摘要
目的建立Qu ECh ERS-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Qu ECh ERS方法净化、RTX-5MS(25 m×0.25 mm,0.25μm)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5.0~100μg/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1.0~2.0μg/kg,定量限(limit of quantitation,LOQ)为2.5~5.0μg/kg;10、20、80μg/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。
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 Qu ECh ERS method. The target compounds were separated on RTX-5 MS 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.
出处
《食品安全质量检测学报》
CAS
2018年第2期422-428,共7页
Journal of Food Safety and Quality
基金
广东检验检疫局科技项目(2016GDK30)
国家质量监督检验检疫总局科技项目(2015IK058)
湛江市财政资金科技专项(2012E0202)~~