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Purity analysis method of 1-methyl-3,5-dinitro-1H-1,2,4-triazole

A HPLC method was established to analyze main ingredient – 1-methyl-3,5-dinitro-1 H -1,2,4-triazole and the main impurity –1-methyl-3-nitro-1 H -1,2,4-triazol-5-amine. The method was carried out on a SinoChrom ODS-BP column (4.6 × 200 mm, 5 μm) using methanol–water (90/10, v/v) as the mobile phase a...

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Bibliographic Details
Published in:Chemistry of heterocyclic compounds (New York, N.Y. 1965) N.Y. 1965), 2017-10, Vol.53 (10), p.1084-1089
Main Authors: Luo, Jin, Liu, Yu-Cun, Liu, Yan, Wang, Guo-Dong, Wang, Jian-Hua, Yuan, Jun-Ming
Format: Article
Language:English
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Summary:A HPLC method was established to analyze main ingredient – 1-methyl-3,5-dinitro-1 H -1,2,4-triazole and the main impurity –1-methyl-3-nitro-1 H -1,2,4-triazol-5-amine. The method was carried out on a SinoChrom ODS-BP column (4.6 × 200 mm, 5 μm) using methanol–water (90/10, v/v) as the mobile phase at a flow rate of 1.0 ml·min –1 . 1-Methyl-3,5-dinitro-1 H -1,2,4-triazole was determined by UV-visible detector at 240 nm. The column temperature was 25°C and the injection volume was 10 μl. Results show that under the optimized chromatographic conditions, the calibration curves of 1-methyl-3,5-dinitro-1 H -1,2,4-triazole and 1-methyl-3-nitro-1 H -1,2,4-triazol-5-amine have good linearity, and the linear correlation coefficient r is greater than 0.999. The detection limits for 1-methyl-3,5-dinitro-1 H -1,2,4-triazole and 1-methyl-3-nitro-1 H -1,2,4-triazol-5-amine were 0.6 and 0.31 mg·ml –1 , respectively, and the quantification limits were 1.02 and 0.53 mg·ml –1 , respectively. The recoveries are 98.17–100.83% with the relative standard deviations between 0.44 and 1.01%. The method has wide linear range, high sensitivity, and good reproducibility, and the results are accurate and reliable.
ISSN:0009-3122
1573-8353
DOI:10.1007/s10593-017-2175-9