快速滤过型净化结合液相色谱-串联质谱法同时测定水产品中16种麻醉剂及其代谢物残留量

Simultaneous determination of 16 kinds of anesthetics and metabolites residual amount in aquatic products by multi-plug filtration cleanup method combined with liquid chromatography-tandem mass spectrometry

中文关键词:  水产品  麻醉剂  快速滤过型净化  液相色谱-串联质谱法

英文关键词:aquatic products  anesthetics  multi-plug filtration cleanup  liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立基于快速滤过型净化(multi-plug filtration cleanup, m-PFC)技术结合液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)同时测定水产品中16种麻醉剂及其代谢物残留量的分析方法。方法 样品经1%甲酸乙腈溶液提取, 提取液盐析后, 经采用无水硫酸镁、N-丙基乙二胺(primary secondary amine, PSA)、增强型脂质去除(enhanced matrix removal-lipid, EMR-Lipid)净化材料装填的m-PFC柱净化, 以甲醇和含0.1%甲酸的2 mmol/L甲酸铵水溶液为流动相, 经C18色谱柱分离, 电喷雾正/负离子扫描, 多反应监测模式下检测, 基质外标法定量。结果 16种麻醉剂及其代谢物在各自的浓度范围内线性关系良好(相关系数r2>0.996), 方法检出限(信噪比为3)为0.03~0.30 μg/kg, 定量限(信噪比为10)为0.10~1.00 μg/kg; 在空白样品基质中低、中、高3个浓度水平下的加标回收率为79.3%~113.8%, 相对标准偏差为1.3%~7.2% (n=6)。结论 该方法操作简便、灵敏度高、稳定性好, 适用于鲜活水产品中16种麻醉剂及其代谢物残留量的快速测定。

英文摘要:

      Objective To establish a method for the simultaneous determination of 16 kinds of anesthetics and metabolites residual amount in aquatic products by multi-plug filtration cleanup (m-PFC)-liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Samples were extracted with acetonitrile containing 1% formic acid, separated by salting-out, and the upper acetonitrile was purified by m-PFC column packed with anhydrous magnesium sulfate, primary secondary amine (PSA), and enhanced matrix removal-lipid (EMR-Lipid). The targets were separated by C18 column using methanol-2 mmol/L ammonium formate containing 0.1% formic acid as mobile phase for gradient elution, detected by positive or negative electrospray ionization-tandem mass spectrometry under multiple reaction monitoring mode, and quantified with matrix external standard method. Results The 16 kinds of anesthetcs and metabolites showed good linear relationships in their respective concentration ranges (r2>0.996). The limits of detection (S/N=3) and limits of quantitation (S/N=10) were 0.03–0.30 μg/kg and 0.10–1.00 μg/kg. The average recoveries at low, medium and high concentration levels in the blank sample matrix were 79.3%–113.8%, and the relative standard deviations were 1.3%–7.2% (n=6). Conclusion This method is simple to operate, sensitive and good in stability, which can be applied to the rapid detection of 16 kinds of anesthetics and metabolites in aquatic products.