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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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1H定量核磁共振波谱法测定二对甲苯磺酸缘生替尼对照品的含量

Determination of yunsintinib ditosylate reference subsfance by 1H quantitative nuclear magnetic resonance spectroscopy

作者(英文):
分类号:R917
出版年·卷·期(页码):2019,39 (3):432-435
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立采用1H定量核磁共振波谱法测定二对甲苯磺酸缘生替尼对照品的含量。方法:采用核磁共振波谱法。使用Bruker AscendTM 400超导核磁共振谱仪,以氘代DMSO为溶剂,脉冲宽度为10.0μs,延迟时间为1 s和扫描次数32的条件下采集试样氢谱。结果:以化学位移δ分别为5.31和6.28的二对甲苯磺酸缘生替尼和顺丁烯二酸的氢质子峰作为定量峰,其峰面积比与其质量比的线性回归方程为Y=0.128 1X-0.000 4,相关系数为0.999 9,含量测定的重复性试验的RSD为0.20%(n=6)。测得二对甲苯磺酸缘生替尼的含量为98.54%。结论:分析结果表明,在没有对照品的情况下,核磁共振波谱法可用于二对甲苯磺酸缘生替尼的含量测定,该方法可行,具有快速、准确、简便的优点。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To develop 1H quatitative nuclear magnetic resonance (1H qNMR) method for the determination of yunsintinib ditosylate. Methods: 1H qNMR spectroscopy was used in DMSO, with a Bruker AscendTM 400 MHz. For each sample,32 scans were recorded with pulses width of 10.0 μs and delay time of 1 s. Results: The integration of proton signals at δ=5.31 for yunsintinib ditosylate and at δ=6.28 for maleic acid was used for the quantification. Linear regression of quantitative peak areas ratio (Ax/As, Y) of yunsintinib ditosylatemaleic acid versus mass ratio (Wx/Ws, X) yielded a correlation coefficient of 0.999 9 and regression equation of Y=0.128 1X-0.000 4, the precision RSD was 0.20% (n=6). The contents of yunsintinib ditosylate was 98.54%. Conclusion: The results showed that 1H qNMR can be used for the quantitative determination of yunsintinib ditosylate without reference substance. This method is reliable,rapid,accurate and simple.

-----参考文献:---------------------------------------------------------------------------------------

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