毛细管柱顶空进样程序升温气相色谱法检测单硝酸异山梨酯缓释片中乙醇量
Determination of ethanol content in Isosorbide Mononitrate Sustained-Release Tablets by gas chromatography
邵雪力 1宋闫军 2谭洋3
作者信息
- 1. 周口市产品质量检验检测中心,周口 466000
- 2. 温县产品质量检验检测中心,焦作 454000
- 3. 濮阳市个体私营经济发展指导中心,濮阳 457000
- 折叠
摘要
目的 建立毛细管柱顶空进样程序升温气相色谱法检测单硝酸异山梨酯缓释片中乙醇残留量.方法 采用 6%氰丙基苯基-94%二甲基聚硅氧烷(或极性相近)为固定液的毛细管柱(30 m×0.320 mm,0.25 μm),起始温度为 50℃,维持 6 min,以每分钟 50℃的速率升温至 200℃,维持 3 min;检测器温度为 250℃;进样口温度为200℃;顶空瓶平衡温度为80℃,平衡时间为30 min;氮气流速为1 mL/min;分流比为50∶1.结果 在上述色谱条件下,乙醇的保留时间为 3 min,乙醇浓度在 0.43～10.8 μg/mL范围内质量浓度与峰面积呈良好的线性关系.方法的加标回收率为87.04%～94.45%之间,RSD=0.17%(n=6).结论:本法样品前处理简便、干扰少、重现性好,精度高,可用于单硝酸异山梨酯缓释片中乙醇量的质量控制.
Abstract
Objective Establishment of a capillary column headspace sampling program for Gas chromatography determination of ethanol residue in Isosorbide Mononitrate sustained-release tablets.Methods A capillary column(30 m×0.320 mm,0.25 μm)with 6%cyanopropylphenyl-94%dimethylpolysiloxane(or similar polarity)as stationary solution was used.The starting temperature was 50℃and maintained for 6 min,the temperature of the detector was 250℃,the temperature of the inlet was 200℃,the equilibrium temperature of the headspace bottle was 80℃,the equilibrium time was 30 min,the flow rate of nitrogen was 1 mL/min,and the temperature of the headspace bottle was 200℃.The shunt ratio was 50∶1.Results Under the above chromatographic conditions,the retention time of ethanol was 3 min and the concentration of ethanol was in the range of 0.43～10.8 μg/mL.The recoveries were 87.04%～94.45%,RSD=0.17%(n=6).Conclusion The method is simple,accurate and can be used for the quality control of ethanol in Isosorbide Mononitrate Sustained-Release Tablets.
关键词
单硝酸异山梨酯缓释片/乙醇/残留量/毛细管柱顶空进样程序升温气相色谱法Key words
Isosorbide Mononitrate Sustained-Release Tablets/ethanol/residual content/temperature gas chromatography for headspace capillary injection引用本文复制引用
出版年
2024
NETL
NSTL
万方数据