人体血清二噁英化合物检测方法的建立

目的建立人体血清二噁英(polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans,PCDD/Fs)化合物测定方法,为开展二噁英人体健康风险评估提供检测技术手段。方法基于国际二噁英的测定方法—同位素稀释的高分辨气相色谱/高分辨质谱联用法,血清样品经C18柱固相萃取、酸性硅胶柱和活性炭柱净化的前处理方法,用DB-5MS毛细管柱(60 m×0.25 mm×0.25μm)分离,高分辨质谱检测分析。结果本方法的检出限为0.35~3.26 pg/g脂肪计,采用血清国际标准参考物质(SRM 1958)进行方法验证,与SRM 1958给出的参考质量分数值范围对比,17个PCDD/Fs单体浓度测定值均在参考质量分数值范围内,相对标准偏差为2%~19%(n=3)。该方法进一步应用于实际人体血清分析,同位素标记的17个二噁英单体回收率为61%~135%。结论本方法灵敏度和准确度高、方法性能稳定,满足人体血清二噁英检测方法的要求。

Establishment the method for polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans determination in human serum

OBJECTIVE To establish the determination method for polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans(PCDD/Fs)in human serum,and further to provide an operable and scientific determination protocal and basis for conducting human health risk assessment for PCDD/Fs.METHODS The serum samples were pretreated by C18 column solid phase extraction,acid silica gel column and activated carbon column purification,separated by DB-5 MS capillary column(60 m×0.25 mm×0.25μm),and PCDD/Fs was quantitative analyzed by high resolution mass spectrometry.RESULTS The method detection limit was in the range of 0.35-3.26 pg/g lipid.This method was further validated using international serum standard reference material sample SRM 1958.According to the reference mass fraction values given for SRM 1958,the concentrations of 17 PCDD/Fs monomers were all in the range of reference mass fraction values,and the relative standard deviation was 2%-19%(n=3).This method was further applied to determination PCDD/Fs in actual serum of human body.The result showed that the recovery rate of isotope labeled PCDD/Fs internal standards were in the range of 61%-135%.CONCLUSION The performance of the method is highly sensitive,stable and highly accurate,which meets the requirements for the determination of PCDD/Fs in human serum and the method can be applied to human health risk assessment for PCDD/Fs in the future.