本文制备了磺胺甲恶唑分子印迹聚合物,通过静态吸附实验及红外光谱等手段研究其性能,并以该聚合物为核心材料自制液体样品快速前处理装置,建立且优化出一种水溶液中微量磺胺甲恶唑的简单、经济的现场批量前处理方法.通过加标回收实验验证了该方法的可行性,并进行了实际样品的现场前处理与测定.结果表明,所制备的印迹聚合物(MIP)具有良好的亲和性和特异选择性;在0.50—1000.00μg·L-1范围内,所建立方法的水样加标回收率为72.0%—100.3%,相对标准偏差为2.2%—5.1%(n=6),方法的检测限为0.01μg·L-1.本实验所采集的5种实际样品(红湖水样、水上乐园水样、鱼塘水样、牛尿和猪尿)中均检出磺胺甲恶唑,其浓度分别为0.76、1.23、1.94、202.0、435.3μg·L-1.
Molecularly imprinted polymers for sulfamethoxazole were prepared as a critical material to establish a rapid in-situ pretreatment method for measuring trace sulfamethoxazole in water.Properties of the molecularly imprinted polymers for sulfamethoxazole were studied by means of the infrared spectroscopy and static adsorption experiment. A simple and economic pretreatment device was assembled in this experiment. The feasibility of the method was verified by combining it with high performance liquid chromatography( HPLC) in the spiked recovery experiment. Real samples were collected and treated with this method,and results showed that molecularly imprinted polymer( MIP) had good affinity and specific selectivity. As the concentration of sulfamethoxazole in water ranged from 0. 50 μg·L- 1to 1000. 00 μg·L- 1,the spiked recoveries of sulfamethoxazole ranged from 72. 0% to 100. 3%,relative standard deviation ranged from 2. 2% to 5. 1%( n = 6),the detection limit of this method was 0. 01μg·L- 1. Three surface water samples and two urine samples were collected and pretreated in-situ with the method and then analyzed with HPLC in the lab. Resultsindicated that sulfamethoxazole concentrations in surface water samples,aquaculture water and urine solution were 0. 76,1. 23,1. 94,202. 0,435. 3 μg·L- 1,respectively. The method could be used for rapid in-situ pretreatment of field samples,which could be employed for automatic monitoring.