双酚A分子印迹聚合物为萃取介质搅拌饼固相萃取的制备及其萃取性能研究

以双酚A为模板,4-乙烯基吡啶为单体,利用整体材料"原位"聚合技术制备分子印迹聚合物为基质的萃取饼,并与利用一次性注射器空管加工而成的萃取器相结合,建立了分子印迹搅拌饼固相萃取(MIP-SCSE)技术。考察了制备条件对MIP-SCSE选择吸附性能的影响。在此基础上,与高效液相色谱-二极管阵列检测器联用,探讨MIP-SCSE对环境水样中双酚A及其它酚类物质的选择萃取性能,考察萃取过程中基底离子强度、pH值以及吸附与解吸时间等萃取条件对萃取性能的影响。结果表明;在最佳萃取条件下,MIP-SCSE对模板分子及其它酚类物质具有一定选择性能和较高的富集能力,对双酚A的线性范围为1.0～200μg/L;检出限LOD(S/N=3)为0.67μg/L;定量限LOQ(S/N=10)为2.24μg/L。在实际水样分析中,模板分子加标回收率为86.2%～112.2%。在MIP-SCSE使用过程中,萃取饼不与容器壁接触,因此具有优良的使用寿命,至少可连续使用600 h。

Preparation of Stir Cake Sorptive Extraction Based on Bisphenol A Imprinted Polymer and Its Extraction Performance

A new stir cake sorptive extraction(SCSE) based on molecularly imprinted polymer(MIP) with bisphenol A(BPA) as template was prepared.The effect of preparation conditions on the extraction performance of MIP-SCSE was studied.Then,a methodology combined the stir cake sorptive extraction and liquid desorption,followed by high performance liquid chromatography with diode array detection for the direct analysis of traces of bisphenol A(BPA) in water was developed.To achieve the optimum extraction performance,several main parameters,including pH value and contents of inorganic salt in the sample matrix,extraction and desorption time,were investigated.Under the optimized experimental conditions,the method showed good linearity between 1-200 μg/L for BPA.The detection limit(S/N=3) and quantification limit(S/N=10) of the proposed method for BPA was 0.67 and 2.24 μg/L,respectively.The recoveries of spiked target compound in real samples ranged from 86.2%-112.2%.The MIP-SCSE shows excellent longevity and can be used more than 600 h.