Zhu Ron
2015
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Journal
Chinese Journal of Pharmaceutical Analysis
Abstract
Objective: To establish a method for determination of the related substances,2-ethenypyridine,2-( pyridine-2-yl) ethanol,and N-methyl-2-( pyridin-2-yl)-N-[2-( pyridine-2-yl) ethyl]ethanamine trihydrochloride,in betahistine hydrochloride tablets. Methods: HPLC method was adopted. The C18 column was used as the analytical column. The mobile phase consisted of acetonitrile and mixed solution( 0. 69 g of ammonium acetate dissolved in 1 000 m L of water,p H adjusted to 4. 7 with glacial acetic acid,then dissolved with 4. 43 g of sodium lauryl sulfate) at a flow rate of 1. 0 m L·min-1,the detection wavelength was set at 259 nm,and the column temperature was 40 ℃. Results: Betahistine hydrochloride and its impurities could be separated from principle substances completely. The limits of detection was 0. 4,0. 4,4 ng( S / N = 3) for 2-ethenypyridine,2-( pyridine-2-yl) ethanol,and N-methyl-2-( pyridin-2-yl)-N-[2-( pyridine-2-yl) ethyl]ethanamine trihydrochloride; their linearities were good,and their recoveries were 97. 9 %,98. 1 %,101. 7 %,respectively.The two known and six unknown impurities were detected in 119 samples from four manufacturers. The number and the mass of impurities were different among different batches of samples. The contents of 2-( pyridine-2-yl) ethanol and N-methyl-2-( pyridin-2-yl)-N-[2-( pyridine-2-yl) ethyl]ethanamine trihydrochloride were 0. 005 %-0. 47 % and 0. 040 %-1. 26 %,respectively. The total impurities were 0. 2 %-5. 3 %.Conclusion: The method is validated and can be used for test of the related substances in betahistine hydrochloride. It is suggested that 2 % is set as the limit of total impurities in betahistine hydrochloride tablets.