色谱 ›› 2018, Vol. 36 ›› Issue (7): 608-614.DOI: 10.3724/SP.J.1123.2018.01040

• 研究论文 • 上一篇    下一篇

磁性反相限进材料的制备及其应用

吴姗姗, 魏缠玲, 赵丽娟, 田央, 王富强, 龚波林   

  1. 北方民族大学化学与化学工程学院, 宁夏 银川 750021
  • 收稿日期:2018-01-28 出版日期:2018-07-08 发布日期:2014-06-03
  • 通讯作者: 龚波林,Tel:0951,2067917,E-mail:gongbolin@163.com
  • 基金资助:

    国家自然科学基金(21565001).

Preparation and application of magnetic reversed-phase restricted access material

WU Shanshan, WEI Chanling, ZHAO Lijuan, TIAN Yang, WANG Fuqiang, GONG Bolin   

  1. School of Chemistry and Chemical Engineering, North Minzu University, Yinchuan, 750021, China
  • Received:2018-01-28 Online:2018-07-08 Published:2014-06-03
  • Supported by:

    National Natural Science Foundation of China(No. 215605001).

摘要:

以磁性二氧化硅(Fe2O3@SiO2)为基质,利用表面原子转移自由基聚合技术(SI-ATRP),在改性后的Fe2O3@SiO2内表面接枝甲基丙烯酸十八烷基酯(SMA)、外表面接枝甲基丙烯酸缩甘油酯(GMA),酸解后得到磁性反相限进材料Fe2O3@SiO2-SMA-GMMA,并通过扫描电镜(SEM)、X射线衍射(XRD)、透射电镜(TEM)、振动样品磁强计(VSM)和元素分析对其进行表征。研究表明,Fe2O3@SiO2-SMA-GMMA对牛血清白蛋白(BSA)的排阻能力为90.4%;对磺胺异恶唑(SIZ)、磺胺二甲氧基嘧啶(SDM)、甲氧苄啶(TMP)和磺胺甲基嘧啶(SMR)的最大吸附量分别为2.76、2.24、1.51和1.34 mg/g。Fe2O3@SiO2-SMA-GMMA应用于牛奶和牛血清样品中SIZ、SMR和SDM的分离富集,SIZ、SMR和SDM的加标回收率为88.7%~90.8%,相对标准偏差为3.3%~5.3%。磁性反相限进材料可简化生物基质样品的前处理过程,对血液样品或食品样品等领域的分析检测具有重要价值。

关键词: 表面引发原子转移自由基聚合, 磁性反相限进材料, 固相萃取, 磺胺类药物, 制备

Abstract:

Using magnetic silica (Fe2O3@SiO2) as the matrix material, a magnetic reversed-phase restricted access material was prepared via surface-initiation atom transfer radical polymerization (SI-ATRP) on the surface of modified Fe2O3@SiO2. Stearyl methacrylate (SMA) was grafted on the inner surface of the modified Fe2O3@SiO2, and glycidylmethacrylate (GMA) was grafted on the outer surface of the modified Fe2O3@SiO2. The magnetic reversed-phase restricted access material was prepared via acid hydrolysis. This material was characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), vibrating sample magnetometer (VSM) and elemental analysis. The exclusion ability of the opened magnetic reversed-phase restricted access material to bovine serum albumin (BSA) was 90.4%. The maximum adsorbed amounts of sulfisoxazole (SIZ), sulfadimethoxine (SDM), trimethoprim (TMP) and sulfamerazine (SMR) were 2.76, 2.24, 1.51 and 1.34 mg/g, respectively. This material was applied to extract and enrich SIZ, SMR and SDM in milk and bovine serum samples. The spiked recoveries of SIZ, SMR and SDM were 88.7%-90.8%, and the relative standard deviations were 3.3%-5.3%. Thus, the magnetic phase restricted access material can simplify the pretreatment of biological matrix samples, and can be applied to the analysis and detection of blood samples or food samples.

Key words: magnetic reversed-phase restricted access material, preparation, solid phase extraction(SPE), sulfonamides(SAs), surface-initiated atom transfer radical polymerization(SI-ATRP)

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