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以己烯雌酚为替代模板,利用整体材料的“原位”合成技术制备了分子印迹聚合物,并将其作为固相萃取搅拌棒的涂层(MIP-SBSE)制备了新的搅拌棒。详细考察了分子印迹聚合物制备条件中模板分子及功能单体用量对MIP-SBSE选择性萃取性能的影响,同时利用元素分析、扫描电镜和红外光谱对聚合物进行表征。以双烯雌酚(DS)和己烷雌酚(HS)为目标化合物,将MIP-SBSE与高效液相色谱-二极管阵列检测器联用,建立起复杂样品中DS和HS的分离分析方法。考察了吸附和解吸时间、解吸溶剂、离子强度和样品pH值等萃取条件对MIP-SBSE选择性萃取性能的影响。结果表明,在最佳萃取条件下,MIP-SBSE对DS和HS具有较高的选择性萃取性能,线性范围分别为1.0～400.0μg/L和5.0～400.0μg/L,利用氮吹再定容的方法,对DS和HS的检出限(S/N=3)分别可低至0.04和0.14μg/L。在对实际污水、蜂蜜和牛尿样品的分析中取得了良好的加标回收率,其值为61.3%～120%。所建方法具有简便、高选择性和灵敏等特点,可用于复杂样品中双烯雌酚和己烷雌酚的分析监测。
Using diethylstilbestrol as a template, the molecularly imprinted polymer was prepared by “in-situ” synthesis of monoliths and was used as a solid phase extraction stirrer coating (MIP-SBSE) to prepare a new stirrer. The influences of the amount of template molecule and functional monomer on the performance of MIP-SBSE selective extraction were investigated in detail, and the polymer was characterized by elemental analysis, scanning electron microscopy and infrared spectroscopy. DDS and HS were selected as the target compounds. MIP-SBSE was coupled with high performance liquid chromatography-diode array detector to establish a method for the separation and analysis of DS and HS in complex samples. The effects of extraction and desorption time, desorption solvent, ionic strength and sample pH on extraction performance of MIP-SBSE were investigated. The results showed that MIP-SBSE had a higher selectivity for DS and HS under the optimal extraction conditions. The linear range was 1.0-400.0μg / L and 5.0-400.0μg / L, respectively. The detection limits (S / N = 3) for DS and HS were as low as 0.04 and 0.14 μg / L, respectively. Good spiked recoveries of 61.3% to 120% have been obtained in the analysis of actual sewage, honey and cow urine samples. The proposed method has the characteristics of simplicity, high selectivity and sensitivity. It can be used for the analysis and monitoring of Dienoessol and Hexestrol in complex samples.