GC法测定某中药复方制剂中甘油的含量

Content Determination of Glycerin in Compound Preparation of Traditional Chinese Medicine by GC

目的:建立某中药复方制剂中甘油的含量测定方法。方法:采用气相色谱法进行测定。色谱柱为KB-Awax石英毛细管柱(30m×0.32mm×0.50μm),进样口温度为250℃,柱温为程序升温,初始温度为165℃;氢火焰离子化检测器(FID),检测器温度为300℃;载气为N2,流速为1.0mL·min-1;分流比为5∶1;进样体积为1μL;以萘为内标物,以无水乙醇为溶剂。结果:甘油与内标物在14min内分离良好;甘油的进样浓度在1.1036～11.0360mg·L-1范围内同其与内标峰面积比值呈良好线性关系(r=0.9999);低、中、高3个浓度的平均回收率分别为100.6%(RSD=1.0%)、98.8%(RSD=1.5%)、99.7%(RSD=1.4%)。结论:本方法简便、准确、重复性好,可用于某中药复方制剂中甘油的含量测定。

OBJECTIVE： To establish a method for the content determination of glycerin in compound preparation of traditional Chinese medicine （TCM）. METHODS： GC method was adopted. The determination was performed on KB-Awax capillary column （30 m×0.32 mm×0.50 μm）. The injection temperature was 250 ℃ and the column temperature was raised by programming with initial temperature at 165 ℃. FID detector was adopted using nitrogen as carrier gas and the detector temperature was 300 ℃. The flow rate was 1.0 mL·min-1 and the split ratio were 5 ∶ 1. The injection volume was 1 μL with naphthalene as internal standard and alcohol as solvent. RERULTS： The glycerin and internal standard were separated perfectly within 14 min. The linear range of glycerin was 1.103 6～11.036 0 mg·L-1（r=0.999 9）. The average recoveries of low, middle and high concentrations of glycerin were 100.6%（RSD=1.0%）,98.8%（RSD=1.5%） and 99.7%（RSD=1.4%）. CONCLUSION： The method is simple, accurate and reproducible for the content determination of glycerin in compound preparation of TCM.