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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)定量检测了奶粉中十七个四至八个氯原子取代的二(口恶)英和呋哺。[方法]采用美国EPA1613方法进行严格的质量控制和同位素稀释的方法定量,对奶粉样品进行索式抽提、自动纯化系统纯化、以HRGC/HRMS-MID方法检测样品中的二(口恶)英。[结果]同位素标准物的回收率分布于90.6%~116.28%之间,检出限在0.077-0.97pg/g。该方法定量可精确到pg/g水平。实验过程中可以控制系统不受污染,样品中只检出1,2,3,4,7,8-HxCDF。[结论]该方法灵敏、定性、定量准确,为目前国际上权威认可的二(口恶)英定量检测方法。
[Objective] The purpose of the present study was to quantitatively detect the dioxins and furilazepines substituted with seventeen four to eight chlorine atoms in milk powder by high resolution gas chromatography / high resolution dual confocal mass spectrometry (HRGC / HRMS). [Method] The method of US EPA1613 was used for the quantitative determination by strict quality control and isotope dilution method. The milk powder samples were sowed and purified by automatic purification system. The samples were analyzed by HRGC / HRMS-MID . [Result] The recoveries of isotope standard ranged from 90.6% to 116.28% with the detection limit of 0.077-0.97pg / g. The method can be quantified to the pg / g level. During the experiment, the system can be controlled from being contaminated, and only 1,2,3,4,7,8-HxCDF is detected in the sample. [Conclusion] The method is sensitive, qualitative and accurate. It is the internationally accepted method for the quantitative determination of bis (Omeprazole).