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目的:建立顶空气相色谱法测定安立生坦原料中甲醇、乙醇、叔丁基甲基醚、乙酸乙酯、二氧六环、N,N-二甲基甲酰胺等残留量的方法。方法:采用HP-5(30 m×0.53 mm,1.5μm)石英毛细管柱,载气为高纯氮气,FID检测器,采用程序升温和顶空进样,柱温35℃保持5 min,再以20℃·min~(-1)升温至110℃,保持5 min。结果:6种残留溶剂的分离度符合要求,线性关系良好(r≥0.999 0)。回收率均在99.3%~105.2%范围内,3批安立生坦样品检测结果均符合限度要求。结论:该方法检测灵敏、准确,可用于检测安立生坦原料药的残留溶剂。
OBJECTIVE: To establish a method for the determination of residues of methanol, ethanol, tert-butyl methyl ether, ethyl acetate, dioxane, N, N-dimethylformamide in the raw materials of andrographolide by headspace gas chromatography. Methods: HP-5 (30 m × 0.53 mm, 1.5 μm) quartz capillary column was used. The carrier gas was high purity nitrogen and FID detector. The sample was heated at 35 ℃ for 5 min. 20 ℃ · min ~ (-1) temperature was raised to 110 ℃ for 5 min. Results: The resolution of the six residual solvents was satisfactory and the linear relationship was good (r ≥ 0.9999). The recoveries ranged from 99.3% to 105.2%. The test results of three batches of Andextran samples all met the limit requirements. Conclusion: The method is sensitive and accurate. It can be used for the determination of residual solvents in Anritsuantang APIs.