Optimization of the detection conditions for the series of 1,2,4-triazole-3-thiones for fia-esi-ms

Authors

  • B. O. Varynskyi Zaporizhzhia State Medical University, Ukraine
  • A. G. Kaplaushenko Zaporizhzhia State Medical University, Ukraine

DOI:

https://doi.org/10.24959/nphj.16.2063

Keywords:

flow injection analysis (FIA), high performance liquid chromatography (HPLC), mass-spectrometry (MS), electrospray ionization (ESI), 1, 2, 4-triazole-3-thions, optimization, polynomial regression

Abstract

Development of methods for determination of 1,2,4-triazole-3-thiones as intermediate substances in the synthesis of 1,2,4-triazole-3-thioacetate acids salts as potential drugs is an important task at the research and production stage. The study of absorption, distribution, metabolism and excretion requires development of the corresponding methods. The most universal and selective methods used in these cases is the HPLC-MS.The aim of this study was to optimize the conditions of mass spectrometric detection for FIA-MS (flow injection analysis with mass-spectrometric detection) and HPLC-MS (high performance liquid chromatography with mass-spectrometric detection) with the electrospray ionization of eight 1,2,4-triazole-3-thiones by three factors of full factorial design and polynomial regression equations. The work has been performed using the technique of direct sample introduction into the ion source (flow injection analysis - FIA) on an Agilent 1260 Infinity HPLC system with an Agilent 6120 single quadrupole mass spectrometer. The equations of polynomial regression dependence of the signal intensity of the mass detector on three important factors such as the gas drier temperature, the fragmentor voltage and the nebulizer gas pressure have been calculated for the substances studied. Based on the location of the maxima of the functions obtained the optimal values of these factors have been determined. The choice of optimal conditions of mass spectrometric detection allows to maximize the signal on the detector and thus to increase the sensitivity and selectivity of determinations.

Author Biographies

B. O. Varynskyi, Zaporizhzhia State Medical University

Physical and Colloidal Chemistry Department

A. G. Kaplaushenko, Zaporizhzhia State Medical University

Physical and Colloidal Chemistry Department

References

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Published

2016-03-11

Issue

No. 1(85) (2016)

Section

Synthesis and Analysis of Biologically Active Substances

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Copyright (c) 2016 National University of Pharmacy

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