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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)定量检测奶粉中二英类化合物。方法 采用索式抽提和自动纯化系统等仪器对奶粉样品中的二英组分进行纯化和富集 ,采用同位素稀释法 ,以HRGC/HRMS联用仪检测。结果 同位素标准物的回收率分布于 90 6%～ 116 3 %之间 ,CRM 5 3 4的检测结果均在标准值范围之内 ,3次实验结果的RSD <2 0 % ,该方法检测下限可达pg/g水平。 结论 该方法灵敏、定性、定量准确 ,为目前国际上权威机构认可的二英定量检测方法。
OBJECTIVE To quantitatively detect dioxins in milk powder by high resolution gas chromatography / high resolution dual confocal mass spectrometry (HRGC / HRMS). Methods Soxhlet components of milk powder samples were purified and enriched by means of Soxhlet extraction and automatic purification system. The isotope dilution method was used to detect the two components of milk powder samples by HRGC / HRMS. Results The recoveries of isotope standards ranged from 90 6% to 116 3%. The results of CRM 5 34 were all within the standard values and the RSDs of 3 experiments were less than 20%. The detection limit of this method was Up to pg / g level. Conclusion The method is sensitive, qualitative and quantitative, and accurate. It is a validated method for quantitative determination of Erzanne in the world.