对羟基苯甲酸印迹聚合物微粒的制备及其固相萃取应用  

Preparation of p-Hydroxybenzoic Acid-Imprinted Polymer Particulates and Application to Solid Phase Extraction

作　　者：张铁莉[1] 柴国平[1] 赫彩霞[1,2] 王磊[1] 

机构地区：[1]唐山师范学院化学系,河北唐山063000 [2]河北科技大学生物科学与工程学院,石家庄050018

出　　处：《应用化学》2016年第2期229-237,共9页Chinese Journal of Applied Chemistry

基　　金：唐山师范学院团队支撑重点项目(2014D07)资助~~

摘　　要：以对羟基苯甲酸（p-HBA）为模板分子,丙烯酰胺（AM）为功能单体,乙二醇二甲基丙烯酸酯为交联剂,采用沉淀聚合法在乙腈溶剂中制备了p-HBA印迹聚合物微粒,研究了p-HBA加入量及聚合反应体系的总浓度对印迹聚合物结合性能的影响,采用色谱法对其进行了评价。结果表明,p-HBA的加入量及反应体系的总浓度对结合性能均有影响,当p-HBA加入量为1.0 mmol（与AM物质的量比为1∶2）时,在37.5 m L乙腈中制得印迹聚合物P2对p-HBA具有高的亲和力（k＇=4.01）和选择性。将印迹聚合物P2作为固相萃取填料,研究了分子印迹固相萃取p-HBA的方法,测得2种不同载样模式下p-HBA的柱容量分别为6.91μg/100 mg和1.93μg/100 mg,测得天麻样品中p-HBA的加标回收率为76.8%-86.6%（RSD=3.4%-6.2%）（n=3）。结果表明,采用沉淀聚合法以AM为功能单体制备的p-HBA印迹聚合物微粒适宜作为固相萃取填料,可实现天麻样品中p-HBA的选择性分离净化。p-Hydroxybenzoic acid（ p-HBA）-imprinted polymer particulates were prepared using p-HBA as the template,acrylamide（ AM） as the functional monomer and ethylene glycol dimethacrylate as the crosslinker in three different amounts of p-HBA and under two different concentrations of pre-polymerization mixtures via precipitation polymerization. Their rebinding performances for p-HBA were characterized by high-performance liquid chromatography. The results reveal that both the amounts of p-HBA and the concentrations of prepolymerization mixtures exhibit notable influence on the binding performances of p-HBA-imprinted polymers.The p-HBA-imprinted polymer（ P2） with high affinity（ k＇ = 4. 01） and selectivity for p-HBA is obtained when the amount of p-HBA is 1. 0 mmol,which is corresponding to the molar ratio of 1 ∶ 2（ p-HBA / AM）,in37. 5 m L of acetonitrile solvent. In addition,the imprinted polymer P2 was chosen as the adsorbent to make the molecularly imprinted solid phase extraction（ MISPE） column and the MISPE method for the extraction of p-HBA was developed. The MISPE column capacities for p-HBA are 6. 91 μg /100 mg and 1. 93 μg /100 mg,respectively,which are determined under two different modes of loading samples. The rhizoma gastrodiae samples spiked with three different amounts of p-HBA are extracted and the recoveries of p-HBA range from76. 8% to 86. 6%,with the RSD of 3. 4% - 6. 2%（ n = 3）. The results demonstrate that the p-HBAimprinted polymer particulates prepared using AM as the functional monomer by precipitation polymerization are suitable as the adsorbent of solid phase extraction column for the selective separation and purification of pHBA in the real sample of rhizoma gastrodiae.

关 键 词：对羟基苯甲酸 沉淀聚合 分子识别 分子印迹固相萃取 

分 类 号：O652.6[理学—分析化学]