顶空气相色谱法测定生脉注射液中乙醇残留量

摘要

OBJECTIVE: To establish the method for determination of alcohol residue in shengmai injection by headspace gas chromatography .METHODS:The alcohol residue in shengmai injection was separated by HP-5 column (30 m ×0.32 mm,0.25 μm);the carrier gas was nitrogen , the flow rate was 1 ml/min.The splitting ratio was 1:1. The temperature of detector and injector was 250 ℃ and 200 ℃, respectively .The temperature of column was maintained at 50 ℃ for 6 min.The containers of headspace injector were in equilibrium at 80 ℃ for 10 min.The injector volume was 1 ml.RESULTS: Under chromatographic condition , the theoretical plate number of ethanol ≥160000, and the separation degree of ethanol peak and adjacent peak ≥3.0.The alcohol concentration was good in the range of 0.001％-0.020％, with limit of detection of 0.00006％( V/V ) .CONCLUSIONS: The established method is simple , sensitive and accurate with good reproducibility , which can be used to determine the alcohol residue in shengmai injection .%目的:建立顶空气相色谱法测定生脉注射液中乙醇残留量的方法.方法:色谱柱为HP-5柱(30 m×0.32 mm,0.25μm);载气为氮气,流速为1 ml/min;分流比1:1;检测器温度250℃;进样口温度200℃;恒温50℃保持6 min.顶空进样,平衡温度80℃,平衡时间10 min,进样量1 ml.结果:色谱条件下,乙醇的理论塔板数≥160000,乙醇峰与相邻峰的分离度≥3.0.乙醇浓度在0.001％～0.020％范围内线性关系良好,检测限为0.00006％(V/V).结论:本方法快速、灵敏且准确,重复性好,适用于生脉注射液中乙醇残留量的检测.