摘要
目的:建立采用^(1)H定量核磁共振(qNMR)波谱法测定那红地那非对照品的含量。方法:在^(1)H qNMR中,使用Bruker Ascend 600超导核磁共振谱仪,以氘代氯仿为溶剂,采用noesyigld1d脉冲序列,弛豫延迟时间为30 s,扫描次数32次。结果:以那红地那非δ8.15和δ9.14的氢质子响应信号作为样品定量信号,以1,3,5-三甲氧基苯δ6.09的氢质子响应信号作为内标物定量信号。样品δ8.15与内标物δ6.09信号响应面积比与质量比的线性回归方程为y=0.119 7x+0.003 4,相关系数为0.999 1,重现性实验的RSD为1.66%(n=5),重复性实验的RSD为0.76%,测得那红地那非的含量为97.48%;样品δ9.14与内标物δ6.09信号响应面积比与质量比的线性回归方程为:y=0.116 8x+0.004 5,相关系数为0.999 1,重现性实验的RSD为1.69%,重复性实验的RSD为0.43%,测得那红地那非的含量为95.35%。^(1)H qNMR法测得那红地那非的含量(两组响应信号测得的含量平均值)为96.42%,与质量平衡法结果(96.54%)以及HPLC外标一点法结果(97.07%)一致。结论:本研究建立的核磁定量方法可用于那红地那非的含量测定,该方法准确、快速,并为质量平衡法对标准物质定值提供有力的佐证。
Objective:To establish an^(1)H quantitative nuclear magnetic resonance(^(1)H qNMR)method for determination of noracetildenafil.Methods:^(1)H qNMR spectra were obtained in CDCL3 by using Bruker Ascend 600 spectrometer with noesyigld1d pulse sequence,the relaxation delay time was 30 s,and 32 scans were recorded.Results:The signalsδ8.15 and 9.14 of noracetildenafil andδ6.09 of 1,3,5-Trimethoxybenzene were used for quantitation.Linear regression of areas ratio(A_(s)/A_(r))versus mass ratio(W_(s)/W_(r))ofδ8.15 and 6.09 yielded a correlation coefficient of 0.9991 and regression equation of y=0.1197x+0.0034,the replicability RSD was 1.66%(n=5),the repeatability RSD was 0.76%(n=5),and the determined content was 97.48%.Linear regression of areas ratio(A_(s)/A_(r))versus mass ratio(W_(s)/W_(r))atδ9.14 and 6.09 yielded a correlation coefficient of 0.9991 and regression equation of y=0.1168x+0.0045,the replicability RSD was 1.69%(n=5),the repeatability RSD was 0.43%(n=5),and the content of noracetildenafil was 95.35%.The result determined by^(1)H qNMR method(96.42%)was consistent with the results by mass balance method(96.54%)and HPLC assay method(97.07%).Conclusion:The established^(1)H qNMR method can be used for the quantitative determination of noracetildenafil.It is accurate and rapid and could be complementary with the mass balance method for the assay of reference substances.
作者
冯玉飞
黄海伟
吴先富
孙会敏
FENG Yu-fei;HUANG Hai-wei;WU Xian-fu;SUN Hui-min(National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《中国新药杂志》
CAS
CSCD
北大核心
2023年第14期1478-1481,共4页
Chinese Journal of New Drugs
关键词
^(1)H定量核磁共振波谱法
含量测定
标准物质
内标法
那红地那非
^(1)H quantitative nuclear magnetic resonance
content assay
chemical reference standard
internal standard method
noracetildenafil
