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

A HPLC method was established to analyze main ingredient 1-methyl-3, 5-dinitro-1, 2, 4-triazole (MDNT) and the main impurity 1-methyl-3-nitro-5-amino-1, 2, 4-triazole (NAMT). The method was carried out on a SinoChrom ODS-BP column (4.6mm×200mm, 5um) using methanol-water (90/10, V/V) as the mobile phase at a flow rate of 1.0 mL·min -1 , and MDNT sample was determined by a UV-visible detector at the wavelength of 240 nm. The column temperature was 25℃ and the injection volume was 10uL. Results show that under the optimized chromatographic conditions, the calibration curves of MDNT and NAMT have good linearity, and the linear correlation coefficient r is greater than 0.999. For MDNT and NAMT, the detection limits for MDNT and NAMT were 0.6 mg·L -1 and 0.31 mg·L -1 , respectively, and the quantification limits for the two were 2mL·L -1 and 1.02 mg·L -1 , respectively. The spiked recoveries are 99.60 %-100.39 % with the relative standard deviations (RSDs) between 1.63 % and 2.07 %. The method has wide linear range, high sensitivity and good reproducibility, and the results are accurate and reliable. The method can be used for the determination of the related substances in the product of MDNT, and can meet the demand of the analysis of actual samples.