Norén K, Sjövall J
J Chromatogr. 1987 Feb 20;414(1):55-63. doi: 10.1016/0378-4347(87)80024-5.
A method using the lipophilic gel Lipidex 5000 for sorption of pentachlorophenol (PCP) from water and urine is described. The procedure for water gives a simultaneous clean-up from lipophilic contaminants and also offers the possibility for determination of less polar compounds, such as 1,1-bis(4-chlorophenyl)-2,2,2-trichloroethane (p,p'-DDT) and 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD), collected in a separate fraction. The extracted PCP is derivatized to pentachlorophenyl acetate, which is determined by electron-capture gas chromatography. The average recovery of 0.01-0.15 ng PCP per ml water was 96% and of labelled p,p'-DDT (ca. 5 ng/ml) and TCDD (ca. 0.001 ng/ml) 95 and 92%, respectively. A similar method for enrichment of PCP was applied to acidified urine and to urine hydrolysed with hydrochloric acid or with digestive juice from Helix pomatia. Recoveries of 0.1-2.5 ng PCP per ml non-hydrolysed urine were on an average 92% and of 2.5-10 ng PCP per ml hydrolysed urine 96%. The analyses indicate that PCP in urine from non-occupationally exposed persons is originally conjugated and to some extent liberated when stored. The contamination of organic solvents and laboratory environments with PCP is discussed.
描述了一种使用亲脂性凝胶Lipidex 5000从水和尿液中吸附五氯苯酚(PCP)的方法。水的处理程序可同时去除亲脂性污染物,还提供了测定极性较小的化合物的可能性,例如收集在单独馏分中的1,1-双(4-氯苯基)-2,2,2-三氯乙烷(p,p'-滴滴涕)和2,3,7,8-四氯二苯并对二恶英(TCDD)。提取的PCP衍生化为五氯苯基乙酸酯,通过电子捕获气相色谱法测定。每毫升水中0.01 - 0.15 ng PCP的平均回收率为96%,标记的p,p'-滴滴涕(约5 ng/ml)和TCDD(约0.001 ng/ml)的平均回收率分别为95%和92%。一种类似的PCP富集方法应用于酸化尿液以及用盐酸或苹果螺消化液水解的尿液。每毫升未水解尿液中0.1 - 2.5 ng PCP的回收率平均为92%,每毫升水解尿液中2.5 - 10 ng PCP的回收率为96%。分析表明,非职业暴露人群尿液中的PCP最初是结合态的,储存时会在一定程度上释放出来。还讨论了PCP对有机溶剂和实验室环境的污染。