摘要
目的建立A群C群脑膜炎球菌多糖疫苗和b型流感嗜血杆菌结合疫苗中丙酮残留量的检测方法并加以验证。方法参照《中华人民共和国药典》三部（2010年版）中＂毛细管柱顶空进样等温法＂,优化色谱条件,建立A群C群脑膜炎球菌多糖疫苗和b型流感嗜血杆菌结合疫苗中丙酮残留量的检测方法并对该方法进行验证及初步应用。结果色谱条件为顶空平衡温度70℃,顶空平衡时间40 min,汽化室温度200℃,柱箱温度40℃,检测器温度250℃,进样量为1.0 m L,载气（高纯氮气）流量1.3 m L/min,尾吹气（高纯氮气）流量5 m L/min,分流比1∶1。丙酮质量分数在2×10^-6-5×10^-5范围内具有良好的线性关系（r〉0.99）。丙酮的平均回收率及相对标准偏差（RSD）分别为86.05%-105.11%及2.1%-9.5%,检测限为2×10^-6,定量限为3×10^-6。结论本方法的线性、特异性、准确性、重复性等均符合规定,方法准确、稳定,可用于A群C群脑膜炎球菌多糖疫苗和b型流感嗜血杆菌结合疫苗中丙酮残留量的检测。
Objective To establish and validate a method in determination of the residual acetone in the group A and C Meningococcal polysaccharide vaccine and Haemophilus influenza type b conjugate vaccine. Methods According to the guideline of capillary column head-space isothermal method published in《Pharmacopoeia of The People＇s Republic of China》Volume Ⅲ 2010 edition,by which the determination for residual acetone was validated and preliminary applied,in addition to optimized the related parameters in chromatography,in the group A and C Meningococcal polysaccharide vaccine and Haemophilus influenza type b conjugate vaccine. Results Head-space gas chromatography with the hydrogen flame detector and HP-5 capillary column（ 5% Phenyl Methyl-Siloxane,30 m × 0. 32 mm × 0. 25 μm） was applied in determination of the residual content of acetone. After optimazation of parameters of chromatography,a good liner correlation was obtained over the range of 2 × 10^-6- 5 × 10^-5,r≥0. 99. The average recovery of the residual content of acetone was 86. 05% - 105. 11% and the average CV value was 2. 1% - 9. 5%. The detection limit was 2 × 10^-6. The quantification limit was 3 × 10^-6. Conclusion The validation results indicated that the indexes of the method met the requirements including linearity,selectivity,accuracy,repeatability,and sensitivity,which was reliable and accuracy in the quality control of the residual acetone in group A and C Meningococcal polysaccharide vaccine and Haemophilus influenza type b conjugate vaccine.
出处
《微生物学免疫学进展》
2016年第2期28-34,共7页
Progress In Microbiology and Immunology
关键词
A群C群脑膜炎球菌多糖疫苗
B型流感嗜血杆菌结合疫苗
顶空气相色谱法
残留丙酮
Group A and C meningococcal polysaccharide vac cine
Haemophilus influenza type b conjugate vaccine
Head space gas chromatography
Residual acetone
