文章摘要
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)
作者单位E-mail
王彩媚 广东省药品检验所 691262952@qq.com 
王淼* 广东省药品检验所 wangmiao@gdidc.org.cn 
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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.
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