| 王瑞芬.顶空气相色谱法同时测定盐酸金刚烷胺原料药中 5种有机溶剂残留量[J].安徽医药,2024,28(8):1529-1531. |
| 顶空气相色谱法同时测定盐酸金刚烷胺原料药中 5种有机溶剂残留量 |
| Simultaneous determination of 5 residual organic solvents in amantadine hydrochloride by headspace GC |
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| DOI：10.3969/j.issn.1009-6469.2024.08.009 |
| 中文关键词: 金刚烷胺 有机溶剂残留 气相色谱 原料药 |
| 英文关键词: Amantadine Residual organic solvents Gas chromatography Active pharmaceutical ingredients |
| 基金项目: |
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| 中文摘要: |
| 目的建立顶空气相色谱法定量分析盐酸金刚烷胺原料药中乙醇、丙酮、乙腈、二氯甲烷和三氯乙烷残留量方法。方采用 Agilent DB-624色谱柱( 30 m×0.53 mm，3.0 μm)，程序升温， FID检测器，进样口温度 200 ℃，检测器温度 250 ℃，载气为法氮气( N2)流速 2.5 mL/min，分流比 5∶1，顶空平衡温度 80 ℃，平衡时间 30 min。结果有机溶剂浓度与峰面积相关性系数大于 0.999 3；加样，回收率 97.78%～101.03%，相对标准偏差( RSD)1.27%～2.26%。结论该分析方法高效快捷、重复性与稳定性好，准确度高，有望为盐酸金刚烷胺原料药中乙醇、丙酮、乙腈、二氯甲烷和三氯乙烷残留溶剂的定量分析控制提供扎实的试验依据。 |
| 英文摘要: |
| Objective To establish a headspace gas chromatography method for quantitative analysis of residual amounts of ethanol,acetone, acetonitrile, dichloromethane, and trichloroethane in amantadine hydrochloride raw materials.Methods The separation used Agilent DB-624 capillary column (30 m×0.53 mm, 3.0 μm), programmed heating, FID detector. The inlet temperature and the detectortemperature were set at 200 ℃ and 250 ℃, respectively. Carrier gas was nitrogen (N2), the flow rate was 2.5 mL/min, the split ratio was 5∶1, and the headspace equilibrium temperature was 80 ℃. Balance time was 30 min.Results There was a good linear relationshipbetween the concentration of the solvent to be tested and its peak area (correlation coefficient>0.999 3); The average sample recoveryrate is 97.78% to 101.03%, and the RSD was 1.27% to 2.26%.Conclusions This analytical method is efficient, fast, with good repeat-ability and stability, and high accuracy. It is expected to provide a solid experimental basis for the quantitative analysis and control ofresidual solvents such as ethanol,acetone,acetonitrile, dichloromethane, and trichloroethane in amantadine hydrochloride raw materials. |
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