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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至8个氯原子取代的噁英和呋喃。样品中的二噁英经过液-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EPA1613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。结果表明,同位素标准物的回收率分布于58.46％～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0.065pg/g和 0.202pg/g,样品的总TEQ值为0.033pgTEQ/g。该方法定性、定量准确,为目前国际上权威认可的二噁英定量检测方法。
Dioxins and furans substituted with 17 4 to 8 chlorine atoms in milk were quantitatively detected by HRGC / HRMS with high resolution gas chromatography / high resolution dual confocal mass spectrometry (HRGC / HRMS). Dioxins in the samples were determined by HRGC / HRMS-MID method after liquid-liquid extraction, carbon column enrichment and column purification, and were quantified by the strict quality control and isotope dilution method of American EPA1613 method. Quantitative accurate to pg / g that ppt level. The results showed that the recoveries of isotope standards ranged from 58.46% to 79.99%. 1,2,3,7,8-PeCDF, 1,2,3,4,7,8,9-HpCDF, 2,3,7,8-TCDD were not detected, 17 homologs The body was highest in OCDF and OCDD, at 0.065 pg / g and 0.202 pg / g, respectively, with a total TEQ of 0.033 pgTEQ / g. The method of qualitative, quantitative and accurate, for the current international authoritative dioxin quantitative detection methods.