以国内外文献及标准方法为基础,优化了血清中17种2、3、7、8位取代的PCDD/Fs的测定方法,建立了同位素内标稀释-索式萃取一段法层析柱净化-高分辨气质联用分析方法.实验结果表明,17种2、3、7、8位取代的PCDD/Fs的方法检出限范围为3.72—14.74 pg.基质加标实验中目标化合物回收率为94.61%—117.14%,标准参考物质SRM1958中PCDD/Fs的多数单体测定结果也在参考值范围内.实际样品同位素内标回收率为66.2%—95.2%,RSD是4.0%—9.0%.该分析方法准确可靠、灵敏、操作简便,适用于血清中二噁英的测定.
Based on the domestic and international literatures and standard methods,this research developed a method for detecting dioxins in serum by Soxhlet extraction chromatography column purification-isotope dilution HRGC-HRMS analysis.The results showed that the limit detection of method was in the range of 3.72—14.74 pg,and the recoveries of 12C—PCDD/Fs ranged from 94.61%—117.14% for matrix spiking samples.The method was successfully employed for the determination of dioxin ins the standard reference material SRM1958.The recovery and the relative standard deviation were in the range of 66.2%—95.2% and 4.0%—9.0% for real samples,respectively.It was proved that this method was accurate,sensitive,operable,and suitable for the determination of dioxins in serum.