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

中文关键词:  QuEChERS  气相色谱-三重四极杆串联质谱法  动物源食品  苯菌酮  残留

英文关键词:QuEChERS  gas chromatography-triple quadrupole tandem mass spectrometry  animal-derived foods  metrafenone  residues

中文摘要:

      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0.005~0.100 μg/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。

英文摘要:

      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?0.100 μg/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.