QuEChERS-液相色谱-串联质谱法同时测定水产品中11种卡因类麻醉剂及其3种代谢物残留量

Simultaneous determination of 11 kinds of caine anesthetics and their 3 kinds of metabolites in aquatic products by QuEChERS-liquid chromatography-tandem mass spectrometry

中文关键词:  液相色谱-串联质谱  卡因类麻醉剂  QuEChERS  水产品

英文关键词:liquid chromatography-tandem mass spectrometry  caine anesthetic  QuEChERS  aquatic product

中文摘要:

      目的 建立一种QuEChERS-液相色谱-串联质谱法同时测定水产品中11种卡因类麻醉剂及其3种代谢物残留量的分析方法。方法 样品经乙腈提取, 无水MgSO4和 NaCl除水, 再经100 mg N-丙基乙二胺(primary secondary amine, PSA)进行净化, 后过0.22 μm有机微孔滤膜, 经液相色谱-串联质谱进行定性定量分析。结果 11种卡因类麻醉剂及其3种代谢物在0.01~5.00 μg/L质量浓度范围内呈良好的线性关系, 相关系数(r)为0.99529~0.99989, 11种卡因类麻醉剂及其3种代谢物的方法检出限(limit of detection, LOD)为0.05~2.00 μg/kg, 方法定量限(limit of quantification, LOQ)为0.15~5.00 μg/kg。在南美白对虾、鲤鱼、多宝鱼3种基质中, 分别进行1倍LOQ、2~2.5倍LOQ和10倍LOQ 3个水平的加标试验, 11种卡因类麻醉剂及其3种代谢物在3种添加水平中的回收率分别为71.3%~114.2%、71.2%~107.0%、70.4%~104.5%, 相对标准偏差分别为0.7%~11.2%、0.5%~11.5%以及0.8%~14.2%。利用该方法对市售的50批次不同品种的水产品进行检测, 结果表明在4批次产品中有卡因类麻醉剂检出, 其余46批产品未检出, 检出率8%; 检出的项目主要为三卡因、苯佐卡因、间氨基苯甲酸和对氨基苯甲酸, 含量在5.68~90.80 μg/kg, 其余10种化合物均未被检出。结论 该方法操作简单快捷, 具有较高的灵敏度、准确度和精密度, 且可同时测定水产品中的多种卡因类麻醉剂, 适用于批量样品的测定, 具有较高的实际应用意义, 可为食品安全监测提供有力的技术支持。

英文摘要:

      Objective To Establish a method for simultaneous determination of 11 kinds of caine anesthetics and their 3 kinds of metabolites in aquatic products by QuEChERS-liquid chromatography-tandem mass spectrometry. Methods The samples were extracted by acetonitrile, dehydrated by anhydrous MgSO4 and NaCl, purified by 100 mg primary secondary amine (PSA), filtered by 0.22 μm organic microporous membrane, and qualitatively and quantitatively determined by liquid chromatography-tandem mass spectrometry. Results The 11 kinds of caine anesthetes and their 3 kinds of metabolites showed a good linear relationship in the mass concentration range of 0.01–5.00 μg/L, and the correlation coefficients (r) were 0.99529–0.99989. The limit of detection (LOD) and the limit of quantification (LOQ) of 11 kinds of caine anesthetics and their 3 kinds of metabolites were 0.05–2.00 μg/kg and 0.15–5.00 μg/kg, respectively. The 3 kinds of substrates, white shrimp, carp and turbinus were performed at 3 levels: 1 times LOQ, 2–2.5 times LOQ and 10 times LOQ. The recoveries of 11 kinds of caine anesthetics and their 3 kinds of metabolites in 3 samples were 71.3%–114.2%, 71.2%–107.0% and 70.4%–104.5%, and the relative standard deviations were 0.7%–11.2%, 0.5%–11.5% and 0.8%–14.2%. The method was used to detect 50 batches of different varieties of aquatic products in the market. The results showed that 4 batches of products were detected with caine anesthetic, and the other 46 batches were not detected, the detection rate was 8%. The detected items were mainly tricaine, benzocaine, m-aminobenzoic acid and p-aminobenzoic acid, the content of which were 5.68–90.80 μg/kg, and the other 10 kinds of compounds were not detected. Conclusions The method is simple and fast, has high sensitivity, accuracy and precision, and can simultaneously determine a variety of caine anesthetics in aquatic products. It is suitable for the determination of batch samples, and has high practical application significance, and can provide powerful technical support for food safety monitoring.