Optimization of detection range of hydrazides of carboxylic acids and 2-acylhydrazinсarbothioamids by HPLC-ECI-MC
Elaboration of control steps of hydrazids and сarbothioamids, raw materials in the synthesis of 1,2,4-triazol-3-yl-thioacetate acids, potential drug substances on research and production stage is an important task. The study of adsorption, distribution, metabolism and excretion of these substances has great importance. The HPLC-MS is the most universal and selective method used in these cases.
The aim of our study was to determine the optimal conditions for mass spectrometric detection of ionization in electrospray in HPLC-MS іzonіcotinohydrazide, furan-2-carbohydrazide, 2-morpholinoacetohydrazide, 2-methoxybenzohydrazide, 2-isonicotinoyl-N-(2-methoxyphenyl)hydrazine-1-carbothioamide, 2-(furan-2-carbonyl)-N-phenylhydrazine-1-carbothioamide, 2-(2-morpholinoacetyl)-N-phenylhydrazine-1-carbothioamide, N-methyl-2-(2-morpholinoacetyl)hydrazine-1-carbothioamide, 2-(2-methoxybenzoyl)hydrazine-1-carbothioamide, precursor substances in the synthesis of salts of 1,2,4-triazol-3-yl-thioacetate acids for 8 synthetic schemes using full factorial design on 3 factors and polynomial regression equations.
Work was carried out using flow injection analysis (the technique of direct sample introduction into the ion source) on a liquid chromatograph Agilent 1260 Infinity HPLC System with a single quadrupole mass spectrometer Agilent 6120.
The optimal conditions of mass spectrometric detection series hydrazides and сarbothioamides for HPLC-ESI-MS on the basis of the calculated maxima polynomial regression functions were obtained. The equation of polynomial regression for the corresponding hydrazides and carbatioamides were suggested. The equations show the dependence of the mass detector signal intensity on three important factors: dryng gas temperature, the fragmentor voltage, the nebulizer pressure. The optimal conditions of mass spectrometric detection choice to maximize the signal detector and thus increase the sensitivity and selectivity of the determinations. It may allow partially separate the signal of these substances from the impurities signal because these conditions have specificity.
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