直接进样气相色谱法用于助悬剂中乙二醇二甘醇和三甘醇残留量测定方法研究  

Direct injection gas chromatography for the determination of ethylene glycol,diethylene glycol and triethylene glycol in suspending solution

作　　者：段盼盼 赵丽娟 吴姿 杨子妮 王燕清 Duan Panpan;Zhao Lijuan;Wu Zi;Yang Zini;Wang Yanqing(Department of Analysis,Zhuhai Livzon Microsphere Technology Co.Ltd.,Zhuhai519000,China)

机构地区：[1]珠海市丽珠微球科技有限公司分析部,珠海519000

出　　处：《实用医技杂志》2024年第4期241-244,共4页Journal of Practical Medical Techniques

摘　　要：目的建立同时测定微球注射剂用助悬剂中乙二醇、二甘醇、三甘醇残留量的气相色谱方法。方法采用直接进样气相色谱法,HP-INNOWAX毛细管柱(30 m×0.32 mm,0.5μm),氢火焰离子化检测器(FID),进样口温度250℃,检测器温度250℃,柱温箱程序升温,载气为N2,流速1.0 ml/min,分流比1∶1。结果3种成分完全分离;乙二醇、二甘醇、三甘醇的定量限浓度分别为1.174、1.166、1.079μg/ml;质量浓度分别在1.174~234.80、1.166~233.28、1.079~215.76μg/ml内与峰面积呈良好的线性关系(r>0.999);平均回收率(n=6)分别为96.2%、96.3%、101.6%,相对标准偏差分别为3.1%、3.1%、5.2%;4批样品中均未检出乙二醇、二甘醇、三甘醇。结论本方法可用于测定助悬剂中乙二醇、二甘醇、三甘醇含量。Objective To establish a GC method for the determination of ethylene glycol,diethylene glycol and trithylene glycol in suspending solution used for microspheres for injection.Methods The gas chromatography analyses were performed on a HP-INNOWAX capillary column(30 m×0.32 mm,0.5μm).Both of the inlet temperature and the FID detector temperature were controlled at 250℃.Programmed temperature was adopted.The flow rate of carried gas(N2)was 1.0 ml/min.The split ratio was 1∶1.Results The 3 components were completely separated.The limits of quantitative were 1.174,1.166,1.079μg/ml,respectively.Glycol,diethylene glycol and trithylene glycol showed a good linear relationship within the range of 1.174~234.80、1.166~233.28 and 1.079~215.76μg/ml(r>0.999).The average recovery was 96.2%(RSD=3.1%),96.3%(RSD=3.1%),101.6%(RSD=5.2%)(n=6),respectively.No residue of these solvents was detected in 4 batches of suspending solution.Conclusion This method can be applied to determine the ethylene glycol,diethylene glycol and trithylene glycol in suspending solution.

关 键 词：色谱法 气相 乙二醇 助悬剂 二甘醇 三甘醇 

分 类 号：R927.2[医药卫生—药学] O657.71[理学—分析化学]