新型反相限进材料及其性能  

A novel reversed phase restrict access material and its properties

作　　者：魏缠玲 赵丽娟[1] 祁玉霞[1] 李亚[1] 李文婧[1] 龚波林[1,2] 

机构地区：[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

出　　处：《色谱》2017年第2期150-155,共6页Chinese Journal of Chromatography

基　　金：国家自然科学基金(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(SIATRP)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4.80mg/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。A novel reversed phase restrict access material was prepared via two steps of sur-face-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 sys-tem. Af^er hydrolysis,we got a hydrophilic reversed phase restrict access material with rich gly-col 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 exclu-sion value up to 90%. The novel reversed phase restrict access material was used for the separa-tion 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.

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

分 类 号：O658[理学—分析化学]