Liu Yan
2014
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Journal
Chinese Journal of Pharmaceutical Analysis
Abstract
Objective: To establish a quantitative NMR( qNMR) method to determine the content of 1H- pyrazole-1- carboxamidine in 1H- pyrazole- 1- carboxamidine hydrochloride. Methods: Hydroquinone was used as an internal standard,methanol- d4as solvent in1H- NMR to characterize 1H- pyrazole- 1- carboxamidine,and calculate the content of 1H- pyrazole- 1- carboxamidine by comparing the response peak area of sample( As) and internal standard( Ar). Results: One sample solution was characterized under the same NMR conditions for six times,RSD of As/Arwas 0. 38. For five sample solutions which were parallel prepared,RSD of As/Arwas 0. 29%. Meanwhile,based on different peaks,the content of 1H- pyrazole- 1- carboxamidine calculated was 65. 6%,65. 8%and 66. 3% respectively,RSD was 0. 71%,0. 97% and 1. 4% respectively. The results were consistent with the result from mass balance method( 65. 7%). Conclusion: Using qNMR to characterize the content of 1H- pyrazole-1- carboxamidine can avoid the effect of hydrochloride. This method can be used for determination of the content of1H- pyrazole- 1- carboxamidine according to the method validation.