核磁共振波谱法测定伐地昔布标准物质的含量  

Assay of valdecoxib reference substance by nuclear magnetic resonance spectroscopy

作　　者：冯玉飞[1] 翟晨斐 金智尚 牛剑钊[1] 孙会敏[1] FENG Yu-fei;ZHAI Chen-fei;JIN Zhi-shang;NIU Jian-zhao;SUN Hui-min(National Institutes for Food and Drug Control,Beijing 100050,China;Beijing Institute of Petrochemical Technology,Beijing 100875,China)

机构地区：[1]中国食品药品检定研究院,北京100050 [2]北京石油化工学院,北京100875

出　　处：《中国新药杂志》2024年第22期2400-2403,共4页Chinese Journal of New Drugs

摘　　要：目的:建立伐地昔布标准物质^(1)H定量核磁共振法(^(1)H quantitative nuclear magnetic resonance,^(1)H qNMR)。方法:在^(1)H qNMR法中,使用Bruker AvanceⅢHD 500超导核磁共振谱仪,以氘代二甲基亚砜为溶剂,采用noesyigld1d脉冲序列,弛豫延迟时间为30 s,扫描次数32次。结果:以伐地昔布δ7.84的氢质子响应信号作为样品定量信号,以三甲基间苯三酚δ6.09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氢原子摩尔量比的线性回归方程为y=0.9922x+0.0023,相关系数为0.9997,重复性实验的RSD为0.12%(n=5)。测得伐地昔布(C_(16)H_(14)N_(2)O_(3)S)的含量为99.25%。与质量平衡法结果(99.61%)、HPLC外标一点法结果(99.87%)一致。结论:本研究建立的^(1)H qNMR法可用于伐地昔布的含量测定,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^(1)H quantitative nuclear magnetic resonance(^(1)H qNMR)method for determination of the content of valdecoxib reference substance.Methods:For^(1)H qNMR,a Bruker AvanceⅢHD 500 superconducting nuclear magnetic resonance spectrometer was used with deudimethyl sulphone as solvent and noesyigld1d pulse sequence with relaxation delay time of 30 s and 32 scanning times.Results:The signalsδ7.84 of valdecoxib andδ6.09 of 1,3,5-trimethoybenzene were used for quantitation.The linear regression equation of response area ratio of internal standard signal and molar ratio of hydrogen atom was y=0.9922x+0.0023,the correlation coefficient was 0.9997,and the RSD of repeatability experiment was 0.12%(n=5).The content of vadoxib(C_(16)H_(14)N_(2)O_(3)S)was 99.25%,which was consistent with the results by mass balance method(99.61%)and HPLC assay method(99.87%).Conclusion:The nuclear magnetic quantitative method established in this paper can be used for the determination of vadoxib content.It is accurate and rapid,providing a strong evidence for the determination of reference material by mass balance method.

关 键 词：伐地昔布 标准物质 含量测定 ^(1)H定量核磁共振波谱法 

分 类 号：R917[医药卫生—药物分析学]