定量核磁共振法测定帕瑞昔布钠的质量分数  

Determination of parecoxib sodium mass fraction by ^(1)H qNMR

作　　者：冯玉飞[1] 马玲云[1] 关皓月[1] 刘倩[1] 杨东升 翟晨斐 张广超 牛剑钊[1] FENG Yu-fei;MA Ling-yun;GUAN Hao-yue;LIU Qian;YANG Dong-sheng;ZHAI Chen-fei;ZHANG Guang-chao;NIU Jian-zhao(National Institute 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》2024年第12期1277-1280,共4页Chinese Journal of New Drugs

摘　　要：目的:建立采用^(1)H定量核磁共振波谱法(^(1)H qNMR)测定帕瑞昔布钠对照品质量分数的方法。方法:在^(1)H qNMR中,使用Bruker Ascend 600超导核磁共振谱仪,以氘代二甲基亚砜为溶剂,采用zg30脉冲序列,弛豫延迟时间为30 s,扫描次数为64次。结果:以帕瑞昔布钠δ7.74的氢质子响应信号作为样品定量信号,以马来酸δ6.23的氢质子响应信号作为内标物定量信号。样品内标物信号响应面积比与质量比的线性回归方程为y=0.2962x-0.0010,相关系数为0.9997,重复性实验的RSD为0.15%(n=6)。测得帕瑞昔布钠(以C_(19)H_(17)N_(2)O_(4)S^(-)计)的质量分数为93.91%,与质量平衡法(93.83%,按C_(19)H_(17)N_(2)O_(4)S^(-)计)、HPLC外标一点法(93.89%)结果一致。结论:本文建立的核磁定量方法可用于帕瑞昔布钠的质量分数测定,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佐证。Objective:To establish an^(1)H quantitative nuclear magnetic resonance(^(1)H qNMR)method for the determination of parecoxib sodium.Methods:^(1)H qNMR spectra were obtained in DMSO-d_6 by using Bruker Ascend 600 spectrometer with zg30 pulse sequence,the relaxation delay time was 30 s,and 64 scans were recorded.Results:The signalsδ7.74 of parecoxib sodium andδ6.23 of maleic acid were used for quantitation.Linear regression of areas ratio versus mass ratio yielded a correlation coefficient of 0.9997 and regression equation of y=0.2962x-0.0010,the repeatability RSD was 0.15%(n=6),and the mass fraction of parecoxib(C_(19)H_(17)N_(2)O_(4)S^(-))was 93.91%,which was consistent with the results by mass balance method(93.83%)and HPLC assay method(93.89%).Conclusion:The established^(1)H qNMR method can be used for the quantitative determination of parecoxib sodium.It is accurate and rapid and could be complementary to the mass balance method for the assay of reference substances.

关 键 词：^(1)H定量核磁共振波谱法 质量分数测定 标准物质 帕瑞昔布钠 

分 类 号：R917[医药卫生—药物分析学]