| 李青翠.米格来宁片有关物质和含量测定方法研究[J].中国药品标准,2023,24(2): |
| 米格来宁片有关物质和含量测定方法研究 |
| Determination of related substances and the contents of Migliening Tablets |
| 投稿时间：2022-03-18 修订日期：2023-04-06 |
| DOI： |
| 中文关键词: 米格来宁片 有关物质 安替比林 咖啡因 含量测定 高效液相色谱法 |
| 英文关键词: migliening tablets relatedsubstances antipyrine caffeine content determination high performance liquid chromatography |
| 基金项目: |
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| 摘要点击次数: 261 |
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| 中文摘要: |
| 目的：建立米格来宁片有关物质与含量测定的HPLC方法。方法：采用Thermo Acclaim TM 120 C18柱（4.6mm×250mm，5μm）色谱柱；有关物质流动相：以0.01mol/L醋酸钠溶液-乙腈进行梯度洗脱；含量测定流动相为0.01mol/L醋酸钠溶液-乙腈（85:15）；流速1.0mL·min-1；检测波长275nm；进样量10μL。结果：安替比林和咖啡因分别与11种杂质完全分离，分离度大于1.5，测定杂质F校正因子为1.01，采用高分辨液质联用仪和ADMET Predictor软件推断主要未知杂质结构与毒性；含量测定咖啡因在11.0~109.6μg/mL浓度范围内线性关系良好（r=1.0000），平均回收率为99.03%（n=9），定量限为4.4ng；安替比林在109.96~1099.6μg/mL浓度范围内线性关系良好（r=1.0000），平均回收率为100.56%（n=9），定量限为11.0ng。结论：本方法专属、灵敏、简便，可用于测定米格来宁片中有关物质（杂质F≤0.03%，总杂质≤0.05%）以及安替比林和咖啡因的含量(安替比林：98.8%~101.4%，咖啡因：84.4%~107.5%)。 |
| 英文摘要: |
| Objective: To establish a method for the determination of related substances and contents in Migliening Tablets by HPLC. Methods: Thermo Acclaim TM 120 C18 column (4.6mm×250mm, 5 μm) was used for chromatographic column;the mobile phase of related substances was gradient elution with 0.01 mol/L sodium acetate solution-acetonitrile; the mobile phase was 0.01 mol/L sodium acetate solution-acetonitrile (85:15); the flow rate was 1.0 mL min-1; the detection wavelength was 275 nm; and the injection volume was 10 microL. Results: Antipyrine and caffeine were completely separated from 11 impurities with a separation degree greater than 1.5. The correction factor for determination of impurity F is 1.01. The structure and toxicity of the main unknown impurities were inferred by high resolution liquid chromatography-mass spectrometry (HPLC-MS) and ADMET Predictor software.The linear relationship between the concentration of caffeine in the range of 11.0-109.6μg/mL was good (r=1.0000),the average recovery was 99.03% (n=9), and the quantitative limit was 4.4 ng. The linear relationship of antipyrine was good in the concentration range of 109.96-1099.6 μg/mL (r=1.0000), the average recovery was 100.56% (n=9), and the quantitative limit was 11.0ng. Conclusion: The method is specific, sensitive and simple. It can be used for the determination of related substances（impurity F ≤0.03%,total impurities ≤0.05%）, antipyrine and caffeine in Miglening Tablets(antipyrine:98.8%~101.4%,caffeine:84.4%~107.5%). |
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