甘油中二甘醇、乙二醇杂质检查方法的改进

目的：对《中国药典》20l0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（30m×0．53mm，3μm）分离，初始柱温80℃，保持6rain，50℃·min^-1升至100％，保持8min，10℃·min“升至220％，保持10mi“；分流进样，分流比100：1；进样口温度250％；检测器温度280℃；流速6.0ml·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。

Improvement in Determination of Diethylene Glycol and Ethylene Glycol in Glycerol

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℃·rain-1 , kept for 8min,finally 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.