| 何文胜,程伟青,陈忠.HS-GC法测定依鲁替尼原料药中6种残留溶剂[J].井冈山大学自然版,2020,41(6):22-26 |
| HS-GC法测定依鲁替尼原料药中6种残留溶剂 |
| SIMULTANEOUS DETERMINATION OF 6 RESIDUAL ORGANIC SOLVENTS IN IBRUTINIB BY HEADSPACE GAS CHROMATOGRAPHY |
| 投稿时间：2020-06-21 修订日期：2020-05-26 |
| DOI：10.3969/j.issn.1674-8085.2020.06.006 |
| 中文关键词: 依鲁替尼原料药 气相色谱法 顶空进样 残留溶剂 |
| 英文关键词: ibrutinib gas chromatography headspace sampling residual |
| 基金项目:2014年福建省科技创新平台项目(2014Y2008);2015年福州市市校(院所)科技合作项目(2015-G-80);2016年福建省省属公益类科研院所基本科研专项(2016R1009-2) |
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| 摘要点击次数: 1924 |
| 全文下载次数: 2965 |
| 中文摘要: |
| 建立了同时测定依鲁替尼原料药中异丙醇、二氯甲烷、乙酸乙酯、四氢呋喃、甲苯、N、N-二甲基甲酰胺(DMF)6种有机溶剂残留量的顶空气相色谱法,并测定样品中的有机溶剂残留量。使用顶空气相色仪,对6种残留溶剂的系统适用性试验、线性范围、定量限、检测限、精密度、重复性和加标回收率进行考察,外标法计算各有机溶剂的残留量残留在样品中的的有机溶剂含量为考察指标。结果显示:异丙醇、二氯甲烷、乙酸乙酯、四氢呋喃、甲苯、DMF分别在:10.21~1060、5.10~138.7、20.22~1035、2.44~360.0、1.98~458.3、20.69~618.5 μg/mL范围内线性关系良好(r > 0.998);各组份检测限分别为0.26、0.27、0.18、0.33、0.08、0.12 μg/mL,在3个添加水平下,各组份的加标回收率在94.5%~100.4%之间。本检测方法灵敏、准确、适用于依鲁替尼(Ibrutinib)中有机残留溶剂的检查。 |
| 英文摘要: |
| To establish a method for the simultaneous determination of 6 kinds of residual organic solvents in ibrutinib，such as isopropyl alcohol，dichloromethane，ethyl acetate，tetrahydrofuran，methylbenzene，N,N-dimethylformamide（DMF）. The applicability test, linear range, quantitative limit, detection limit, precision, repeatability and recovery rate of six kinds of residual solvents were investigated by headspace gas chromatography. The content of residual organic solvents in samples calculated by external standard method was taken as the evaluation index.A good linear correlation of isopropyl alcohol，dichloromethane，ethyl acetate，tetrahydrofuran，methylbenzene，N,N-dimethylformamide were showed at the range of 10.21~1060，5.10~138.7，20.22~1035，2.44~360.0，1.98~458.3，20.69~618.5 μg/mL with r > 0.998，respectively；Detection limit of each components was 0.26、0.27、0.18、0.33、0.08、0.12 μg/mL respectively；At the three levels of addition，the recovery of each component was 94.5%~100.4%. The method is sensitive and accurate，can be used for determination of residual organic solvents in ibrutinib. |
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