论文部分内容阅读
目的：对《中国药典》2010版甘油中二甘醇、乙二醇杂质检查方法进行优化。方法：甘油经甲醇提取,气相色谱法(GC-FID)定量检测。选用DM-624毛细管柱(30 m ×0.53 mm,3μm)分离,初始柱温80℃,保持6 min,50℃·min-1升至100℃,保持8 min,10℃·min-1升至220℃,保持10 min；分流进样,分流比100∶1；进样口温度250℃；检测器温度280℃；流速6.0 ml·min-1。结果：方法精密度(RSD)小于5%,各色谱峰分离度符合《中国药典》要求,采用该方法对市售甘油进行分析,杂质量均小于规定的限量。结论：改进后的方法简便、稳定、可靠,可用于甘油的杂质检查。“,”Objective:To establish an improved method for the determination of diethylene glycol and ethylene glycol in glycerol on the basis of the method in Chinese pharmacopoeia (2010 edition). Methods: Glycerol samples were extracted by methanol, and detected by gas chromatography with a flame ionization detector. The column was a DM-624 capillary column(30 m × 0. 53 mm,3μm), and the initial temperature was 80℃ in the first 6min and then risen to 100℃ at the speed of 50℃·min-1, kept for 8min,fi-nally risen to 220℃ at the speed of 10℃·min-1 , kept for 10min. The split injection was used with the split ratio of 100∶1. The in-jection temperature was 250℃ and the detector temperature was 280℃. The flow rate was 6. 0ml·min-1 . Results:The RSD(%) of the method was lower than 5%, and the resolution of all chromatographic peaks met the requirements of the pharmacopoeia. The meth-od was used to analyze the commercial product of glycerol, and the contents of diethylene glycol and ethylene glycol were both less than the specified limits. Conclusion:The method is simple and rapid, and suitable for glycerol impurity inspection.