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目的:建立同时测定甘草酸二铵原料中5种溶剂(甲醇、乙醇、乙腈、乙酸和N,N-二甲基甲酰胺(DMF))残留量的方法。方法:采用气相色谱法。以DB-624毛细管为色谱柱,氮气为载气,氢火焰离子化检测器,检测器温度240℃,进样口温度200℃,程序升温;以二甲基亚砜为溶剂,采用直接进样方式,测定10批原料药中5种溶剂的残留量。结果:甲醇、乙醇、乙腈、乙酸、DMF检测浓度线性范围分别为7·5～150、12·5～250、1·0～20·5、1·25～25·0、0·21～4·38μg·mL-1(r为0·9992～1·0000);平均回收率(n=9)均在98·0%以上,RSD<8%;10批样品中溶剂残留量均在合格范围内。结论:建立的方法简便、重复性好,能较好地控制甘草酸二铵原料药的质量。
Objective: To establish a method for the simultaneous determination of five solvents (methanol, ethanol, acetonitrile, acetic acid and N, N-dimethylformamide (DMF)) in the raw materials of diammonium glycyrrhizinate. Methods: Gas chromatography. Using DB-624 capillary as the column, nitrogen as the carrier gas, hydrogen flame ionization detector, detector temperature 240 ℃, inlet temperature 200 ℃, the program temperature; dimethyl sulfoxide as solvent, using direct injection Method, the determination of 10 batches of drug residues in the five kinds of solvents. Results: The linear range of the concentration of methanol, ethanol, acetonitrile, acetic acid and DMF was from 7.5 to 150, from 12.5 to 250, from 1.0 to 20.5, from 1.25 to 25.0, from 0.21 to 4 · The average recoveries (n = 9) were above 98.0% and the RSD was less than 8%. The residual solvents of 10 batches of samples were within the acceptable range Inside. Conclusion: The established method is simple and reproducible, and can control the quality of diammonium glycyrrhizinate.