耵聍中多氯联苯的气相色谱-质谱测定法

Determination of Polychlorinated Biphenyls in Cerumen by GC-MS

目的建立人体耵聍中多氯联苯(PCBs)的测定方法。方法样品用正己烷萃取、液-液分配萃取分离、柱层析净化、气相色谱法定量和气相色谱-质谱联用仪定性,并探讨了最佳实验条件。结果采用Aroclor1242、1254、1260为标准品,其混合标样的浓度在0.05～0.25μg/ml范围内,色谱峰的峰高与浓度值呈正相关,其r≥0.9990。方法最低检出浓度为0.15μg/g耵脂,平均回收率为92.1%,相对标准偏差为3.0%～4.6%(n=12)。结论该方法简易可靠,是一种新颖的生物材料中PCBs的检测方法。

Objective To establish a method of GS-MS for determination of polychlorinated biphenyls (PCBs) in human cerumen. Methods The PCBs in cerumen samples was separated by n-hexane extraction, liquid-liquid extraction separation and column chromatography purification, then was analyzed quantitatively by gas chromatography and affirmed qualitatively by mass spectroscopy. Results The detection limit, average recovery rate and precision of this method were 0.15 μg/g fat, 92.1% and 3.0%-4.6% (n=12) respectively. The contents of PCBs in 90 cerumen samples collected in polluted and control areas were detected. The levels(0.00-18.42 μg/g fat) of PCBs in cerumen collected in polluted area were significantly higher than that in the control area(P<0.01). Conclusion This methods is practical, simple and reliable. The cerumen, as a biological specimen, is suitable for environmental epidemiology investigation in PCBs polluted area.