新型内表面反相限进填料的制备与评价  

Preparation and application of internal surface reversed-phase restricted-access material

作　　者：武晓玉[1] 王荣[1,2] 谢华[1] 王剑锋[1] 杨沛[2] 贾正平[1,2] 张强[1] 王先华[1] 

机构地区：[1]兰州军区兰州总医院全军高原损伤防治重点实验室,甘肃兰州730050 [2]兰州大学药学院,甘肃兰州730050

出　　处：《色谱》2012年第8期810-815,共6页Chinese Journal of Chromatography

基　　金：科技部重大项目(2008ZXJ09014-010)

摘　　要：通过在硅烷化硅胶内表面和外表面分别键合己胺和聚乙烯醇,制备了能够在线直接进样分析生物样品的新型内表面反相限进填料。采用元素分析、电镜观察对该限进填料的结构进行了表征。以普萘洛尔、阿替洛尔、苯巴比妥、卡马西平作溶质探针,并以Merck公司生产的限进填料柱作参比,对合成的限进填料的色谱性能进行了研究。研究结果表明,所制备的限进填料有较好的蛋白质排阻能力、富集能力和反相色谱性能,能同时实现排阻生物大分子杂质和富集小分子被分析物的功能,可作为在线、快速直接进样检测分析生物样品的预处理柱,适用于普萘洛尔血浆的直接进样分析。A new convenient synthetic method was developed for the preparation of restricted-access material belonging to the group of the internal surface reversed-phase supports,which can be used for the direct injection and analysis of complex biological samples such as plasma samples.The supports,owning the function of reversed-phase chromatography,have an alkyl-chain only to the internal surfaces of the porous silica.Polyvinyl alcoholic groups chemically bound to the external surfaces of the porous silica that has the ability of hydrophilicity.Its structure was characterized by elemental analysis and electron microscope observation.The reversed-phase chromatographic performance was evaluated by using different solute probes,including propranolol,atenolol,phenobarbital and carbamazepine.Meanwhile,the comparative study with Merck Company＇s ADS columns was carried out to prove capability of removing protein.At the same time,the plasma sample of propranolol was applied for the determination by direct injections.The results showed that the new internal surface reversed-phase restricted-access material owned the capabilities of protein exclusion and reversed-phase stationary,which could come true the double functions of excluding biomacromolecules and enriching micromolecule analysis.It can be used as a pretreatment column,which has the ability of on-line and fast analyzing biological specimen by direct probe inlet.

关 键 词：内表面反相限进填料 制备 评价 高效液相色谱法 普萘洛尔 血浆 

分 类 号：O658[理学—分析化学]