Abstract
In the previous studies, NUPh scientists proved that the search of potential anticonvulsants among derivatives of 1,3,4-thiadiazole is very perspective [1-3]. At the medicinal chemistry department of NUPh N-(5-ethyl-[1,3,4]-thiadiazole-2-yl)-2-nitrobenzamide was synthesized. This substance demonstrated high anticonvulsive activity on pentylentetrazole model of seizure compared to classic drug «Depakin». The substance is patented and proposed for further preclinical studies. One of the most important stages in the introduction of a new medicinal product or substance into medical practice is the development of quality control techniques.The aim. The aim of this work was to develop methods of identification, determination of impurities and quantitative determination of N- (5-ethyl- [1,3,4] -thiadiazole-2-yl)-2-nitrobenzamide for further application in standardization of the substance.Methods. Chromatographically pure sample of N- (5-ethyl- [1,3,4] -thiadiazole-2-yl) -2-nitrobenzamide, methods of IR, UV and 1H NMR spectroscopy.Results. The physical-chemical properties and spectral characteristics of N-(5-ethyl-[1,3,4]-thiadiazole-2-yl)-2-nitrobenzamide were studied, and chemical identification methods were proposed. The optimal conditions for the determination of the impurities by the method of thin-layer chromatography using the method of internal normalization are selected. The assay for N- (5-ethyl- [1,3,4] -thiadiazol-2-yl) -2-nitrobenzamide was carried out by absorption spectrophotometry in the alcohol solution at the wavelength of 282 nm with the absorption index 631. For application of methods such validation characteristics as robustness, linearity, correctness, stability of analytical solutions, precision, convergence, reproducibility, calculation of uncertainty of samples preparation were studied.Conclusions. The methods of identification of N- (5-ethyl- [1,3,4] -thiadiazol-2-yl) -2-nitrobenzamide with the use of chemical reactions and spectral methods of analysis - IR and UV and 1H NMR spectroscopy have been developed. To determine the concomitant impurities in the substance, the TLC method is recommended. Specific and nonspecific impurities were determined. The method of quantitative determination of substance by absorption spectrophotometry method in the ultraviolet region by the method of specific absorption index have been developed
Highlights
Derivatives of 1,3,4-thiadizole, which contain various substituents of the aliphatic, aromatic and heterocyclic series at C2 and C5 atoms of the 1,3,4-thiadiazole cycle are a promising class of biologically active substances, as evidenced by extensive scientific work both domestic and foreign scholars
For preparation of the implementation of a substance, we have developed the methods of identification, tests for purity and quantitative analysis of the perspective anticonvulsant N- (5-ethyl- [1,3,4] -thiadiazol-2-yl) 2-nitrobenzamide
Spectrum 1Н NMR of N- (5-ethyl- [1,3,4] thiadiazol-2-yl) -2-nitrobenzamide acid contains all signals of hydrogen containing groups which are characteristic for this substance, so the 1H NMR data can be recommended for introduction in the project of quality control methods [12]
Summary
Попередніми дослідженнями вчених НФАУ доведена перспективність пошуку потенційних антиконвульсантів в ряду похідних 1,3,4-тіадіазолу[1,2,3]. Метою даної роботи була розробка методик ідентифікації, визначення домішок та кількісного визначення N-(5-етил-[1,3,4]-тіадіазол-2-іл)-2-нітробензаміду з метою подальшого застосування в стандартизації субстанції. Хроматографічно чистий зразок N-(5-етил-[1,3,4]-тіадіазол-2-іл)-2-нітробензаміду, методи ІЧ-, УФ- та 1Н ЯМР спектроскопії. Вивчено фізико-хімічні властивості і спектральні характеристики N-(5-етил-[1,3,4]тіадіазол-2-іл)-2-нітробензаміду, запропоновано хімічні методи ідентифікації. Розроблено методи ідентифікації N- (5-етіл- [1,3,4] -тіадіазол-2-іл) -2-нітробензаміду з використанням хімічних реакцій і спектральних методів аналізу - ІЧ і УФ та 1Н ЯМР -спектроскопії. Для визначення супутніх домішок в субстанції рекомендований метод ТШХ. Розроблено методику кількісного визначення субстанції методом абсорбційної спектрофотометрії в ультрафіолетовій ділянці методом питомого показника поглинання. Ключові слова: фармацевтичний аналіз, ідентифікація, кількісне визначення, домішки, спектроскопія, тонкошарова хроматографія антиконвульсант
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