目的：建立食品样品中P26, P50, P62等三大指示性毒杀芬的检测分析方法,为进一步开展常规监测提供技术平台和基础数据。方法食品样品使用索式提取系统(Soxtec)提取,提取液依次由30%酸性硅胶柱和氧化铝柱净化,利用同位素稀释-高分辨气相色谱/高分辨双聚焦磁式质谱联用(ID-HRGC/HRMS)技术对三种指示性毒杀芬单体P26, P50, P62进行定量定性分析。结果本研究所建成的检测方法相对标准偏差(RSD)小于25%,回收率可以达到40%~120%；P26, P50, P62的方法检测限分别为0.08、0.02、0.06 pg/g；方法性能达到开展食品样品中毒杀芬检测技术的要求。结论该方法可以对食品样品中毒杀芬进行检测,检测效率高,结果准确可靠。%Objectives To develop the analyzing methods of 3 indicator toxaphenes (P26, P50 and P62) in food samples, so as to provide technical platform and basic data for further routine monitoring. Methods The food sample was extracted by using Soxtec followed by purification on 30%multilayer acidic silica column and neutral aluminum oxides column, utilizing isotope dilution high-resolution gas chromatography/high-resolution double-focusing magnetic mass spectrometry (HRGC/HRMS) to carry out quantitative and qualitative analysis on toxaphene monomer P26, P50, and P62. Results The developed analytical method for three indicator tox-aphenes monomer was built successfully, and suitable for the determination of toxaphene specific congeners in food. The relative standard deviation (RSD) was below 25% and the spiked recoveries were in the range of 40%~120%. The five point calibration curves showed a good linearity for all the congeners (R2>0.99). Method detection limit (MDL) was 0.08, 0.02, and 0.06 pg/g for P26, P50, and P62, respectively. Conclusion Three congeners of toxaphene can be measured simultaneously in food sample matrix, the method is efficient and the results are accurate and reliable.
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