| 王彩媚,王淼.结冷胶中残留溶剂测定方法的优化探讨[J].中国药品标准,2023,24(1): |
| 结冷胶中残留溶剂测定方法的优化探讨 |
| Discussion on the optimization of the determination method of residual solvent in gellan gum |
| 投稿时间：2022-06-07 修订日期：2023-02-01 |
| DOI： |
| 中文关键词: 顶空气相色谱法 结冷胶 乙醇 异丙醇 |
| 英文关键词: headspace gas chromatography gellan Gum ethanol isopropyl alcohol |
| 基金项目:国家药品标准提高研究课题（编号：2019Y029） |
|
| 摘要点击次数: 252 |
| 全文下载次数: 18 |
| 中文摘要: |
| 目的：建立顶空气相色谱法同时测定结冷胶中的残留溶剂异丙醇和乙醇。方法：在顶空平衡条件下用0.5mol·L-1氢氧化钠溶液将结冷胶水解后，采用顶空气相色谱法测定，色谱柱为DB-624柱（30m×0.53mm，3.0μm）；柱温为50℃；进样口温度为230℃；检测器为FID，温度为260℃；顶空瓶平衡温度为80℃，平衡时间为60min。结果：乙醇在0.051～1.0209 mg·mL-1范围内线性关系良好（r=0.999），异丙醇在0.0077～0.1543 mg·mL-1范围内线性关系良好（r=0.999）；乙醇平均回收率分别为104.2%（RSD=2.3%，n=9），异丙醇的平均回收率为100.6%（RSD=0.9%, n=9）。测定样品22批，结果乙醇含量均小于0.3%，异丙醇含量均小于0.04%。结论：该法操作较为简单、绿色环保，且方法专属性、精密度、重复性、耐用性均良好，可用于评价结冷胶中的残留溶剂情况。 |
| 英文摘要: |
| Objective:To establish a headspace headspace?gas?chromatography for determination of residual solvents Isopropyl Alcoholand ethanol in gellan gum.Methods:Gellan gum was hydrolyzed with 0.5mol·L-1Sodiumm hydroxide solution at headspace equilibrium conditions. Headspace gas chromatography was performed on DB-624GC column(30m×0.53mm，3.0μm）.the column temperature at 50℃.The injection temperature was 230℃;The detector was FID and the temperature was 260℃.The equilibrum temperature of the headspace bottle is 80℃ and the equilibrium time is 60 minuties.Results:The liner ranges of ethanol and isopropyl alcohol were 0.051-1.0209mg·mL-1 (r=0.999) and 0.0077-0.1543mg·mL-1 (r=0.999).The average recoveries of ethanol and Isopropyl Alcohol were 104.2% (RSD= 2.3%,n=9) and 100.6% ( RSD=0.9%,n=9),respectively. 22 batches of samples were tested, and the results showed that the ethanol content was less than 0.3% and the Isopropyl Alcohol content was less than 0.04%. Conclusion: The method is simple,energy conservation, and has good specificity, precision, repeatability and durability. It can be used to evaluat residual solvents in gellan gum. |
|
查看/发表评论 下载PDF阅读器 |
| 关闭 |