文章摘要
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:
作者单位E-mail
李青翠* 山西省食品药品检验所 LQC8819@sina.com 
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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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