基于分子印迹材料的雌酮快速检测方法研究

Rapid determination estrone method on the basis of molecular imprinted polymer

以合成的雌酮分子印迹聚合物为微柱填料,建立了分子印迹聚合物富集雌酮原位显色反应的方法,并对影响测定结果的显色剂用量、填料量、上样流速和上样时间等主要实验参数进行了优化,在印迹材料填料量为0.030g,上样流速为1.0mL·min-1,1.00μg·L-1雌酮-甲醇标准溶液富集10.0mL条件下,再加入稀氢氧化钾-乙醇溶液1.0mL条件下,显色剂15.00g·L-1间二硝基苯溶液1.0mL,在暗处反应1h,最低检出限可达10.00μg·L-1。为了验证所建立的方法的实用性,本研究对湖水样品中的痕量雌酮残留进行了检测分析。通过对检测为空白的样品进行浓度为10.00,50.00,100.00μg·L-1的添加,以所建立的分析方法进行检测,结果均有比较明显的颜色反应,从而说明所建立的检测方法的可行性。

A method to detect trace estrone in environment was developed with a novel molecularly imprinted polymer as enrichment sorbent for situ enrichment of estrone by color reaction. The parameters affecting the procedure including the color reagent,the weight of MIPs,loading flow rate and time were optimized.With a loading flow rate of 1.0mL·min-1 for sampling 10.0mL of 1.00μg·L-1 estrone-methanol solution,then add in watery KOHethanol solution 1.0mL and color reagent 1.0mL of m-Dinitrobenzene 15.00g·L-1 reacted 1h in dark.The detection limit was 10.00μg·L-1.To evaluate the usefulness of the novel imprinted sorbent,the samples of lake water from Tianjin University of Science Technology,determined to be free of estrone,were spiked with three levels of estrone（ 10.00,50.00 and 100.00μg · L-1 ） and analyzed after simple pretreatment under optimal experimental conditions.At each concentration,evident change of color in lake water,respectively.It is proved that the detection of estrone in environment is feasible in this method.