^1HNMR快速定量测定咔啦咪星B硅烷化反应的硅烷化程度  

Rapid Determination of Silylating Degree in Synthesis of Silylated Kanamycin B by 1H Nuclear Magnetic Resonance

作　　者：马学兵[1] 王宁[1] 周光明[1] 

机构地区：[1]西南师范大学化学化工学院,重庆400715

出　　处：《分析化学》2004年第10期1345-1348,共4页Chinese Journal of Analytical Chemistry

基　　金：重庆市科委应用基础研究项目资助课题 (No .2 0 0 3 8117)

摘　　要：当作为内标的N ,N 二甲基甲酰胺醛基氢的积分面积与已知浓度的HMDS氢的积分面积相近时 ,定量分析HMDS的相对误差为 0 .35 %。在咔啦咪星B的硅烷化反应中应用1HNMR技术快速测定HMDS和HMDSO的百分含量 ,其RSD分别为 2 .4 2 %和 5 .31%。硅烷化反应 10 .5h时 ,咔啦咪星B引入 9个Si(CH3 ) 3 基团 ;反应 14h时 ,咔啦咪星B已完全硅烷化。1HNMR技术是一种快速而准确地跟踪咔啦咪星B硅烷化反应的手段。There is a good accuracy with relative error 0.35 % for quantitative determination of (CH_3)_3SiNHSi(CH_3)_3 (HMDS) with known concentration by 1H nuclear magnetic resonance (NMR) technique if the intergration area of aldehydic hydrogen used as internal standard material is approximate to that of HMDS. The application of 1H NMR technique in the synthesis of silylated kanamycin B for rapid determination of the content of HMDS and (CH_3)_3SiOSi(CH_3)_3 (HMDSO) has excellent precision with RSD 2.42 % and 5.31 % for HMDS and HMDSO, respectively. Nine silyl groups Si(CH_3)_3 were introduced into kanamycin B after the silylating reaction carried out for 10.5 h, and kanamycin B could be completely silylated for 14 h. 1H NMR is a very good and rapid technique to monitor the silylation degree of kanamycin B and hydrolytic decomposition of HMDS.

关 键 词：咔啦咪星B 硅烷化反应 核磁共振氢谱 硅烷化程度 快速测定 抗菌素 

分 类 号：O657.2[理学—分析化学]