校正了血浆或土壤中污染物的损失。
