摘要
目的:建立毛细管气相色谱法测定穿心莲内酯原料乙醇溶剂残留量。方法:采用气相色谱法测定,N,N-二甲基甲酰胺为溶剂,正丙醇为内标。色谱柱为DB-624石英毛细管色谱柱(30mm×0.53mm,3.0μm),载气为氮气。检测器温度:250℃;进样口温度:150℃;程序升温:初始温度70℃,保持6min,以90℃/min升温至200℃,保持5min。结果:被测物在52.3~523.4μg/ml范围内呈良好线性关系,回收率为100.2%,精密度、重复性良好。结论:方法快速,准确可靠,可用于穿心莲内酯原料中乙醇残留的检测。
OBJECTIVE To establish a method of capillary gas chromatography (CGC) for the determination of residual solvents (ethanol) in andrographolide. METHODS The method was developed by DB -624 capillary column (30 m × 0.53 mm,3.0 μm) with FID detector. The carried gas was nitrogen. The injector temperature and the detector temperature were controlled at 150 ℃ and 250 ℃, respectively. The programmed column temperature was set as follows : maintained at 70℃ for 6 min and then raised to 200 ℃ at the rate of 90 ℃/min followed by holding for 5 min. the sample was dissolved in N, N - dimethylformamide and n - propanol was used as the internal standard. RESULTS The calibration curve showed a good linear relationship at the range of 52.3 - 523.4 μg,/ml with good precision and accuracy. CONCLUSION The method is accurate and reliable. It can be used for the determination of residual solvents (ethanol) in andrographolide.
出处
《天津药学》
2008年第4期23-25,共3页
Tianjin Pharmacy
关键词
穿心莲内酯
毛细管气相色谱
有机溶剂
残留量
andrographolide, capillary gas chromatography, organic solvents, contents of residual