摘要
目的采用顶空气相色谱法测定23价肺炎球菌多糖疫苗中乙醇、丙酮及乙醚的残留量。方法采用顶空气相色谱法,以水为溶剂,甲醇为内标,测定23价肺炎球菌多糖疫苗中乙醇、丙酮及乙醚的残留量,并对该方法进行系统适用性、线性关系、检测限与定量限、精密性、准确性验证及初步应用。结果该方法可使待测组分得到良好分离;测定乙醇、丙酮和乙醚的线性范围分别为:2.660～532.000μg/ml(r=1.000 0)、0.530～105.400μg/ml(r=0.999 8)和0.049～9.760μg/ml(r=0.998 9),检测限分别为0.80、0.16和0.01μg/ml,定量限分别为2.66、0.53和0.05μg/ml,精密性RSD值小于5.0%,平均回收率在95.0%～105.6%之间。该法检测3个批号23价肺炎球菌多糖疫苗中乙醇残留量,均未超过《中国药典》三部(2010版)规定的限度。3批疫苗中均未检出丙酮和乙醚。结论顶空气相色谱法操作简便,准确可靠,可用于23价肺炎球菌多糖疫苗中乙醇、丙酮及乙醚残留量的检测。
Objective To determine the residual ethanol,acetone and ether in 23-valent pneumococcal polysaccharide vaccine by headspace gas chromatography.Methods The residual ethanol,acetone and ether contents in 23-valent pneumococcal polysaccharide vaccine were determined by headspace gas chromatography（GC）,using water as dissolvent and methanol as internal standard,based on which the developed method was verified for system suitability,linear relationship,detection and quantitative detection limits,precision and accuracy,then applied preliminarily.Results The components to be tested were separated effectively by the developed method.The linear ranges of the method for determinations of ethanol,acetone and ether were 2.660 ～ 532.000（r = 1.000 0）,0.530 ～ 105.400（r = 0.999 8） and 0.049 ～ 9.760 μg / ml（r = 0.998 9）,while the detection limits were 0.80,0.16 and 0.01 μg / ml,and the quantitative detection limits were 2.66,0.53 and 0.05 μg / ml,respectively,with a RSD of less than 5.0% in precision test and mean recoveries of 95.0% ～ 105.6%.All the residual ethanol conteints in three batches of 23-valent pneumococcal polysaccharide vaccine determined by the method met the requirements in Chinese Pharmacopoeia（Volume Ⅲ,2010 edition）,while no acetone or ether was detected.Conclusion Headspace GC method was easy to handle,precise and reliable,which might be used for the determination of residual ethanol,acetone and ether in 23-valent pneumococcal polysaccharide vaccine.
出处
《中国生物制品学杂志》
CAS
CSCD
2011年第8期971-973,976,共4页
Chinese Journal of Biologicals
关键词
色谱法
气相
肺炎球菌疫苗
残留溶剂
Chromatography
gas
Pneumococcal vaccine
Residual solvents
作者简介
通讯作者：赵荣丽，E-mail：niceweather@163.com
