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以双酚A(BPA)为模板分子,乙腈(ACN)为致孔剂,α-甲基丙烯酸为功能单体(MAA),乙二醇二甲基丙烯酸酯(EDMA)为交联剂,偶氮二异丁腈(AIBN)为引发剂,快速制备了双酚A分子印迹聚合物(MIP)萃取头。聚合反应在内径为530μm的毛细管中进行,微波聚合7 min。得到的双酚A分子印迹聚合物从毛细管中推出,在安培瓶中洗脱后再次插入毛细管中用于固相微萃取(SPME)。在不同的模板分子和功能单体的比例(BPA/MAA)、NaCl浓度、萃取和解吸时间、pH值和解吸溶剂条件下考察了聚合物的萃取性能。选取结构类似物苯酚(P)、对羟基联苯(PP)和非结构类似物二聚氰胺(DCD),对MIP和非印迹聚合物(NIP)的选择性吸附性能进行了对比。所建立的SPME方法结合高效液相色谱法(HPLC)成功用于饮料中双酚A的检测。在优化的实验条件下,双酚A的线性范围为10~400μg/L,检出限(LOD)为0.45μg/L,在矿泉水中的回收率为88.4%~102.8%。结果表明所建立的方法能够用于检测实际样品中的BPA,具有样品预处理简便、分析快速、检出限低和消耗低的优点。
Using BPA as template, acetonitrile (ACN) as pore former, MAA as functional monomer and ethylene glycol dimethacrylate as crosslinking agent, AIBN was used as initiator to prepare bisphenol A molecularly imprinted polymer (MIP) heads. The polymerization was carried out in a capillary tube with an inner diameter of 530 μm and polymerized in microwave for 7 min. The resulting bisphenol A molecularly imprinted polymer is pushed out of the capillary, eluted in an ampule and reinserted into a capillary tube for solid phase microextraction (SPME). The extraction performance of the polymers was investigated under different template / functional monomer ratios (BPA / MAA), NaCl concentration, extraction and desorption time, pH value and desorption solvent. The structural analogues of phenol (P), p-hydroxybiphenyl (PP) and non-structural analogue melamine (DCD) were selected for selective adsorption of MIP and non-imprinted polymer (NIP). The established SPME method combined with high performance liquid chromatography (HPLC) was successfully used in the detection of bisphenol A in beverages. Under the optimized experimental conditions, the linear range of bisphenol A was 10-400μg / L, the limit of detection (LOD) was 0.45μg / L, and the recovery of mineral water was 88.4% -102.8%. The results show that the proposed method can be used to detect BPA in real samples with the advantages of simple sample pretreatment, fast analysis, low detection limit and low consumption.