用单壁羟基碳纳米管/壳聚糖内涂层分析柱毛细管电泳法测定药剂中的盐酸金刚烷胺含量  

Determination of Amantadine Hydrochloride in Drug Samples by Capillary Electrophoresis Using a Modified Column Coated with the Single-Walled Hydroxylation Carbon Nanotube/Chitosan Composite

作　　者：王荣 马永钧 Wang Rong;Ma Yongjun(College of Chemistry and Chemical Engineering,Northwest Normal University,Key Laboratory of Bioelectrochemistry and Environmental Analysis of Gansu Province,Lanzhou 730070,China)

机构地区：[1]西北师范大学化学化工学院,甘肃省生物电化学与环境分析重点实验室,甘肃兰州730070

出　　处：《山东化工》2020年第8期124-127,共4页Shandong Chemical Industry

摘　　要：本文用单壁羟基碳纳米管/壳聚糖内涂层修饰的毛细管为分离柱,以一种Mg2+-海藻糖-SiO32-三元缔合物凝胶(MTS-gel)作为分离添加剂,建立了一种柱前衍生电泳-电致化学发光联用法(CE-ECL)检测药剂中盐酸金刚烷胺含量的新方法。主要考察了柱前N-甲基化衍生盐酸金刚烷胺的关键反应条件、背景电解质中各添加剂的成分和浓度等因素的影响。在最优实验条件下,盐酸金刚烷胺衍生物和以固定浓度水平加入样品中内标肌氨酸衍生物的电泳峰间可在450 s内达到基线分离,且两个电泳峰的峰面积比值与盐酸金刚烷胺的初始浓度在10~250μmol/L和400~750μmol/L的范围内呈现出两段线性良好的定量关系曲线,其拟合方程分别为:AAH/ASar=-0.1509+0.0942CAH,R2=0.9995;AAH/ASar=-30.1729+0.1133 CAH,R2=0.9991,检出下限为2.4μmol/L(S/N=3)。同时,对几种市售感冒药剂中的盐酸金刚烷胺含量进行了测定,实样加标回收率介于90.2~102.9%之间,结果令人满意。In this article,with a modified quartz capillary coated with the single-walled hydroxylation carbon nanotube/chitosan composite as separation column and a ternary ionic association gel(Mg 2+-trehalose-SiO 2-3,MTS-gel)as a separation additive,we had established the quantitative assay method of amantadine hydrochloride by using pre-column derivatization capillary electrophoresis coupled with electrogenerated chemiluminescence detection(CE-ECL).In the experiments,the critical influencing factors that included the reaction conditions of amantadine hydrochloride in pre-column N-methylation derivatization process,both composition and concentration of several additives in the background electrolyte were investigated.Under the optimal experimental conditions,the derivative’s electrophoretic peaks from amantadine hydrochloride and the internal standard substance(sarcosine)to be added into the sample at a fixed concentration level could completely reach baseline separation within 450 s,and their peaks area ratio(AAH/ASar)showed a good linear relationship to the initial concentration value of amantadine hydrochloride in the two segment range of 10~250μmol/L(A AH/A Sar=-0.1509+0.0942 C AH,R 2=0.9995)and 400~750μmol/L(A AH/A Sar=-30.1729+0.1133 C AH,R 2=0.9991),respectively.The detection limit was also estimated to be 2.4μmol/L(S/N=3).In addition,the new analytical method could also be applied to the determination of amantadine hydrochloride content in several anti-cold medicaments.The recoveries for the real samples were between 90.2 and 102.9%,and the results were satisfactory.

关 键 词：毛细管电泳 电致化学发光 柱前衍生反应 盐酸金刚烷胺 

分 类 号：O657.3[理学—分析化学] TQ460.72[理学—化学]