表面印迹聚合物萃取/气相色谱质谱联用检测双酚A  被引量:9

Determination of bisphenol A by gas chromatography-mass spectrometry with molecularly imprinted solid phase extraction

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作  者:朱军峰[1] 王卓妮[2] 李元博[1] 张光华[1] 

机构地区:[1]陕西科技大学化学与化工学院,教育部轻化工助剂化学与技术重点实验室,西安710021 [2]中国石油天然气股份有限公司兰州化工研究中心,兰州730060

出  处:《分析试验室》2014年第1期59-63,共5页Chinese Journal of Analysis Laboratory

基  金:陕西省教育厅专项科研计划项目(11JK0562);陕西科技大学博士科研启动项目(BJ13-04)资助

摘  要:以双酚A(BPA)为模板分子,甲基丙烯酸为单体,乙二醇二甲基丙烯酸酯作为交联剂,在硅胶表面合成双酚A分子印迹聚合物。通过红外光谱、比表面积测定等对表面印迹聚合物进行分析和表征;采用静态吸附法和动态吸附法对其吸附性能进行考察。红外光谱表明硅胶表面生成了对模板分子具有识别功能的官能团;热重分析证明该印迹聚合物具有良好的热稳定性;静态吸附实验说明表面印迹聚合物比非印迹聚合物具有良好的吸附性能,该印迹聚合物对双酚A最大吸附容量Q max为1.501 mg/g,吸附速率常数k为0.01586g/(mg·min)。用表面印迹聚合物萃取(MISPE)和气相色谱质谱(GC-MS)联用检测了BPA样品,BPA的回收率接近90%,并将该双酚A表面印迹聚合物用于牛奶样品中的BPA测试,结果表明该印迹聚合物具有较好的吸附选择性。Bisphenol A molecularly imprinted polymers (BPA-MIPs on silica) were synthesized on the silica gelwith bisphenol A as the template molecule, methacrylic acid( as crossing-linkers. The MIPs were characterized using FTIR tion property of the MIPs was tested by static and dynamic MAA) and ethylene glycol dimethacrylate(EDMA) specrometry and specific surface area. The adsorp- adsorption experiments. FTIR spectrum shows the functional group with recognition has generated on the surface of silica gel. The MIPs had good thermostability. The adSorption experiments show the maximum adsorption amount (Qmax) is 1.501 mg/g and the adsorption rate constant is 0. 01586 g/( mg · min). A new rapid and effective sample pretreatment technique, molecularly im- printed solid-phase extraction (MISPE) was achieved by combination of molecular imprinted technology and sol- id-phase extraction (SPE). The recovery and elution effect of BPA were examined by MISPE and gas chromatog- raphy-mass spectrometry (GC-MS). The experimental result shows that the recovery of BPA is nearly 90%. The MIPs were used to test BPA in milk samples, and it had good adsorption selectivity.

关 键 词:双酚A 分子印迹技术 固相萃取 气质联用 

分 类 号:O657.63[理学—分析化学]

 

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