邻-硝基酚分子印迹聚合物为涂层固相萃取搅拌棒的制备及其萃取性能研究

Preparation of Stir Bar Sorptive Extraction Based on o-Nitrophenol Imprinted Polymer and Its Extraction Performance

以邻-硝基酚为模板,甲基丙烯酸二甲胺乙酯和4-乙烯基吡啶为混合单体,利用整体材料"原位"聚合技术制备分子印迹聚合物为涂层的固相萃取搅拌棒(MIP-SBSE)。考察了制备条件对MIP-SBSE选择吸附性能的影响,并与高效液相色谱-二极管阵列检测器联用,探讨MIP-SBSE对环境水样中邻-硝基酚及其它酚类物质的选择萃取性能。考察了样品基底中离子强度、pH值以及吸附时间和解吸时间等萃取条件对目标化合物选择性能影响。结果表明,在最佳萃取条件下,MIP-SBSE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,对邻-硝基酚的线性范围为3.0～200μg/L;检出限LOD(S/N=3)为0.13μg/L;定量限LOQ(S/N=10)为0.40μg/L。在实际样品分析中,模板分子加标回收率为83.4%～120.9%;其它酚类物质的加标回收率在59.8%～129.0%之间。

A new stir bar sorptive extraction（SBSE） based on molecularly imprinted polymer（MIP） with o-nitrophenol as template molecule was prepared.The effect of preparation conditions on the extraction performance of MIP-SBSE was studied.Then,a methodology combined SBSE and liquid desorption,followed by high performance liquid chromatography with diode array detection for the direct determination of trace o-nitrophenol（o-NP） and phenolsin in real samples was developed.To achieve the optimum extraction performance,several main parameters including pH value and ionic strength in the sample matrix,extraction and desorption time were investigated.Under the optimized experimental conditions,the method showed good linearity between 3.0 and 200 μg/L for o-NP.The detection limit（S/N=3） and quantification limit（S/N=10） of the proposed method for o-NP was 0.13 and 0.40 μg/L,respectively.The spiked recoveries for o-NP in real samples ranged from 83.4%-120.9% and 59.8%-129.0% for other phenols.