核磁共振氢谱分析法在肺炎球菌荚膜多糖疫苗质量控制中的应用  

Quality control of components of pneumococcal capsular polysaccharide vaccines by ~1H-NMR spectroscopic method

作　　者：王玺[1] 李阿妮[1] 张轶[1] 张新庄[1] 任克明[1] 王剑虹[1] 沈荣[1] 

机构地区：[1]兰州生物制品研究所有限责任公司甘肃省疫苗工程技术研究中心,兰州730046

出　　处：《中国新药杂志》2015年第23期2681-2686,共6页Chinese Journal of New Drugs

摘　　要：目的：将一维核磁共振氢谱（~1H-NMR）法分析应用于肺炎球菌荚膜多糖（Pn Ps）的质量控制。方法：用~1H-NMR法检测供试品Pn Ps,对部分特征信号进行归属,判断供试品化学结构是否与文献公布结果一致。对图谱异常的Pn Ps22F、23F的1H-NMR图谱进一步分析,辨认其水解特征信号。分析样品中是否有C-多糖（3.23ppm）、乙酸盐（1.92ppm）和Tris（3.73 ppm）等残留。结果：~1H-NMR分析结果显示Pn Ps14,6B,1,12F和33F结构与分析文献公布结果一致,样品中均含有少量的C多糖残留。图谱异常的Pn Ps22F和Pn Ps23F分别有部分脱氧乙酰基和部分脱磷酸甘油酯基团。3型中含有Tris残留。结论：1H-NMR检定方法快捷、所需样品量少、结果直观,可用于Pn Ps的质量控制。Objective： To apply the ~1H-NMR spectroscopic method in the quality control of pneumococcal capsular polysaccharide. Methods：~1H-NMR spectra were recorded using a standard pulse,and parts of characteristic signals were assigned. The results were compared with that published in literature. The abnormal samples PnPs22 F and PnPs23 F were further analyzed. The characteristic signal of hydrolyzed samples was identified. The residuals in Pn Ps were analyzed,including C-polysaccharide,acetate and Tris. Results： The ~1H-NMR spectra of PnPs14,6B,1,12 F and 33 F were identical to those in published literature,but only contained low level C-Polysaccharide contaminants. The PnPs22 F and 23 F showed partial O-deacetylated and dephosphorylate,respectively.PnPs3 contained low level Tris residual. Conclusions： The ~1H-NMR method is rapid and only needs a small amount of sample with more visualized result,so it can be used as a daily measurement for Pn Ps quality control.

关 键 词：肺炎球菌荚膜多糖 核磁共振 质控控制 

分 类 号：R979.5[医药卫生—药品]