Dong Xiangchao, Wang Ning, Wang Shengli, Zhang Xuewei, Fan Zhijin
Department of Chemistry, Nankai University, Tianjin 300071, China.
J Chromatogr A. 2004 Nov 19;1057(1-2):13-9. doi: 10.1016/j.chroma.2004.09.036.
A novel sample clean-up procedure using molecularly imprinted polymer as the solid-phase extraction material for the determination of monosulfuron residue in soil samples has been developed. The molecularly imprinted polymer (MIP) was synthesized by non-covalent method with monosulfuron as the template. The selectivity and affinity of the MIP was evaluated by equilibrium adsorption and HPLC experiments, which demonstrated that the MIP has specific affinity for the template. The template-MIP interaction was studied by investigating the influence of different mobile phases on the retention of the template, which provided basic knowledge for the selection of the washing and elution solutions in the molecularly imprinted solid-phase extraction (MISPE) process. The study indicated that polar organic solvents with hydrogen bonding abilities have stronger eluting strength for the monosulfuron. After the MISPE procedure, a clean baseline was obtained in the HPLC quantification analysis. The recoveries of the method using the combination of MISPE and HPLC were above 93% and the R.S.D. was less than 3.2% in the soil sample determinations. Low detection limit (0.08 microg g(-1), when defined as 3 times of the noise) was also obtained in the method evaluation study.
已开发出一种新型的样品净化程序,该程序使用分子印迹聚合物作为固相萃取材料来测定土壤样品中的单嘧磺隆残留量。以单嘧磺隆为模板,通过非共价法合成了分子印迹聚合物(MIP)。通过平衡吸附和高效液相色谱(HPLC)实验评估了MIP的选择性和亲和力,结果表明MIP对模板具有特异性亲和力。通过研究不同流动相对模板保留的影响,研究了模板与MIP之间的相互作用,这为分子印迹固相萃取(MISPE)过程中洗涤和洗脱溶液的选择提供了基础知识。研究表明,具有氢键能力的极性有机溶剂对单嘧磺隆具有更强的洗脱强度。经过MISPE程序后,在HPLC定量分析中获得了干净的基线。在土壤样品测定中,使用MISPE和HPLC相结合的方法回收率高于93%,相对标准偏差(R.S.D.)小于3.2%。在方法评估研究中还获得了低检测限(当定义为噪声的3倍时为0.08μg g-1)。