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  

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

作　　者：董婵婵[1] 胡艳云[2,3] 吕亚宁[2,4] 宋伟[2,4] 韩芳[2,4] 郑平[2,4] 邓宁[1] 

机构地区：[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]安徽医科大学公共卫生学院,安徽合肥230032 [4]食品安全分析与检测安徽省重点实验室,安徽合肥230022

出　　处：《色谱》2016年第9期850-859,共10页Chinese Journal of Chromatography

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)~~

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 pg/kg,定量限（ LOQ, S/N=10） 为0.5-25.4 pg/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.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 （ p-SPE） coupled with liquid chro-matography-mass spectrometry detection. Samples were homogenized and extracted with acidi-fied acetonitrile. After defatting with the high speed frozen centrifugation, the sample solutions were defatted with n-hexane followed by p-SPE. Some important parameters influencing the extraction efficiency including the extraction time, the pH value of sample solution and the elu-tion 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 puri-fication 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.

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 

分 类 号：O658[理学—分析化学]