本文關(guān)鍵詞：磁性石墨烯分散微固相萃取-液相色譜-四極桿串聯(lián)質(zhì)譜法測定畜禽肉中9種非甾體抗炎劑　出處：《色譜》2016年09期 　論文類型：期刊論文

  更多相關(guān)文章： 磁性分散微固相萃取 液相色譜-四極桿串聯(lián)質(zhì)譜 磁性石墨烯納米復(fù)合材料 非甾體類抗炎劑 畜禽肉

【摘要】：以磁性石墨烯納米復(fù)合材料(Fe3O4-G)作為吸附劑,建立了磁性分散微固相萃取-液相色譜-四極桿串聯(lián)質(zhì)譜(LC-MS/MS)測定畜禽肉樣品中9種非甾體抗炎劑(NSAIDs)殘留的方法。試樣經(jīng)酸化乙腈均質(zhì)、冷凍離心除油、乙腈飽和正己烷脫脂后,采用磁性分散微固相萃取凈化。對影響萃取效率的因素(萃取時間、樣品溶液的pH值和洗脫條件)進行了優(yōu)化。9種非甾體抗炎劑的檢出限(LOD,S/N=3)為0.2~8.2μg/kg,定量限(LOQ,S/N=10)為0.5~25.4μg/kg。在添加水平分別為LOQ、2倍LOQ和10倍LOQ時,9種藥物的加標回收率為83.3%~104.5%,相對標準偏差為1.2%~6.8%。與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、分離效果好,負載量大,可重復(fù)利用,為畜禽肉中非甾體抗炎劑殘的測定提供了一種新的前處理技術(shù)。
[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.
【作者單位】： 合肥工業(yè)大學(xué)化學(xué)與化工學(xué)院;安徽出入境檢驗檢疫局;安徽醫(yī)科大學(xué)公共衛(wèi)生學(xué)院;食品安全分析與檢測安徽省重點實驗室;
【基金】：安徽省自然科學(xué)基金項目(1408085MKL97) 國家質(zhì)檢總局科技計劃項目(2014IK134) 上海長三角科技合作項目(15395810100) 安徽省科技計劃項目(1604b0602028)~~
【分類號】：O657.63;TS251.7
【正文快照】： *通訊聯(lián)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 ，

本文編號：1341904