Liu Junwei, Wang Yong, Li Weixia, Zhang Peimin, Wang Nani, Wu Shuchao, Zhu Yan
Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou 310028, China.
Institute of Forensic Science and Technology of Nanjing Public Security Bureau, Nanjing 210001, China.
Talanta. 2016 Nov 1;160:298-305. doi: 10.1016/j.talanta.2016.07.021. Epub 2016 Jul 8.
Poly (glycidylmethacrylate-divinylbenzene) (Poly (GMA-DVB)) microspheres were prepared by the two-staged swelling and polymerization method, and modified with octadecylamine (ODA) to obtain ODA-poly (GMA-DVB) stationary phase for HPLC. The new material was characterized by scanning electron microscope, nitrogen adsorption-desorption measurement, Fourier transform infrared spectrum, elemental analysis and thermogravimetric analysis. The results showed that poly (GMA-DVB) microspheres had good monodispersity, porosity and ball shapes. The diameters and specific surface area of the microspheres were about 6µm and 396m(2)g(-1), respectively. ODA-poly (GMA-DVB) stationary phase had good thermal stability. Furthermore, the chromatographic performance of the stationary phase was illustrated by separating n-alkylbenzenes, mono-substituted benzenes and N-nitrosamines. Auxiliary quantum chemistry calculation was also carried out to evaluate the interaction mechanism. According to the evaluation, ODA-poly (GMA-DVB) stationary phase exhibited good hydrophobicity and hydrophobic selectivity, strong stereo-selectivity, polar interaction and π-π interaction. The multi-interaction mechanisms could very likely guarantee its excellent chromatographic performance for the analysis of complex samples. Finally, the column was successfully applied in the determination of N-nitrosamines in pickles sample.
采用两步溶胀聚合法制备了聚(甲基丙烯酸缩水甘油酯 - 二乙烯基苯)(聚(GMA - DVB))微球,并用十八烷基胺(ODA)对其进行改性,以获得用于高效液相色谱的ODA - 聚(GMA - DVB)固定相。通过扫描电子显微镜、氮吸附 - 脱附测定、傅里叶变换红外光谱、元素分析和热重分析对新材料进行了表征。结果表明,聚(GMA - DVB)微球具有良好的单分散性、孔隙率和球形。微球的直径和比表面积分别约为6μm和396m²g⁻¹。ODA - 聚(GMA - DVB)固定相具有良好的热稳定性。此外,通过分离正烷基苯、单取代苯和N - 亚硝胺来说明固定相的色谱性能。还进行了辅助量子化学计算以评估相互作用机理。根据评估,ODA - 聚(GMA - DVB)固定相表现出良好的疏水性和疏水选择性、强立体选择性、极性相互作用和π - π相互作用。多种相互作用机理很可能保证其在分析复杂样品时具有出色的色谱性能。最后,该色谱柱成功应用于泡菜样品中N - 亚硝胺的测定。