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无衍生化-气相色谱法测定药用胶塞提取液中硬脂酸和棕榈酸
引用本文:余秋玲,马艳,谢威,杨倩,龙梅.无衍生化-气相色谱法测定药用胶塞提取液中硬脂酸和棕榈酸[J].分析测试技术与仪器,2022,28(3):299-303.
作者姓名:余秋玲  马艳  谢威  杨倩  龙梅
作者单位:重庆市计量质量检测研究院,重庆 401123
基金项目:重庆市计量质量检测研究院自立项目[2020(研)-3]
摘    要:建立了无衍生化-气相色谱法测定药用胶塞提取液中硬脂酸和棕榈酸的分析方法. 采用3种不同介质(pH值为3的酸性缓冲溶液、pH值为10的碱性缓冲溶液、20%乙醇溶液)对胶塞进行提取,得到的提取液经正己烷萃取后,采用DB-FFAP(30 m×0.25 mm×0.25 μm)色谱柱进行分离,经火焰离子化检测器(FID)检测,外标法定量. 结果表明,在最优条件下,硬脂酸和棕榈酸峰形对称,分离效果和标准曲线线性良好,平均加标回收率为97.6%~100.5%,相对标准偏差(RSD)为0.4%~2.3%(n=6),检出限(LOD)为1.0~1.5 mg/L. 方法前处理简单、准确度高,可用于药用胶塞提取液中硬脂酸和棕榈酸的检测.

关 键 词:硬脂酸    棕榈酸    无衍生化    气相色谱法    药用胶塞
收稿时间:2022-07-04

Determination of Stearic Acid and Palmitic Acid in Medical Rubber Plug Extracting Solution by Non-derivative Gas Chromatography
Institution:Chongqing Academy of Metrology and Quality Inspection, Chongqing 401123, China
Abstract:A non-derivative gas chromatography (GC) for determining stearic acid and palmitic acid in the extracting solution of medical rubber plug has been established. Three different media (pH=3 acidic buffer solution, pH=10 alkaline buffer solution, 20% ethanol solution) were used to extract the rubber plug. The extracted solution was extracted by hexane, separated on a DB-FFAP (30 m×0.25 mm×0.25 μm) column, detected by a flame ionization detector (FID), and quantified by an external standard method. The results showed that the peaks of stearic acid and palmitic acid were symmetrical under optimal conditions. The separation effect was good and the linear curve fitted well. The average recoveries were 97.6%~100.5%, and the relative standard deviations (RSD) were 0.4%~2.3% (n=6). The detection limit (LOD) was 1.0 mg/L to 1.5 mg/L. The method is simple and accurate, and can be used for the determination of stearic acid and palmitic acid in the extracting solution of medicinal rubber plug.
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