QuEChERS-气相色谱-三重四极杆串联质谱法测定动物源食品中苯菌酮残留

Determination of metrafenone residue in animal-derived foods by QuEChERS combined with gas chromatography-triple quadrupole tandem mass spectrometry

目的建立QuEChERS前处理结合气相色谱-三重四极杆串联质谱法(gas chromatography-triple quadrupole tandem mass spectrometry,GC-MS/MS)测定3种动物源食品(鱼肉、鸡肉和猪肉)中苯菌酮残留量的分析方法。方法动物源性试样用1%甲酸乙腈振荡提取,提取液经QuEChERS提取盐包提取及石墨化碳黑/乙二胺基-N-丙基柱(graphitized carbon black/primary secondary amine,GBC/PSA)净化,滤液氮吹至近干,乙酸乙酯定容,在电子轰击离子源(electron impact source,EI)和定时选择反应检测(timed selective reaction monitoring,Timed-SRM)模式下分析,基质匹配曲线,外标法定量。结果苯菌酮在0.005~0.100μg/mL的不同基质质量浓度范围内都呈线性关系,相关系数为0.9999、0.9994和0.9997。在0.01、0.02、0.05 mg/kg 3个添加水平下,苯菌酮在鱼肉、鸡肉和猪肉中的平均回收率范围均处于91%~105%之间,相对标准偏差(relative standard deviations,RSDs)小于等于11.2%,苯菌酮在3种基质中的定量限均为0.01 mg/kg。结论本方法具有快速、简便、灵敏等特点,能满足动物源食品中苯菌酮的检测。

Objective To establish an analytical method for determination of metrafenone residues in 3 kinds of animal-derived foods(fish,chicken and pork)by QuEChERS pretreatment combined with gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS).Methods The samples of animal-derived foods were extracted with 1%formic acid acetonitrile under shaking condition,and the extractive solutions were subjected to salt package extraction by QuEChERS extraction and purification by graphitized carbon black/primary secondary amine(GBC/PSA)column,the nitrogen in the filtrate was blown to near dryness,and the volume of ethyl acetate was fixed,the analytes were analyzed in electron impact source(EI)and timed selective reaction monitoring(Timed-SRM)modes,with matrix matching curve and external standard method for quantification.Results A linear relationship was established across the mass concentration ranges of 0.005-0.100μg/mL metrafenone,with correlation coefficients of 0.9999,0.9994 and 0.9997.Under the 3 addition levels of 0.01,0.02 and 0.05 mg/kg,the average recovery rates of metrafenone in fish,chicken and pork were within the range of 91%-105%,the relative standard deviations(RSDs)were less than or equal to 11.2%,and the limits of quantitation of metrafenone in the three matrices were 0.01 mg/kg.Conclusion This method is rapid,simple and sensitive,and can meet the requirements of detection of metrafenone in food of animal-derived foods.