School of Chemistry and Chemical Engineering, Henan University of Technology, Zhengzhou, P.R. China.
College of Chemistry and Molecular Engineering, Zhengzhou University, Zhengzhou, P.R. China.
J Sep Sci. 2017 Mar;40(6):1327-1333. doi: 10.1002/jssc.201601108. Epub 2017 Feb 9.
Novel molecularly imprinted polymers of phthalate esters were prepared by atom transfer radical polymerization using methyl methacrylate as functional monomer, cyclohexanone as solvent, cuprous chloride as catalyst, 1-chlorine-1-ethyl benzene as initiator and 2,2-bipyridyl as cross-linker in the mixture of methanol and water (1:1, v/v). The effect of reaction conditions such as monomer ratio and template on the adsorption properties was investigated. The optimum condition was obtained by an orthogonal experiment. The obtained polymers were characterized using scanning electron microscopy. The binding property was studied with both static and dynamic methods. Results showed that the polymers exhibited excellent recognition capacity and outstanding selectivity for ten phthalate esters. Factors affecting the extraction efficiency of the molecularly imprinted solid-phase extraction were systematically investigated. An analytical method based on the molecularly imprinted coupled with gas chromatography and flame ionization detection was successfully developed for the simultaneous determination of ten phthalate esters from edible oil. The method detection limits were 0.10-0.25 μg/mL, and the recoveries of spiked samples were 82.5-101.4% with relative standard deviations of 1.24-5.37% (n = 6).
新型邻苯二甲酸酯分子印迹聚合物是通过原子转移自由基聚合，以甲基丙烯酸甲酯为功能单体、环己酮为溶剂、氯化亚铜为催化剂、1-氯-1-乙苯为引发剂、2,2-联吡啶为交联剂，在甲醇和水（1:1，v/v）的混合物中制备的。考察了单体比和模板等反应条件对吸附性能的影响。通过正交实验得到了最佳条件。用扫描电子显微镜对得到的聚合物进行了表征。采用静态和动态方法研究了结合性能。结果表明，该聚合物对十种邻苯二甲酸酯具有优异的识别能力和选择性。系统研究了分子印迹固相萃取的萃取效率的影响因素。建立了一种基于分子印迹与气相色谱和火焰离子化检测相结合的分析方法，用于食用油中十种邻苯二甲酸酯的同时测定。该方法的检出限为 0.10-0.25μg/mL，加标样品的回收率为 82.5-101.4%，相对标准偏差为 1.24-5.37%（n=6）。
