分散固相萃取-气相色谱-四极杆-飞行时间质谱法快速测定鲜鱼中的5种酚类麻醉剂

Rapid determination of 5 kinds of phenolic anesthetics in fresh fishes by dispersive solid phase extraction-gas chromatography-quadrupole- time of flight mass spectrometry

中文关键词:  气相色谱-四极杆-飞行时间质谱法  分散固相萃取  鲜鱼  酚类麻醉剂

英文关键词:gas chromatography-quadrupole-time of flight mass spectrometry  dispersive solid phase extraction  fresh fish  phenolic anesthetics

中文摘要:

      目的 建立分散固相萃取-气相色谱-四极杆-飞行时间质谱法(gas chromatography-quadrupole-time of flight mass spectrometry, GC-Q-TOF/MS)测定鲜鱼中5种酚类麻醉剂的快速分析方法。方法 样品经乙酸乙酯提取后, 氮气浓缩, 复溶后使用C18和乙二胺-N-丙基硅烷(primary secondary amine, PSA)混合粉末净化, 采用电子轰击离子源进行电离, 选择离子对模式对目标母离子和子离子进行测定。结果 5种酚类麻醉剂的空白基质标准曲线在5~500 μg/L范围内呈良好线性关系, 相关系数r均大于0.999, 日内不同水平的加标回收率在83.5%~104.0之间, 相对标准偏差为2.56%~5.28%。方法检出限为3.58~8.96 μg/kg, 定量限为8.46~19.85 μg/kg。结论 该方法操作简单、回收率好、灵敏度高、重复性好, 可满足鲜鱼中酚类麻醉剂快速测定的要求。

英文摘要:

      Objective To establish an analytical method for rapid determination of 5 kinds of phenolic anesthetics in fresh fishes by dispersive solid phase extraction-gas chromatography-quadrupole-time of flight mass spectrometry (GC-Q-TOF/MS). Method The samples were extracted with ethyl acetate, concentrated with nitrogen, redissolved and purified with C18 and primary secondary amine (PSA) mixed powder, ionized by electron impact ion source, the target parent ion and daughter ion were determined by ion pair mode. Result The standard curves of blank matrix of 5 kinds of phenolic anesthetics exhibited good linear relationships in the range of 5?500 μg/L with correlation coefficients r were both greater than 0.999. The recovery rates of different levels within the day were between 83.5% and 104.0%, and the relative standard deviations were between 2.56% and 5.28%. The limits of detection and limits of quantitation were in the range of 3.58?8.96 μg/kg and 8.46?19.85 μg/kg respectively. Conclusion The method concluded simple operation, good recovery rate, high sensitivity and good repeatability that satisfied the requirements of rapid determination of phenolic anesthetics in fresh fish.