Brock J W, Burse V W, Ashley D L, Najam A R, Green V E, Korver M P, Powell M K, Hodge C C, Needham L L
Division of Environmental Health Laboratory Sciences, National Center for Environmental Health (NCEH), Centers for Disease Control and Prevention (CDC), Atlanta, GA 30341, USA.
J Anal Toxicol. 1996 Nov-Dec;20(7):528-36. doi: 10.1093/jat/20.7.528.
Chlorinated pesticides and polychlorinated biphenyls (PCBs) remain public health concerns because of their unresolved health impact and their persistence in humans. Current epidemiological studies of cancer, non-Hodgkins lymphoma, and endocrine disruption in National Center for Environmental Health (NCEH) laboratories require exposure assessment of many analytes in thousands of people. Previous methods of analyzing pesticides and PCBs in serum have proven inadequate for timely processing of the number of samples required for epidemiological studies. A new method that involves solid-phase extraction (SPE) and cleanup followed by dual-column gas chromatographic separation and electron capture detection has been developed. Nine surrogate compounds were added to the serum prior to sample workup to provide quality assurance for the SPE steps. These surrogates mimic the chemistry of the analytes in the extraction, cleanup, and gas chromatographic analysis steps. To increase selectivity, extracts were injected onto two gas chromatographs with different capillary columns, a DB-1701 and a DB-5. Recoveries of 17 pesticides, 28 PCB congeners, and one polybrominated biphenyl congener ranged from 40 to 80%. Recoveries from this procedure were found to be similar to those from the previously used liquid-liquid extraction method. Correlation of analyte and surrogate recoveries were compared to examine the ruggedness of the technique. The SPE method was found to provide improved sample throughput by a factor of 15.
由于其对健康的影响尚未解决且在人体内具有持久性，含氯农药和多氯联苯（PCBs）仍然是公共卫生关注的问题。美国国家环境卫生中心（NCEH）实验室目前针对癌症、非霍奇金淋巴瘤和内分泌干扰的流行病学研究需要对数千人的多种分析物进行暴露评估。以往分析血清中农药和多氯联苯的方法已证明不足以及时处理流行病学研究所需的样本数量。一种新的方法已被开发出来，该方法包括固相萃取（SPE）和净化，然后进行双柱气相色谱分离和电子捕获检测。在样品处理前向血清中添加了九种替代化合物，以确保SPE步骤的质量。这些替代物在萃取、净化和气相色谱分析步骤中模拟分析物的化学性质。为了提高选择性，将提取物注入两台配备不同毛细管柱（DB-1701和DB-5）的气相色谱仪中。17种农药、28种多氯联苯同系物和1种多溴联苯同系物的回收率在40%至80%之间。发现该方法的回收率与先前使用的液液萃取方法的回收率相似。比较分析物和替代物回收率的相关性以检验该技术的耐用性。发现SPE方法可将样品通量提高15倍。
