李金峰;李颖;蒋原;薛峰;朱海;

• 1:深圳市易瑞生物技术有限公司
• 2:江苏出入境检验检疫局动植物与食品检测中心

摘要(Abstract)：

[目的]建立一种应用C18键合磁珠固相萃取-液质联用检测蜂王浆中磺胺二甲嘧啶残留的方法。[方法]MCX固相萃取小柱联合C18磁珠对蜂王浆进行前处理,用HPLC-串联质谱仪对净化后样本进行检测。[结果]该方法的线性范围是5～80μg/kg,相关系数0.993 1。添加水平为5、10、20μg/kg时各种化合物的平均回收率范围为93%～104%,RSD值均不大于11.3%。[结论]该方法简单、快速,结合自动化设备,可实现蜂王浆样品中磺胺二甲嘧啶测定前处理的自动化。

关键词(KeyWords)： 固相萃取;磁珠;磺胺二甲嘧啶;超高效液相色谱-串联质谱

Abstract:

Keywords:

基金项目(Foundation): 科技部科技型中小企业技术创新基金项目(09C26214425280);; 十二五国家科技支撑计划项目(2012BAK17B10);; 国家国际科技合作与交流专项项目(2011DFA32930)

作者(Author): 李金峰;李颖;蒋原;薛峰;朱海;

Email:

DOI: 10.13989/j.cnki.0517-6611.2012.27.156

参考文献(References)：

• [1]SONG Y,ZHAO S,TCHOUNWOU P,et al.A nanoparticle-based solid-phase extraction method for liquid chromatography-electrospray ionization-tandem mass spectrometric analysis[J].J Chromatogr A,2007,1166:79-84.
• [2]SHA Y,DENG C,LIU B.Development of C18-functionalized magnetic silicananoparticles as sample preparation technique for the determination of er-gosterol in cigarettes by microwave-assisted derivatization and gas chroma-tography/mass spectrometry[J].J Chromatogr A,2008,1198/1199:27-33.
• [3]NAGY M,OTREMBA P,KRUGER C,et al.Optimization and validation ofa fully automated silica-coated magnetic beads purification technology inforensics[J].Forensic Sci Int,2005,152:13-22.
• [4]LI Y,QI D,DENG C,YANG P,et al.Ceriumion-chelated magnetic silicamicrospheres for enrichment and direct determination of phosphopeptidesby matrix-assisted laser desorption ionization mass spectrometry[J].J Pro-teome Res,2008,7(4):1767-1777.
• [5]BALLESTEROS-GOMEZ A,RUBIO S.Hemimicelles of alkyl carboxylateschemisorbed onto magnetic nanoparticles:study and application to the ex-traction of carcinogenic polycyclic aromatic hydrocarbons in environmentalwater samples[J].Anal Chem,2009,81:9012-9020.
• [6]MORALES-CID G,FEKETE A,SIMONET B M,et al.In situ synthesis ofmagnetic multiwalled carbon nanotube composites for the clean-up of(fluo-ro)quinolones from human plasma prior to ultrahigh pressure liquid chro-matography analysis[J].Anal Chem,2010,82:2743-2752.