QuEChERS-气相色谱-质谱联用法同时测定水产品中6种丁香酚类麻醉剂的残留量

Determination of 6 kinds of eugenol derivatives residues in aquatic products by QuEChERS-gas chromatography-mass spectrometry

中文关键词:  QuEChERS  气相色谱-质谱法  丁香酚类化学物  水产品  渔用麻醉剂

英文关键词:QuEChERS  gas chromatography-mass spectrometry  eugenol derivatives  aquatic products  fish anesthetic

中文摘要:

      目的 建立QuEChERS-气相色谱-质谱联用法同时测定水产品中6种丁香酚类麻醉剂残留量的分析方法。方法 样品采用乙腈超声提取、基于QuEChERS方法净化、RTX-5MS(25 m×0.25 mm, 0.25 μm)毛细管柱分离后, 采用SIM模式检测, 外标法定量。结果 6种丁香酚类麻醉剂在5.0~100 μg/L范围内具有良好的线性关系, 相关系数为0.9921~0.9995; 对于5.00 g样品方法的检出限(limit of detection, LOD)为1.0~2.0 μg/kg, 定量限(limit of quantitation, LOQ)为2.5~5.0 μg/kg; 10、20、80 μg/kg添加水平的加标实验中, 平均回收率范围为73.2%~101.8%, 相对标准偏差(relative standard deviation, RSD)为3.4%~13.6%。结论 本方法具有操作简便、快速、灵敏度高、实用性强等特点, 符合丁香酚类麻醉剂残留分析要求。

英文摘要:

      Objective To establish a method for the simultaneous determination of 6 kinds of eugenol derivatives residues in aquatic products by QuEChERS-gas chromatography-mass spectrometry. Methods The samples were ultrasonic extracted by acetonitrile and purified by a modified QuEChERS method. The target compounds were separated on RTX-5MS column (25 m×0.25 mm, 0.25 μm) and detected by SIM mode. External standard method was applied for quantitative analysis. Results The linear range was from 5.0 to 100 μg/L with good correlation coefficients (r=0.9921~0.9995) for 6 kinds of eugenol derivatives. The limits of detection (LODs) and limits of quantitation (LOQs) were 1.0~2.0 μg/kg and 2.5~5.0 μg/kg for all compounds based on a 5.0 g sample. When the spiked concentrations were 10, 20 and 80 μg/kg, the average recoveries were in the range of 73.2%~101.8% with the relative standard deviations (RSDs) of 3.4%~13.6%. Conclusion This method is simple, quick, highly sensitive and practical and it can meet the requirements of residual analysis.