^(1)H定量核磁共振波谱法测定那红地那非的含量  

Determination of noracetildenafil by ^(1)H qNMR

作　　者：冯玉飞[1] 黄海伟[1] 吴先富[1] 孙会敏[1] FENG Yu-fei;HUANG Hai-wei;WU Xian-fu;SUN Hui-min(National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]中国食品药品检定研究院,北京100050

出　　处：《中国新药杂志》2023年第14期1478-1481,共4页Chinese Journal of New Drugs

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.

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 

分 类 号：R917[医药卫生—药物分析学]