南京农业大学学报2017,Vol.40Issue(6):1105-1110,6.DOI:10.7685/jnau.201606019
猪可食性组织中氟尼辛残留量的UPLC-MS/MS检测方法的建立
Development of an ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of flunixin in edible swine tissues
摘要
Abstract
[Objectives] To establish a reliable,rapid and sensitive method for determination of flunixin residues in swine tissues (muscle,skin + fat,liver,kidney),ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed and optimized.[Methods] The samples were extracted with acetonitrile and ethyl acetate (volume ratio 1 ∶ 1),and then purified via an Oasis MCX solid-phase extraction cartridge.Chromatographic separation was performed on an Acquity UPLC BEH C18 column.The analysis was carried out on UPLC-ESI-MS/MS working with multiple reaction monitoring mode.External standard was used for quantitation of target drug.[Results] The analyte has a good hnearity at the range of 0.5-500 μg· kg-1,with related coefficient of R2>0.999.Recoveries of spiked samples ranged from 74.8% to 90.3% with relative standard deviation(RSD) less than 16.5 %.The limits of detection (LOD) and quantification (LOQ) were 0.5 and 1.0 μg· kg-1,respectively.[Conclusions] The results show that the pretreatment and purification process established by this study are easy to operate.The method has good stability,reproducibility,sensitivity,and great accuracy.关键词
氟尼辛/猪可食性组织/UPLC-MS/MS/残留Key words
flunixin/edible swine tissues/UPLC-MS/MS/residues分类
农业科技引用本文复制引用
罗小清,张珍瑞,郭凡溪,郭洋洋,吴峰,余祖功..猪可食性组织中氟尼辛残留量的UPLC-MS/MS检测方法的建立[J].南京农业大学学报,2017,40(6):1105-1110,6.基金项目
农业行业标准制定与修订(农产品质量安全)项目(2014) (农产品质量安全)