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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 ,高灵敏度
OBJECTIVE To determine 17 4 ~ 8 chlorine-substituted dioxins and furans in milk by high resolution gas chromatography / high resolution dual confocal mass spectrometry (HRGC / HRMS). Methods The samples were identified as HRGC / HRMS -MID by liquid-liquid extraction, carbon column enrichment, column chromatography, and quantified by the strict quality control and isotope dilution method of the American EPA 16 13 method. This method can be quantified to the pg / g ppt level. Results The limit of detection (TCDF) and TCDD (TCDD) of this method were 0 0 2 2 2 pg / μl and 0 0 317 pg / μl, respectively. The detection limits of 17 PCDDs / PCDFs were the lowest. The recoveries of isotope standards ranged from 58.46% to 79.99%. 1, 2, 3,7,8-PeCDF, 1,2,4,7,8,9-HpCDF, 2,3,7,8-TCDD were not detected in the sample 17 homologues isomers The highest contents of OCDF and OCDD were 0 0 6 5 pg / g and 0 2 0 2 pg / g, respectively. The total TEQ of the samples was 0 0 33 pg TEQ / g. Conclusion High-resolution gas chromatography / high resolution dual-confocal magnetic resonance spectroscopy and isotope dilution method for the detection of the target compound Erhualin, the qualitative, quantitative and accurate, high sensitivity