定量核磁共振氢谱测定新药替格瑞洛  

A Proton Nuclear Magnetic Resonance Method for Quantitative Analysis of Ticagrelor

作　　者：张芬芬 沈文斌[2] 徐开兵 杨明 ZHANG Fen-fen;SHEN Wen-bin;XU Kai-bing;YANG Ming(Research Center for Analysis and Measurement,Donghua University,Shanghai 201620,China;Pharmaceutical Research Institute,China Pharmaceutical University,Nanjing 210009,China)

机构地区：[1]东华大学分析测试中心,上海201620 [2]中国药科大学药物研究院,江苏南京210009

出　　处：《波谱学杂志》2020年第2期216-223,共8页Chinese Journal of Magnetic Resonance

摘　　要：本文建立了基于核磁共振氢谱(~1H NMR)测定新药替格瑞洛绝对含量的方法.采用Bruker Avance 300型NMR谱仪,以磺胺多辛为内标;以替格瑞洛中质子信号δH7.14(2H,m)和δH7.04(1H,s),磺胺多辛质子信号δH8.04(1H,s)、δH 7.73(2H,d)和δH 6.54(2H,d)作为定量峰;以氘代甲醇(CD3OD)为溶剂进行测定.测定条件为:探头温度为308 K,谱宽为3511.5 Hz,中心频率为1470.6 Hz,脉冲翻转角为θ=30°,延迟时间为10 s,采样次数为16,线宽因子为0.3Hz.在此实验条件下,替格瑞洛样品与内标磺胺多辛的定量峰分离良好,实验结果精密度较高、重复性较好、线性范围较宽,其线性拟合方程为:Y=1.053X-0.081(r=0.996,n=5).最终测得样品中替格瑞洛含量为99.4%,相对标准偏差(RSD)为0.20%.该方法简便、准确、快速,适用于替格瑞洛样品的绝对含量测定.A novel proton nuclear magnetic resonance(~1H NMR)method for determining the absolute content of ticagrelor was proposed.The ideal spectra were obtained on a Bruker Avance-300 spectrometer with deuterated methanol(CD3 OD)as the solvent and sulfadoxin as the internal standard.The ticagrelor signals atδ_H 7.14(2 H,m)andδ_H 7.04(1 H,s),as well as those of sulfadoxin atδ_H 8.04(1 H,s),δ_H 7.73(2 H,d)andδ_H 6.54(2 H,d),were selected for quantitative analysis.The detection conditions were as following:probe temperature 308 K,spectrum width 3511.5 Hz,center frequency 1470.6 Hz,pulse angleθ=30?,delay time(d1)10 s,number of scans 16 and line broadening 0.3 Hz.The signals from ticagrelor and internal standard sulfadoxin showed good separation,precision,reproducibility,and wide linearity ranges with Y=1.053 X-0.081(r=0.996,n=5).The content of ticagrelor was estimated to be 99.4%(RSD=0.20%).This method was proven simple,accurate and rapid.

关 键 词：核磁共振氢谱 替格瑞洛 含量测定 

分 类 号：O657.61[理学—分析化学] O482.53[理学—化学]