论文部分内容阅读
目的:建立检测苄星青霉素原料药中5种残留溶剂(甲醇、乙醇、乙酸乙酯、正丁醇、乙酸丁酯)的方法。方法:以二甲基亚砜为溶剂,采用顶空气相色谱法,色谱柱为DB-624;程序升温;载气为氮气,流速为4.5mL·min-1;进样口温度为200℃;氢离子火焰检测器温度为250℃;顶空瓶平衡温度为80℃,平衡时间为30min。结果:5种残留溶剂峰分别与相邻峰分离完全,在各自的浓度范围内与峰面积呈良好的线性关系(r为0.9990～0.9993),加样回收率为97.9%～103.1%,RSD为1.1%～2.4%(n=9),最低检测限为0.5～1.2μg·mL-1。结论:该方法简便、准确、灵敏,可用于苄星青霉素原料药中残留溶剂的检测。
Objective: To establish a method for the determination of five residual solvents (methanol, ethanol, ethyl acetate, n-butanol and butyl acetate) in the raw material of benzathine penicillin. Methods: The solvent was dimethylsulfoxide (DMSO), and the column was DB-624 by headspace gas chromatography. The temperature of the system was increased. The carrier gas was nitrogen and the flow rate was 4.5mL · min-1. The inlet temperature was 200 ℃. The temperature of the hydrogen ion flame detector is 250 ° C .; the equilibrium temperature of the headspace bottle is 80 ° C and the equilibration time is 30 min. Results: The five residual solvent peaks were completely separated from the adjacent peaks, respectively, and showed a good linear relationship with the peak area in each concentration range (r ranged from 0.9990 to 0.9993). The average recoveries were 97.9% -103.1% with RSD 1.1% ~ 2.4% (n = 9), the lowest detection limit was 0.5 ~ 1.2μg · mL-1. Conclusion: The method is simple, accurate and sensitive and can be used for the determination of residual solvents in benzathine penicillin.