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

B. O. Varynskyi, A. G. Kaplaushenko

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.


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

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References


Каплаушенко А.Г. Синтез, будова і біологічна активність похідних 4-моно- та 4,5-дизаміщених 1,2,4-триазол-3-тіону: Автореф. дис. ... докт. фарм. наук.: 15.00.02. / Запорізький держ. мед. ун-тет, 2012. – 43 с.

Каплаушенко А.Г., Панасенко О.І., Книш Є.Г. та ін. // Фармац. журн. – 2008. – №2. – C. 67-72.

Самелюк Ю.Г., Каплаушенко А.Г. // Актуальні питання фармац. та мед. науки та практики. – 2013. – №2. – С. 125-128.

Щербіна Р.О., Панасенко О.І., Книш Є.Г. та ін. // Актуальні питання фармац. та мед. науки та практики. – 2014. – №3. – С. 18-21.

Cremin P., Kasim-Karakas S., Waterhouse A.L. // J. Agric. Food Chem. – 2001. – Vol. 49. – P. 1747-1750.

Gratz S.R., Flurer Ch.L., Wolnik K.A. // J. Pharmac. Biomed. – 2004. – Vol. 36. – P. 525-533.

Haverford college. Department of Chemistry. Resources. Instruments. Analysis by Direct Injection on the Agilent LC/MS. http://www.haverford.edu/chem/Agilent%20Direct%20Inject.pdf

Huang L.-F. et al. // J. Pharmac. Biomed. – 2003. – Vol. 33. – P. 1155-1162.

Lin L.-Z. et al. // J. Agric. Food Chem. – 2000. – Vol. 48. – P. 354-365.

Takino M. Determination of the metabolites of nitrofuran antibacterial drugs in chicken tissue by LC-ESI-MS, Agilent Technologies, 2003 (application note).


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DOI: https://doi.org/10.24959/88832

Abbreviated key title: Vìsn. farm.

ISSN 2415-8844 (Online), ISSN 1562-7241 (Print)