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目的建立猪肉和鸡肉组织中五氯酚的气相色谱-离子阱质谱(MS~n)同位素内标衍生测定方法,为国家食品污染和有害因素风险监测提供实验室依据,以保障消费者食品安全。方法样品中加入内标2,4-二溴酚-D_3后,经5%三氯乙酸沉淀蛋白质,正己烷-乙酸乙酯溶液振荡提取,SLC柱净化后,乙酸酐-吡啶溶液衍生,Thermo Fisher ELite-5MS色谱柱(30 m×0.25 mm,0.25μm)分离,GC-MS~n(n=2)模式测定,同位素内标法定量。结果五氯酚被衍生剂衍生成五氯苯乙酸酯,2,4-二溴酚-D3被衍生成2,4-二溴苯乙酸酯-D_3,两者均得到很好的响应,五氯酚的浓度为10 ng/ml~1 000 ng/ml时,线性关系良好,相关系数为0.999,检出限为0.3μg/kg。在3种加标浓度下,空白基质五氯酚的加标回收率为70%~93%,相对标准偏差为4%~23%。结论该方法的灵敏度高,选择性好,定性、定量准确,适用于猪肉和鸡肉中五氯酚钠残留的检测要求。
Objective To establish a gas chromatography - ion trap mass spectrometry (MS ~ n) internal standard derivatization method for determination of pentachlorophenol in pork and chicken tissues and provide a laboratory basis for the national risk monitoring of food contamination and harmful factors to ensure the safety of consumers’ food. Methods After the internal standard 2,4-dibromophenol-D_3 was added into the sample, the protein was precipitated with 5% trichloroacetic acid and extracted with n-hexane-ethyl acetate. The residue was purified by SLC column and derivatized with acetic anhydride-pyridine. Thermo Fisher ELite-5MS column (30 m × 0.25 mm, 0.25 μm), GC-MS ~ n (n = 2) mode and isotope internal standard method. As a result, pentachlorophenol was derivatized to pentachlorophenylacetate by derivatizing agent and 2,4-dibromophenol-D3 was derivatized to 2,4-dibromophenylacetate-D3, both of which were well responded to, When the concentration of pentachlorophenol was 10 ng / ml ~ 1 000 ng / ml, the correlation coefficient was 0.999 and the limit of detection was 0.3 μg / kg. The spiked recoveries of blank matrix pentachlorophenol were 70% ~ 93% and the relative standard deviations were 4% ~ 23% at the three spiked concentrations. Conclusion The method of high sensitivity, good selectivity, qualitative, quantitative and accurate, suitable for pork and chicken pentachlorophenol sodium residue detection requirements.