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猪可食性组织中氟尼辛残留量的UPLC-MS/MS检测方法的建立

罗小清 张珍瑞 郭凡溪 郭洋洋 吴峰 余祖功

南京农业大学学报2017,Vol.40Issue(6):1105-1110,6.
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

罗小清 1张珍瑞 1郭凡溪 1郭洋洋 1吴峰 1余祖功1

作者信息

  • 1. 南京农业大学动物医学院,江苏南京210095
  • 折叠

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)

南京农业大学学报

OA北大核心CSCDCSTPCD

1000-2030

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