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,0.25μm),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0.43~10.8μg/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。
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,0.25μm)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 0.43~10.8μg/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.
作者
邵雪力
宋闫军
谭洋
SHAO Xue-Li;SONG Yan-Jun;TAN Yang(Zhoukou Product Quality Inspection and Testing Center,Zhoukou 466000,China;Wen County Product Quality Inspection and Testing Center,Jiaozuo 454000,China;Puyang Self-employed Private Economic Development Guidance Center,Puyang 457000,China)
出处
《实验室检测》
2024年第10期165-167,共3页
Laboratory Testing
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
Isosorbide Mononitrate Sustained-Release Tablets
ethanol
residual content
temperature gas chromatography for headspace capillary injection
