色谱 ›› 2017, Vol. 35 ›› Issue (2): 150-155.DOI: 10.3724/SP.J.1123.2016.07037

• 研究论文 • 上一篇    下一篇

新型反相限进材料及其性能

魏缠玲1, 赵丽娟1, 祁玉霞1, 李亚1, 李文婧1, 龚波林1,2   

  1. 1. 宁夏大学化学化工学院, 宁夏 银川 750021;
    2. 北方民族大学化学与化学工程学院, 宁夏 银川 750021
  • 收稿日期:2016-07-27 出版日期:2017-02-08 发布日期:2013-06-09
  • 通讯作者: 龚波林,Tel:(0951)2067867,E-mail:gongbolin@163.com
  • 基金资助:

    国家自然科学基金(21565001).

A novel reversed phase restrict access material and its properties

WEI Chanling1, ZHAO Lijuan1, QI Yuxia1, LI Ya1, LI Wenjing1, GONG Bolin1,2   

  1. 1. School of Chemistry & Chemical Engineering, Ningxia University, Yinchuan 750021, China;
    2. School of Chemistry & Chemical Engineering, Beifang University of Nationalities, Yinchuan 750021, China
  • Received:2016-07-27 Online:2017-02-08 Published:2013-06-09
  • Supported by:

    National Natural Science Foundation of China (No. 21565001).

摘要:

以溴代硅胶为引发剂,CuBr/2,2-联吡啶为催化体系,在改性硅胶上经二步表面引发原子转移自由基聚合(SI-ATRP)制备内表面接枝甲基丙烯酸十八烷基酯(C18)、外表面接枝甲基丙烯酸环氧丙酯(GMA)、水解得到表面含大量二醇基的新型反相限进材料。使用傅里叶变换红外光谱(FT-IR)、元素分析和热重分析(TGA)对其表征,采用静态吸附实验研究反相限进材料的吸附性能,其对磺胺二甲氧嘧啶和土霉素的最大吸附量分别为18.02和4.80 mg/g。结合固相萃取(SPE)评价其对大分子蛋白质的排阻性能,以牛血清白蛋白(BSA)作为排阻大分子模型,排阻能力达90%。将其用于牛奶中土霉素的分离富集,经高效液相色谱(HPLC)检测,土霉素的平均加标回收率为89.19%,相对标准偏差为3.03%。有望将新型反相限进材料和HPLC或液相色谱-质谱(LC-MS)等分析系统结合应用于生物样品的处理和检测。

关键词: 表面引发原子转移自由基聚合, 磺胺二甲氧嘧啶, 牛奶, 牛血清白蛋白, 土霉素, 限进材料

Abstract:

A novel reversed phase restrict access material was prepared via two steps of surface-initiated atom transfer radical polymerization (SI-ATRP). The stearyl methacrylate (C18) and glycidylmethacrylate (GMA) were grafted on inner and outer surfaces of modified silica, allowing brominated silica and CuBr/2,2-pyridine to serve as macro-initiator and catalyst system. After hydrolysis, we got a hydrophilic reversed phase restrict access material with rich glycol group, which was characterized by Fourier transform infrared (FT-IR) spectrum, elementary analysis and thermogravimetric (TGA) analysis. The static adsorption experiment was employed for evaluating the binding capacity of the novel reversed phase restrict access material. The maximum adsorption amounts of sulfadimethoxine and oxytetracycline were 18.02 and 4.80 mg/g, respectively. The properties of material for the exclusion of proteins like bovine serum albumin (BSA) were evaluated using solid-phase extraction (SPE) and its exclusion value up to 90%. The novel reversed phase restrict access material was used for the separation and enrichment of oxytetracycline in milk. The high-performance liquid chromatography (HPLC) was used to detect the oxytetracycline and the average recovery was 89.19% with the relative standard deviation (RSD) of 3.03%. It is expected that the novel inversed restrict access material combined with HPLC or liquid chromatography-mass (LC-MS) analysis system is applied to the extraction and detection of biological samples.

Key words: bovine serum albumin (BSA), milk, oxytetracycline (OTC), restrict access material, sulfadimethoxine (SDM), surface-initiated atom transfer radical polymerization (SI-ATRP)

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