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

发布时间：2017-12-27 13:28

  本文关键词：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　出处：《色谱》2016年09期 　论文类型：期刊论文

  更多相关文章： 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

【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0.2~8.2μg/kg,定量限(LOQ,S/N=10)为0.5~25.4μg/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。
[Abstract]:Using magnetic graphene nanocomposites (Fe3O4-G) as adsorbent, a method for the determination of 9 nonsteroidal anti-inflammatory drugs (NSAIDs) residues in livestock and poultry meat samples by magnetic dispersive micro solid phase extraction liquid chromatography quadrupole tandem mass spectrometry (LC-MS/MS) was established. After acidified acetonitrile homogenization, frozen centrifugation and degreasing, acetonitrile saturated n-hexane was defatted, magnetic dispersive micro solid extraction was used to purify the sample. The factors affecting the extraction efficiency (extraction time, pH value of the sample solution and elution conditions) were optimized. The detection limit of the 9 NSAIDs (LOD, S/N=3) is 0.2~8.2 mu g/kg, and the quantitative limit (LOQ, S/N=10) is 0.5~25.4 u g/kg. When the addition level was LOQ, 2 times LOQ and 10 times LOQ, the recovery rate of the 9 drugs was 83.3%~104.5%, and the relative standard deviation was 1.2%~6.8%. Compared with Sep-Pak Vac NH2 and Oasis HLB solid phase extraction column, magnetic dispersive micro solid phase extraction method has the advantages of good concentration and separation effect, large loading capacity, and can be reused. It provides a new pre-processing technology for the determination of NSAIDs residues in livestock and poultry meat.
【作者单位】： 合肥工业大学化学与化工学院;安徽出入境检验检疫局;安徽医科大学公共卫生学院;食品安全分析与检测安徽省重点实验室;
【基金】：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)~~
【分类号】：O657.63;TS251.7
【正文快照】： *通讯联系人.Tel:(0551)62856373,E-mail:huyanyun@ahciq.gov.cn.Foundation item:Provincial Natural Science Foundation of Anhui,China(No.1408085MKL97);State Quality InspectionAdministration Science and Technology Projects(No.2014IK134);Shanghai Yangtze River ，

本文编号：1341904