Özer Elif Tümay, Osman Bilgen, Yazıcı Tuğçe
Department of Chemistry, Faculty of Arts and Science, Uludag University, 16059 Bursa, Turkey.
Department of Chemistry, Faculty of Arts and Science, Uludag University, 16059 Bursa, Turkey.
J Chromatogr A. 2017 Jun 2;1500:53-60. doi: 10.1016/j.chroma.2017.04.013. Epub 2017 Apr 9.
The aim of this study was to investigate the usability of newly synthesized dummy molecularly imprinted microbeads (DMIMs) as a solid phase extraction (SPE) material to determine six phthalate esters (PEs) in water by GC-MS analysis. Diethyl phthalate (DEP) was used as a dummy template to prepare poly(ethylene glycol dimethacrylate N-methacryloyl-l-tryptophan methyl ester) [PEMATrp)] DMIMs by using suspension polymerization. The PEMATrp DMIMs were characterized by using Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Firstly, the adsorption capacities of the DMIMs prepared in different template molecule (DEP) to functional monomer (MATrp) ratios were investigated by using DEP solutions in the concentration range of 1-500mg/L at pH 3.0. Styrene and vanillic acid were used to evaluate the selectivity of the prepared DMIMs towards the template molecule (DEP). Then, the best analytical conditions were investigated for the simultaneous determination of dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), benzylbutyl phthalate (BBP), di-(2-ethylhexyl) phthalate (DEHP) and di-n-octyl phthalate (DnOP) in aqueous media by using the PEMATrp DMIMs as SPE material. Validation experiments showed that the PEMATrp DMIMs-SPE method had good linearity at 12.5-250.0μg/L (0.988-0.999), good precision (1.2-5.9%), and limits of detection in a range of 0.31-0.41μg/L.
本研究的目的是研究新合成的虚拟分子印迹微珠(DMIMs)作为固相萃取(SPE)材料,通过气相色谱-质谱(GC-MS)分析测定水中六种邻苯二甲酸酯(PEs)的适用性。以邻苯二甲酸二乙酯(DEP)为虚拟模板,采用悬浮聚合法制备聚(乙二醇二甲基丙烯酸酯-N-甲基丙烯酰基-L-色氨酸甲酯)[PEMATrp] DMIMs。通过傅里叶变换红外光谱(FTIR)、X射线光电子能谱(XPS)和扫描电子显微镜(SEM)对PEMATrp DMIMs进行了表征。首先,在pH 3.0条件下,使用浓度范围为1-500mg/L的DEP溶液,研究了不同模板分子(DEP)与功能单体(MATrp)比例制备的DMIMs的吸附容量。用苯乙烯和香草酸评估制备的DMIMs对模板分子(DEP)的选择性。然后,研究了以PEMATrp DMIMs为SPE材料同时测定水介质中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二正丁酯(DBP)、邻苯二甲酸苄基丁酯(BBP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)和邻苯二甲酸二正辛酯(DnOP)的最佳分析条件。验证实验表明,PEMATrp DMIMs-SPE方法在12.5-250.0μg/L范围内具有良好的线性(0.988-0.999)、良好的精密度(1.2-5.9%),检测限在0.31-0.41μg/L范围内。