^(1)H定量核磁共振波谱法测定新型P2Y_(12)受体抑制剂TSD-1中非氘TSD-1-ND的含量

Determination of Non-deuterium TSD-1-ND in TSD-1,A Novel P2Y_(12) Receptor Inhibitor,by ^(1)H Quantitative Nuclear Magnetic Resonance Method

目的建立^(1)H定量核磁共振波谱(^(1)H quantitative nuclear magnetic resonance,^(1)H qNMR)法测定TSD-1原料药中非氘TSD-1-ND的含量。方法采用核磁共振波谱法,使用BRUKER AV-400型核磁共振仪,以氘代氯仿为溶剂,弛豫延迟时间为10 s,扫描次数32次。结果以化学位移δ分别为3.75和3.03的TSD-1-ND和丁二酸酐的氢质子峰作为定量峰,其峰面积比与其质量比的线性回归方程为Y=3.4931X-0.0597,相关系数(r)为0.9981,3批TSD-1-ND测得含量分别为0.1697%、0.1806%和0.1677%。结论该法操作简单,测定结果准确,可用于TSD-1中非氘TSD-1-ND的含量测定。

OBJECTIVE To establish an ^(1)H quantitative nuclear magnetic resonance(^(1)H qNMR)method for determination of non-deuterium TSD-1-ND in TSD-1 active pharmaceutical ingredient.METHODS ^(1)H qNMR spectra were obtained in CDCl_(3) by using a BRUKER AV-400 NMR spectrometer.The relaxation delay time was 10 s.Thirty-two scans were recorded.RESULTS The integration of proton signals atδ=3.75 for TSD-1-ND andδ=3.03 for succinic anhydride was used for the quantification.Linear regression of quantitative peak areas ratio of TSD-1-ND and succinic anhydride versus mass ratio yielded a correlation coefficient of 0.9981 and regression equation of Y=3.4931X-0.0597.The contents of three batches of TSD-1-ND were 0.1697%,0.1806%and 0.1677%.CONCLUSION This method is easy and simple to operate,and the analysis results are accurate.Therefore,^(1)H qNMR method can be used for the quality control of TSD-1-ND.