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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。
Objective To establish a method for the detection and analysis of three indicated toxic pesticides such as P26, P50 and P62 in food samples, and provide a technical platform and basic data for further routine monitoring. Methods The food samples were extracted by Soxtec. The extracts were purified by 30% acidic silica gel column and alumina column, and identified by isotope dilution-high resolution gas chromatography / high resolution dual confocal mass spectrometry (ID-HRGC / HRMS) techniques were used to quantitatively and qualitatively analyze the three indicated toxic monomers P26, P50 and P62. Results The relative standard deviations (RSDs) of detection methods established in this study were less than 25% and the recovery rates were 40% -120%. The detection limits of P26, P50 and P62 were 0.08, 0.02 and 0.06 pg / g, respectively. To carry out food poisoning poisoning detection technology requirements. Conclusion The method can detect toxaphene in food samples with high detection efficiency and accurate and reliable results.