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

• 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
• Subjects: Analysis; Chemistry; Chemistry and Materials Science; Correlation coefficients; Flow velocity; High performance liquid chromatography; Linearity; Methanol; Methods; Organic Chemistry; Pharmacy; Reproducibility; Triazoles
• ISSN: 0009-3122; 1573-8353
• DOI: 10.1007/s10593-017-2175-9

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.