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二氧化锆包覆的二氧化硅核壳型填料的制备及在选择性吸附磷脂中的应用研究

ISSN号：1000-8713
期刊名称：分析化学
时间：2013.9
页码：1214-1219
分类：TQ633[化学工程—精细化工]
作者机构：[1]上海交通大学药学院,上海200240
相关基金：国家自然科学基金项目（Nos.21105064 21175092）; 国家重大科学仪器设备开发专项（Nos.2011YQ150072 2011YQ15007204 2011YQ15007207 2011YQ15007210）; 上海市自然基金科学（No.12ZR1413600）资助
相关项目：基于金属氧化物核壳型材料的血清样品中磷脂代谢物轮廓分析

关键词：磷脂, 二氧化锆, 核壳, 固相萃取, 高效液相色谱, Phospholipids, Zirconium dioxide, Core-shell, Solid phase extraction, High performance liquid chromatography

中文摘要：

提出了一种基于ZrO2/SiO2核壳型材料吸附磷脂的分析方法。首先利用NH3/H2O内部水解法制备了含不同比例ZrO2包覆的ZrO2/SiO2核壳型颗粒,并通过电镜和紫外吸收漫反射图谱对其进行了表征,证明在SiO2表面包覆有ZrO2材料。采用RP-HPLC-ELSD（Reversed phase-high performance liquid chromatogra-phy-evaporative light scattering detector）,以甲醇-水（含醋酸铵）为流动相,优化并建立了5种磷脂的分析方法。在以上基础上将ZrO2/SiO2核壳型材料制成固相萃取（Solid phase extraction,SPE）小柱,以5种磷脂标准品为研究对象,用RPLC-ELSD方法评价了SPE小柱吸附磷脂的效率。发现包覆有3.5%和7%ZrO2的ZrO2/SiO2核壳型材料吸附磷脂的能力均强于单纯的ZrO2材料,且3.5%的ZrO2/SiO2核壳型材料吸附效果最好,并将其初步应用于血清中磷脂的选择性吸附,结果表明,通过SPE富集后,能检测到更多的磷脂类代谢产物。

英文摘要：

A strategy for selectively enrich phospholipids（PLs） using zirconia coated silica（ZrO2/SiO2） core-shell microspheres was developed.ZrO2/SiO2 was first prepared by NH3/H2O vapor-induced internal hydrolysis method,and characterized by SEM and UV-VIS.The results showed zirconia layer was coated on the surface of silica indeed.A method of reversed phase-high performance liquid chromatography-evaporative light scattering detector（RP-HPLC-ELSD） for the analysis of phospholipid standards was also established.A good separation of five standards was achieved by using methanol-water（including ammonium acetate） as mobile phase.Based on these methods,the absorption ability of ZrO2/SiO2 microspheres packed into the solid phase extraction（SPE） towards PLs was investigated.The results demonstrated ZrO2/SiO2 SPE column had a much higher selectivity and higher recoveries than those of bulk ZrO2 particles.In addition,the best recovery rate of PLs was obtained from 3.5% ZrO2/SiO2 materials.At last,the ZrO2/SiO2 microsphere was also applied to enrich endogenous phospholipids form human serum,and more metabolites were found by using ZrO2/SiO2 SPE column.