摘要
目的采用核磁共振法测定甲磺酸阿帕替尼原料药中甲磺酸阿帕替尼,提供一种有效的化学样品测定手段。方法以1,4-二硝基苯为内标,甲磺酸阿帕替尼为样品,DMSO-d6为溶剂,采用zg30脉冲序列在恒温(25℃)下获取1H-NMR谱。以δ7.50处样品定量峰和δ8.46处内标峰面积比值测定氢核磁共振谱,计算甲磺酸阿帕替尼的质量分数。并与质量平衡法测定结果进行了比较。结果甲磺酸阿帕替尼在0.01-0.05 mmol/L线性关系良好。原料药中甲磺酸阿帕替尼质量分数为96.66%,RSD值为0.33%。与质量平衡法测定的结果 96.25%基本一致。结论本法样品制备简单,测定快速,结果准确,可用于测定甲磺酸阿帕替尼原料药中甲磺酸阿帕替尼。
Objective To establish a nuclear magnetic resonance method to determine the content of apatinib mesylate in apatinib mesylate raw materials, so as to provide an effective method for chemical sample. Methods 1,4-Dinitrobenzene was used as an internal standard, apatinib mesylate was used as a sample, DMSO-d6 was used as solvent, and the 1H-NMR data of apatinib mesylate were determined at constant temperature (25 ℃) using zg30 pulse sequence. 1H-NMR data of the sample peak area at δ7.50 and internal standard peak area ratio at δ8.46 were obtained. And the results of nuclear magnetic resonance method were compared with those of mass balance method. Results There was a good linear relationship of apatinib mesylate in the rang of 0.01 - 0.05 mmol/L. The content of apatinib mesylate in raw material was calculated to be 96.66% with RSD 0.33%. The result was consistent with that calculated by mass balance method (96.25%). Conclusion This method is simple, rapid, and accurate results, which can be used for determination content of apatinib mesylate in raw material.
出处
《现代药物与临床》
CAS
2016年第12期1887-1890,共4页
Drugs & Clinic
基金
国家重大新药创制专项(2015ZX09303001)
中国食品药品检定研究院中青年基金资助项目(2014A6
2015A01)