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采用带微电子捕获检测器的气相色谱法测定人血清中的多氯联苯和有机氯农药。

Determination of polychlorinated biphenyls and organochlorine pesticides in human serum by gas chromatography with micro-electron capture detector.

作者信息

Cao Lu-Lu, Yan Chong-Huai, Yu Xiao-Dan, Tian Ying, Zou Xiang-Yu, Lu Da-Sheng, Shen Xiao-Ming

机构信息

XinHua Hospital affiliated to Shanghai Jiao Tong University School of Medicine, MOE-Shanghai Key Laboratory of Children's Environmental Health, No. 1665, Kongjiang Road, Shanghai, 200092, China.

出版信息

J Chromatogr Sci. 2012 Feb;50(2):145-50. doi: 10.1093/chromsci/bmr031.

Abstract

A method for determination of concentrations of polychlorinated biphenyl congeners (PCB-28, 52, 101, 118, 138, 153, 156, and 187) and organochlorine pesticides (hexachlorobenzene, alpha-hexachlorocyclohexane, beta-hexachlorocyclohexane, gamma-hexachlorocyclohexane, delta-hexachlorocyclohexane, p,p'-dichlorodiphenyl dichloroethylene, o,p'-dichlorodiphenyl trichloroethane, p,p'-dichlorodiphenyl dichloroethane, p,p'-dichlorodiphenyl trichloroethane, alpha-chlordane, gamma-chlordane, heptachlor, heptachlor epoxide, and aldrin) in human serum is developed. Recovery is assessed with artificial serum, in which PCBs and OCPs could not be detected. The method is then confirmed with pooled human serum. Experiments are performed by adding two concentrations of analytes (0.5 µg/L and 1.0 µg/L) to both matrices. The sample pretreatment process involves denaturing with a mixture of water-1-propanol (v:v, 85:15), extraction with a C-18 cartridge, and cleanup with an Alumina B cartridge. This process required about 2 mL of serum. The limit of detection ranged from 0.05-0.35 µg/L for all the analytes. Recovery of analytes at low and high spiking concentrations varied from 63-122% and 61-124% for artificial serum and pooled human serum, respectively. Relative standard deviation was lower than 16% and 18% for artificial serum and pooled human serum, respectively. Stability of the method, expressed as relative standard deviation, was lower than 14%. The method has been applied in epidemiological research.

摘要

开发了一种测定人血清中多氯联苯同系物(PCB - 28、52、101、118、138、153、156和187)以及有机氯农药(六氯苯、α - 六氯环己烷、β - 六氯环己烷、γ - 六氯环己烷、δ - 六氯环己烷、p,p'-二氯二苯二氯乙烯、o,p'-二氯二苯三氯乙烷、p,p'-二氯二苯二氯乙烷、p,p'-二氯二苯三氯乙烷、α - 氯丹、γ - 氯丹、七氯、七氯环氧化物和艾氏剂)浓度的方法。使用人工血清评估回收率,在人工血清中未检测到多氯联苯和有机氯农药。然后用混合人血清对该方法进行验证。通过向两种基质中添加两种浓度的分析物(0.5 µg/L和1.0 µg/L)来进行实验。样品预处理过程包括用水 - 1 - 丙醇混合物(体积比为85:15)变性、用C - 18柱萃取以及用氧化铝B柱净化。该过程大约需要2 mL血清。所有分析物的检测限范围为0.05 - 0.35 µg/L。对于人工血清和混合人血清,低加标浓度和高加标浓度下分析物的回收率分别为63 - 122%和61 - 124%。人工血清和混合人血清的相对标准偏差分别低于16%和18%。以相对标准偏差表示的该方法的稳定性低于14%。该方法已应用于流行病学研究。

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