色谱 ›› 2016, Vol. 34 ›› Issue (9): 850-859.DOI: 10.3724/SP.J.1123.2016.04039

• 研究论文 • 上一篇    下一篇

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2,4, 吕亚宁2,3, 宋伟2,3, 韩芳2,3, 郑平2,3, 邓宁1   

  1. 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;
    3. 食品安全分析与检测安徽省重点实验室, 安徽 合肥 230022;
    4. 安徽医科大学公共卫生学院, 安徽 合肥 230032
  • 收稿日期:2016-04-27 出版日期:2016-09-08 发布日期:2016-08-26
  • 通讯作者: 胡艳云
  • 基金资助:

    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);上海长三角科技合作项目(15395810100);安徽省科技计划项目(1604b0602028).

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

DONG Chanchan1, HU Yanyun2,4, LÜ Yaning2,3, SONG Wei2,3, HAN Fang2,3, ZHENG Ping2,3, DENG Ning1   

  1. 1. School of Chemistry and Chemical Technology, Hefei University of Technology, Hefei 230009, China;
    2. Anhui Entry-Exit Inspection and Quarantine Bureau, Hefei 230022, China;
    3. Anhui Province Key Laboratory of Analysis and Detection for Food Safety, Hefei 230022, China;
    4. School of Public Health, Anhui Medical University, Hefei 230032, China
  • Received:2016-04-27 Online:2016-09-08 Published:2016-08-26
  • Supported by:

    Provincial Natural Science Foundation of Anhui, China (No. 1408085MKL97); State Quality Inspection Administration Science and Technology Projects (No. 2014IK134); Shanghai Yangtze River Science and Technology Cooperation Projects (No. 15395810100); Anhui Science and Technology Program (No. 1604b0602028).

摘要:

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。

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

Abstract:

A novel analytical method was developed for the determination of nine non-steroidal anti-inflammatory drugs (NSAIDs) in meat samples by magnetic graphene nanocomposite (Fe3O4-G) based on dispersive micro-solid-phase extraction (μ-SPE) coupled with liquid chromatography-mass spectrometry detection. Samples were homogenized and extracted with acidified acetonitrile. After defatting with the high speed frozen centrifugation, the sample solutions were defatted with n-hexane followed by μ-SPE. Some important parameters influencing the extraction efficiency including the extraction time, the pH value of sample solution and the elution conditions were optimized. The limits of detection (LODs, S/N=3) of the nine NSAIDs ranged from 0.2 to 8.2 μg/kg, and the limits of quantification (LOQs, S/N=10) ranged from 0.5 to 25.4 μg/kg. The average recoveries were 83.3%-104.5% with the relative standard deviations between 1.2% and 6.8% obtained from samples spiked at LOQ, 2LOQ and 10LOQ levels. Compared with Sep-Pak Vac NH2 and Oasis HLB cartridges, Fe3O4-G has excellent purification effect, high loading amounts and good reusability. The results demonstrated that the method provide a novel pretreatment technique for the determination of NSAID residues in meat samples.

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

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