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高分辨气相色谱/高分辨双聚焦磁式质谱联用定量检测市售牛奶中的二噁英和呋喃
Determination of Polychlorinated Dibenzo - p - Dioxins and Dibenzo - Furans in saled milk by Isotope Dilution High Resolution Gas Chromatography/High Resolution Mass Spectrometry(HRGC/HRMS)
【摘要】 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。
【Abstract】 A sensitive and accurate High Resolution Gas Chromatography/High Resolution Mass Spectrometry (HRGC/HRMS) method has been developed for determination of seventeen Polychlorinated Dibenzo- p- Dioxins and Dibenzo- Furans in saled milk using isotope dilution quantitation technique. 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. The result showed that 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, the concentration of OCDF and OCDD were 0.065 pg/g and 0.202 pg/g in the sample respectively among all the seventeen Dioxins and Furan, and Total Toxicity Equivalency Factor (TEQ) was 0.033pg TEQ/g.
- 【文献出处】 中国卫生检验杂志 ,Chinses Journal of Health Laboratory Technology , 编辑部邮箱 ,2002年01期
- 【分类号】R155.5
- 【被引频次】4
- 【下载频次】210