磁性石墨烯分散微固相萃取-液相色谱-四极杆串联质谱法测定畜禽肉中9种非甾体抗炎剂

色谱 , 2016, 34(9): 850-859. doi: 10.3724/SP.J.1123.2016.04039

磁性石墨烯分散微固相萃取-液相色谱-四极杆串联质谱法测定畜禽肉中9种非甾体抗炎剂

董婵婵 ^1, , 胡艳云 ^2, , 吕亚宁 ^3, , 宋伟 ^4, , 韩芳 ^5, , 郑平 ^6, , 邓宁 ^7,

1.合肥工业大学化学与化工学院,安徽合肥,230009

2.安徽出入境检验检疫局,安徽合肥230022;安徽医科大学公共卫生学院,安徽合肥230032

3.安徽出入境检验检疫局,安徽合肥230022;食品安全分析与检测安徽省重点实验室,安徽合肥230022

4.安徽出入境检验检疫局,安徽合肥230022;食品安全分析与检测安徽省重点实验室,安徽合肥230022

5.安徽出入境检验检疫局,安徽合肥230022;食品安全分析与检测安徽省重点实验室,安徽合肥230022

6.安徽出入境检验检疫局,安徽合肥230022;食品安全分析与检测安徽省重点实验室,安徽合肥230022

7.合肥工业大学化学与化工学院,安徽合肥,230009

基金项目: 上海长三角科技合作项目(15395810100) Shanghai Yangtze River Science and Technology Cooperation Projects(15395810100) Anhui Science and Technology Program(1604b0602028) 安徽省科技计划项目(1604b0602028).Provincial Natural Science Foundation of Anhui,China(1408085MKL97) State Quality Inspection Administration Science and Technology Projects(2014IK134) 安徽省自然科学基金项目(1408085MKL97) 国家质检总局科技计划项目(2014IK134)

关键词：磁性分散微固相萃取 , 液相色谱-四极杆串联质谱 , 磁性石墨烯纳米复合材料 , 非甾体类抗炎剂 , 畜禽肉

Magnetic graphene based dispersive micro-solid-phase extraction coupled with liquid chromatography-tandem quadrupole mass spectrometry for the analysis of nine non-steroidal anti－inflammatory drugs in livestock and poultry meat

Keywords： dispersive micro-solid-phase extraction , liquid chromatography-quadrupole mass spectrometry (LC-MS/MS) , magnetic graphene nanocomposite , non-steroidal anti-inflammatory drugs , livestock and poultry meat

以磁性石墨烯纳米复合材料(Fe3O4-G)作为吸附剂,建立了磁性分散微固相萃取-液相色谱-四极杆串联质谱(LC-MS/MS)测定畜禽肉样品中9种非甾体抗炎剂(NSAIDs)残留的方法.试样经酸化乙腈均质、冷冻离心除油、乙腈饱和正己烷脱脂后,采用磁性分散微固相萃取净化.对影响萃取效率的因素(萃取时间、样品溶液的pH值和洗脱条件)进行了优化.9种非甾体抗炎剂的检出限(LOD,S/N=3)为0.2～ 8.2 μg/kg,定量限(LOQ,S/N=10)为0.5～25.4 μg/kg.在添加水平分别为LOQ、2倍LOQ和10倍LOQ时,9种药物的加标回收率为83.3％～104.5％,相对标准偏差为1.2％～6.8％.与Sep-Pak Vac NH2和Oasis HLB固相萃取柱相比,磁性分散微固相萃取方法富集、分离效果好,负载量大,可重复利用,为畜禽肉中非甾体抗炎剂残的测定提供了一种新的前处理技术.

参考文献

[1]	Jedziniak, P.;Szprengier-Juszkiewicz, T.;Pietruk, K.;Ledziska, E.;Zmudzki, J..Determination of non-steroidal anti-inflammatory drugs and their metabolites in milk by liquid chromatography-tandem mass spectrometry[J].Analytical and bioanalytical chemistry,201210(10):2955-2963.
[2]	Hu, T.;Peng, T.;Li, X.-J.;Chen, D.-D.;Dai, H.-H.;Deng, X.-J.;Yue, Z.-F.;Wang, G.-M.;Shen, J.-Z.;Xia, X.;Ding, S.-Y.;Zhou, Y.-N.;Zhu, A.-L.;Jiang, H.-Y..Simultaneous determination of thirty non-steroidal anti-inflammatory drug residues in swine muscle by ultra-high-performance liquid chromatography with tandem mass spectrometry[J].Journal of chromatography, A: Including electrophoresis and other separation methods,2012:104-113.
[3]	Wang, W.;Ma, R.;Wu, Q.;Wang, C.;Wang, Z..Magnetic microsphere-confined graphene for the extraction of polycyclic aromatic hydrocarbons from environmental water samples coupled with high performance liquid chromatography-fluorescence analysis[J].Journal of chromatography, A: Including electrophoresis and other separation methods,2013:20-27.

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