摘要
目的:建立5种动物源食品中氟啶虫酰胺残留量的气相色谱检测及液相色谱-质谱联用确证方法。方法:4种肉和水产品样品经乙酸乙酯均质提取,提取液经凝胶渗透色谱仪和氨基固相萃取柱净化,蜂蜜经CHROMABOND XTR固相萃取柱和氨基固相萃取柱净化,气相色谱仪带电子捕获(ECD)检测器和液相色谱-串联质谱仪带电喷雾(ESI源)进行氟啶虫酰胺残留量的分析和确证分析。结果:气相色谱法中氟啶虫酰胺在10μg/kg～500μg/kg呈线性关系(r≥0.999),5种动物源食品添加氟啶虫酰胺浓度为10μg/kg～200μg/kg时,回收率为74.5%～98.2%,相对标准偏差为1.02%～7.98%,检出限(LOD)为1.0μg/kg,定量限(LOQ)为5.0μg/kg。液质联用法作为氟啶虫酰胺的确证方法,检测低限为5.0μg/kg。结论:该方法简便、快速、准确。
Objective：To establish a method for determination and confirmation of flonicamid residue in five kinds of animal-derived foods by gas chromatography（GC） and liquid chromatography mass-mass spectrometry（LC/MS-MS）.Methods： The samples of meat and aquatic products were extracted by ethyl acetate,then the extract was cleaned up by gel permeation chromatography（GPC） and NH2SPE cartridge,while honey was cleaned up by CHROMABOND XTR and NH2SPE cartridges.The concentration of flonicamid residue was analyzed by GC with ECD and confirmed by LC/MS-MS with EI.Results： For GC-ECD,there was a good linear relationship between the peak area and the concentration of flonicamid within range of 10 μg/kg to 500 μg/kg（correlation coefficient ≥ 0.999）.When the spiked level of flonicamid ranged from 10 μg/kg to 200 μg/kg,the mean recoveries of the method varied from 74.5% to 98.2% and the relative standard deviations（RSD） ranged from 1.02% to 7.98%.The results showed that the limit of detection（LOD） was 1.0 μg/kg and the limit of quantification（LOQ） was 5.0 μg/kg.The flonicamid was confirmed by LC/MS-MS and the limit of detection was 5.0 μg/kg.Conclusion： The method was simple,fast and accurate.
出处
《中国卫生检验杂志》
CAS
2011年第11期2604-2608,共5页
Chinese Journal of Health Laboratory Technology
基金
应对"日本肯定列表制度"关键技术研究和应用(2006Z1-E0121)
