Nony C R, Bowman M C
Int J Environ Anal Chem. 1978;5(3):203-20. doi: 10.1080/03067317808071146.
A gas chromatographic method is described for determining traces of 13 carcinogens and related compounds (aromatic amines and estrogens) in admixture in wastewater and human urine. This method was developed for use in toxicological research for monitoring the safe disposal of wastewater and to signal any accidental exposure of personnel to hazardous test substances. Salient elements of the procedure are: extraction of phenolic and neutral residues from the acidified sample, liquid--liquid partitioning cleanup and separation of neutral from phenolic residues at pH 14 and 10.2, acid hydrolysis of the neutral component, subsequent alkalinization of the sample and extraction of the basic residues as the free amines, conversion of all residues to the corresponding pentafluoropropionyl (PFP) derivatives and quantification by electron-capture gas chromatography. Residues were detectable in wastewater and urine at the 0.1 and 1 ppb levels, respectively. Additional information is provided concerning partition values for all PFP derivatives in five solvent systems, structure verification of the derivatives by mass spectrometry and the adaption of this method to the monitoring of surfaces and air in potentially contaminated work areas.
本文描述了一种气相色谱法,用于测定废水中和人尿液中混合存在的13种致癌物及相关化合物(芳香胺和雌激素)的痕量。该方法是为毒理学研究而开发的,用于监测废水的安全处置,并提示人员意外接触有害测试物质的情况。该方法的主要步骤包括:从酸化样品中萃取酚类和中性残留物,在pH值为14和10.2的条件下进行液-液分配净化并分离中性和酚类残留物,对中性成分进行酸水解,随后将样品碱化并萃取作为游离胺的碱性残留物,将所有残留物转化为相应的五氟丙酰(PFP)衍生物,并通过电子捕获气相色谱法定量。废水中和尿液中的残留物检测限分别为0.1 ppb和1 ppb。还提供了关于所有PFP衍生物在五种溶剂系统中的分配值、通过质谱对衍生物进行结构验证以及该方法在潜在污染工作区域的表面和空气监测中的应用等补充信息。