[1]罗小清,张珍瑞,郭凡溪,等.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.[doi:10.7685/jnau.201606019]
 LUO Xiaoqing,ZHANG Zhenrui,GUO Fanxi,et al.Development of an ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of flunixin in edible swine tissues[J].Journal of Nanjing Agricultural University,2017,40(6):1105-1110.[doi:10.7685/jnau.201606019]
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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()
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《南京农业大学学报》[ISSN:1000-2030/CN:32-1148/S]

卷:
40卷
期数:
2017年6期
页码:
1105-1110
栏目:
出版日期:
2017-11-10

文章信息/Info

Title:
Development of an ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of flunixin in edible swine tissues
作者:
罗小清 张珍瑞 郭凡溪 郭洋洋 吴峰 余祖功
南京农业大学动物医学院, 江苏 南京 210095
Author(s):
LUO Xiaoqing ZHANG Zhenrui GUO Fanxi GUO Yangyang WU Feng YU Zugong
College of Veterinary Medicine, Nanjing Agricultural University, Nanjing 210095, China
关键词:
氟尼辛猪可食性组织UPLC-MS/MS残留
Keywords:
flunixinedible swine tissuesUPLC-MS/MSresidues
分类号:
S859
DOI:
10.7685/jnau.201606019
摘要:
[目的] 建立一种可靠、快速、灵敏的超高效液相色谱-串联质谱法(UPLC-MS/MS)用于猪可食性组织中氟尼辛残留量的检测。[方法] 猪可食性组织(肌肉、皮脂、肝脏、肾脏)经绞碎、均质后,用乙酸乙酯-乙腈(体积比1:1)提取,MCX固相萃取柱净化,Acquity UPLC BEH C18色谱柱梯度洗脱,在电喷雾正离子(ESI+)下选用多反应监测(MRM)模式进行待测物的分析,外标法定量。[结果] 该方法的检测限(LOD)与定量限(LOQ)分别为0.5 μg·kg-1和1.0 μg·kg-1;待测物氟尼辛含量在0.5~500 μg·kg-1范围内,峰面积与药含量呈良好的线性关系(R2>0.999);氟尼辛在猪肌肉、皮脂、肝脏、肾脏组织中的添加回收率为74.8%~90.3%,批内精密度及批间精密度均不大于16.5%。[结论] 建立了猪超高效液相色谱-串联质谱检测方法,适用于猪可食性组织中氟尼辛残留量的测定。
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 linearity 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.

参考文献/References:

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备注/Memo

备注/Memo:
收稿日期:2016-06-15。
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)
作者简介:罗小清,硕士研究生。
通信作者:余祖功,副教授,主要从事新兽药药理研究及兽药新制剂的研发,E-mail:yuzugong@njau.edu.cn。
更新日期/Last Update: 1900-01-01