实用医技杂志2024,Vol.31Issue(4) :241-244.DOI:10.19522/j.cnki.1671-5098.2024.04.004

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

段盼盼 赵丽娟 吴姿 杨子妮 王燕清
实用医技杂志2024,Vol.31Issue(4) :241-244.DOI:10.19522/j.cnki.1671-5098.2024.04.004

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

段盼盼 1赵丽娟 1吴姿 1杨子妮 1王燕清1
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作者信息

  • 1. 珠海市丽珠微球科技有限公司分析部,珠海 519000
  • 折叠

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,0.5 μm),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、1.079 μg/ml;质量浓度分别在1.174~234.80、1.166~233.28、1.079~215.76 μg/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.

Abstract

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,0.5 μm).Both of the inlet temperature and the FID detector temperature were controlled at 250 ℃.Programmed temperature was adopted.The flow rate of earried 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 1.174,1.166,1.079 μg/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 1.079~215.76 μg/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

Key words

Chromatography,gas/Ethylene glycol/Suspending agent/Diethylene glycol/Trithylene glycol

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出版年

2024
实用医技杂志
山西医药卫生传媒集团有限责任公司

实用医技杂志

影响因子:0.534
ISSN:1671-5098
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