HRGC/HRMS定量检测市售牛奶中二湲碢和呋喃  

Detrmination of Polychlorinated Dibenzo-p-Dioxins and Dibenzo-Furans in Saled Milk by Isotope Dilution High Resolution Gas Chromatography/High Resoultion Mass Spectrometry(HRGC/HRMS)

作　　者：张建清[1] 姜杰 刘桂华[1] 李良成[1] 钟伟祥 

机构地区：[1]深圳市卫生防疫站,518020 [2]香港政府化验所

出　　处：《中国公共卫生》2002年第3期356-358,共3页Chinese Journal of Public Health

摘　　要：目的　采用高分辨气相色谱 /高分辨双聚焦磁式质谱联用仪 (HRGC/HRMS)定量检测了牛奶中 17个 4～ 8个氯原子取代的二和呋喃。方法　样品中的二经过液 -液萃取、碳柱富集、色谱柱纯化、分离 ,以HRGC/HRMS -MID方法检测 ,用美国EPA16 13方法进行严格的质量控制和同位素稀释的方法定量 ,该方法定量可精确到pg/g即 ppt水平。结果　该方法的检测限TCDF和TCDD分别为 0 0 2 2 2 pg/ μl和 0 0 317pg/ μl,在 17个PCDDs/PCDFs中 ,其检测限为最低。同位素标准物的回收率分布于 5 8 4 6 %～ 79 99%之间。 1,2 ,3,7,8-PeCDF、1,2 ,3,4 ,7,8,9-HpCDF、2 ,3,7,8-TCDD均未检出 ,样品中 17个同系物异构体以OCDF和OCDD的含量为最高 ,分别为0 0 6 5 pg/g和 0 2 0 2 pg/g ,样品的总TEQ值为 0 0 33pgTEQ/g。 结论　采用高分辨气相色谱 /高分辨双聚焦磁式质谱联用仪和同位素稀释的方法对基质中的目标化合物二进行检测 ,该法定性、定量准确 。Objective A sensitive and accurate High Resolution Gas Chromatography/High Resolution Mass Spectrometry(HRGC/HRMS)method was developed for determinating seventeen Polychlorinated Dibenzo-p-Dioxins and Dibenzo-Furans in saled milk using isotope dilution quantitation technique.Methods Dibenzo-p-Dioxins and Dibenzo-Furans was extracted from milk by liquid-liquid extraction,carbon column enrichment,chromatograph column cleaning up,separation,and followed by HRGC/HRMS-MID determination and quantitation in ppt(pg/g)level.Results The method Detection Limit for TCDF and TCDD is 0.022 2pg/μl and 0.031 7pg/μl respectively.The recovery was 58.46%-79.99%,1,2,3,7,8-PeCDF,1,2,3,4,7,8,9-HpCDF,2,3,7,8-TCDD was non-detection,concentration of OCDF and OCCD were 0.065pg/g and 0.202pg/g in the sample respectively among all the seventeen Dioxins and Furan,and Total Toxicity Equivalency Factor(TEQ) was 0.033pg TEQ/g.Conclusion HRGC/HRMS and method of isotope dilution had the characteristics of quality, accurate quantative,high sensitvity in determinating dioxins of matrix.

关 键 词：HRGC/HRMS 同位素稀释 二恶英 呋喃 牛奶 食品检验 食品卫生 

分 类 号：R155.57[医药卫生—营养与食品卫生学]