核磁共振法测定依帕列净含量  

Quantitative Determination of Empagliflozin by Nuclear Magnetic Resonance

作　　者：孙林林[1] 张芬芬[2] 沈文斌[3] 丁娅[1] 

机构地区：[1]中国药科大学药物分析教研室,江苏南京210009 [2]东华大学分析测试中心,上海201620 [3]中国药科大学药物科学研究院,江苏南京210009

出　　处：《分析测试学报》2016年第9期1157-1161,共5页Journal of Instrumental Analysis

摘　　要：分别以盐酸吉西他滨和齐多夫定为内标，采用定量核磁共振法对依帕列净含量进行测定。以氘代二甲亚砜和重水混合液为溶剂，确定氢定量核磁共振方法（1H-qNMR）的测试条件为：激发脉冲角度30°；时间域数据点32 K；测定温度303 K；脉冲延迟时间20 s；采样次数32；窗函数0.3 Hz。在此实验条件下，结果专属性良好，稳定性可达24 h，耐用性符合要求。以样品与内标的峰面积比对其摩尔比绘制标准曲线，结果显示，依帕列净与内标盐酸吉西他滨的摩尔比在0.512 5~1.953 8范围内，依帕列净与内标齐多夫定的摩尔比在0.494 7~1.966 0范围内线性关系良好，相关系数（r2）均为0.999 9。以盐酸吉西他滨和齐多夫定为内标时,依帕列净的含量测定结果分别为99.83%和99.77%，相对标准偏差（RSD）分别为0.06%和0.19%。2种内标方法的测定结果一致，所建立的方法专属、准确、简便、快捷，适用于新药的含量测定。A method was established to determine the content of empagliflozin by 1H nuclear magnetic resonance spectroscopy（1H-NMR），using gemcitabine hydrochloride and zidovudine as the internal standard，repectively.NMR spectra were recorded using a standard 1D pulse sequence at a 30° flip angle and with DMSO-d6-D2O as the solvent.Thirty two scans of 32 K data points were acquired at a temperature of 303 K，a relaxation delay of 20 s and a line broad of 03 Hz.Under the optimal conditions，method validation indicated specificity，robustness and stability up to 24 h.A good linear relationship was obtained between peak area ratio and molar ratio of empagliflozin to the internal standard.For gemcitabine，the regression equation was y=0.009x-0.003（r2=0.999 9） with a molar ratio range of 0.512 5-1.953 8.For zidovudine，the regression equation was y=0.576x-0.026（r2=0.999 9） with a molar ratio range of 0.494 7-1.966 0.The contents of empagliflozin were 99.83%（n=3，RSD=0.06%）and 99.77%（n=3，RSD=0.19%）corresponding to the internal standards gemcitabine hydrochloride and zidovudine，respectively.The results were consistent with each other，indicating that the method had the advantages of accuracy，high sensitivity and good repeatability，and could be used for the quantification of new drugs.

关 键 词：依帕列净 定量核磁共振 盐酸吉西他滨 齐多夫定 

分 类 号：O482.532[理学—固体物理] TQ460.72[理学—物理]