~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：仲艳[1] 李家春[1] 王志霞[1] 黄文哲[1] 王振中[1] 肖伟[1] ZHONG Yan;LI Jia-chun;WANG Zhi-xia;HUANG Wen-zhe;WANG Zhen-zhong;XIAO Wei(Jiangsu KAN ION Pharmaceutical Co. ,Ltd,Lianyungang 222047,China)

机构地区：[1]江苏康缘药业股份有限公司,连云港222047

出　　处：《药物分析杂志》2019年第3期432-435,共4页Chinese Journal of Pharmaceutical Analysis

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 Ascend^(TM) 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。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 1 X-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.

关 键 词：1H定量核磁共振波谱法 内标法 二对甲苯磺酸缘生替尼 含量测定 方法验证 

分 类 号：R917[医药卫生—药物分析学]