气相色谱法同时检测A群脑膜炎球菌多糖疫苗中的残留乙醇和丙酮

目的 建立可同时检测A群脑膜炎球菌多糖疫苗等生物制品中的残留乙醇和丙酮的毛细管气相色谱法.方法 通过实验选择DB-FFAP型色谱柱为分离柱,气相色谱条件设置为:进样口温度200℃、检测器温度250 ℃、柱温60℃、进样体积1 μl、分流比10:1、载气(氮气)流速2.0 ml/min.在已确定的色谱条件下,对乙醇和丙酮进行定位及最低检出限和线性范围测定,重复性和准确性实验及样品测定同时进行.结果 在本色谱条件下,乙醇和丙酮得到完全分离,最低检出限分别为0.196和0.102mg/L,每种溶剂的线性关系均良好,相关系数均为0.9997.此法的重复性良好,乙醇和丙酮的平均加样回收率分别为102.8%和102.9%.结论 此法适合同时检测A群脑膜炎球菌多糖疫苗中的残留乙醇和丙酮.

Gas chromatography for simultaneous determination of residual ethanol and acetone in group A meningococcal polysaccharide vaccine

Objective To establish a capillary gas chromatography method for simultaneous determination of the residual ethanol and acetone in biologicals, such as group A meningoeeceal polysaccharide vaccine. Methods The DB-FFAP-type column was selected as a separation column by test. The temperatures of injection port, detector and column were set at 200, 250 and 60 ℃, respectively. The injection volume was 1 μl and the split ratio was 10: 1. The flow rate of carrier gas (nitrogen) was kept at 2.0 ml/min. In the definitive chromatographic conditions, ethanol and acetone were located, and the minimum detection limits and the linear ranges of ethanol and acetone were determined. The tests of repeatability, accuracy and sample were carried out. Results In the definitive chromatographic conditions, ethanol and acetone were separated completely, the minimum detection limits of ethanol and acetone were O. 196 and 0. 102 rag/L, respectively. There was a good linearity in each solvents ( r = 0. 9997). The method had a good repeatability, and the average recovery rates of ethanol and acetone were 102.8% and 102.9%, respectively. Conclusion The method is suitable for simultaneous determination of the residual ethanol and acetone in group A meningococcal polysaceharide vaccine.