VALIDATION OF HPLC METHOD FOR THE DETERMINATION OF RIVAROXABAN FOR COMPARATIVE EXTRACTION IN STUDYING THE DELIVERY OF THE DRUG VIA NASOGASTRIC TUBE IN VITRO.
A new coordination compound of Ni(II) with cyclohexylacetoacetate and N,N-diethylnicotinamide was synthesized and characterized by IR spectroscopy and X-ray analysis. The IR spectrum exhibits intense broad absorption bands corresponding to the stretching vibrations of the C=O and C=C bonds conjugat...
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| Дата: | 2026 |
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| Автори: | , , , , , |
| Формат: | Стаття |
| Мова: | Англійська |
| Опубліковано: |
V.I.Vernadsky Institute of General and Inorganic Chemistry
2026
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| Онлайн доступ: | https://ucj.org.ua/index.php/journal/article/view/767 |
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| Назва журналу: | Ukrainian Chemistry Journal |
Репозитарії
Ukrainian Chemistry Journal| _version_ | 1861952645695012864 |
|---|---|
| author | Yegorova , A. Sysenko , O. Skrypynets , Yu. Chebotarska , I. Aleksandrova , D. Kashutskуy , S. |
| author_facet | Yegorova , A. Sysenko , O. Skrypynets , Yu. Chebotarska , I. Aleksandrova , D. Kashutskуy , S. |
| author_sort | Yegorova , A. |
| baseUrl_str | https://ucj.org.ua/index.php/journal/oai |
| collection | OJS |
| datestamp_date | 2026-04-08T12:23:19Z |
| description | A new coordination compound of Ni(II) with cyclohexylacetoacetate and N,N-diethylnicotinamide was synthesized and characterized by IR spectroscopy and X-ray analysis. The IR spectrum exhibits intense broad absorption bands corresponding to the stretching vibrations of the C=O and C=C bonds conjugated within the chelate ring (1625, 1502 cm⁻¹), as well as other absorption bands characteristic of β-dicarbonyl complexes, in particular a sharp band at 775 cm⁻¹ attributed to the out-of-plane bending vibration of the C–H bond in the chelate ring. In the high-frequency region of the spectrum, there are signals of stretching vibrations of the C-H bonds of alkyl groups (2855–2990 cm–1) and weak signals of stretching vibrations of the C-H of the pyridine ring (3080–3110 cm–1). The absorption bands of the amide group (νС=О 1620–1650 cm–1) and the pyridine ring (νС=С, νС=N 1500–1600 cm–1) of N,N‑diethylnicotinamide overlap with the vibration bands of the chelate rings and cannot be unambiguously assigned. The medium-intensity band at 1300 cm⁻¹, present in both the free ligand and the complex, is assigned to C–N stretching vibrations of the amide group. The low-intensity bands in the 600–400 cm⁻¹ region are assigned to Ni–N and Ni–O vibrations. According to X-ray data, the crystal system of NiL2NK2 complex is monoclinic, space group P21/с, a = 7.0360(15) Å, b = 13.233(4) Å, c = 23.619(5) Å, α = γ = 90º,  β = 93.301(12)º. The structure corresponds to the formula [Ni(C10H15O3)2(C10H14N2O)2] and represents a mononuclear complex located in a special position relative to the inversion center. The central Ni atom has a O4N2 distorted octahedral environment. The axial positions of the coordination polyhedron are occupied by the nitrogen atoms of the pyridine ring of N,N‑diethylnicotinamide. The molecules of chelating ligands, coordinated through oxygen atoms, occupy an equatorial position with a trans configuration relative to each other. In the crystal, the complex molecules are bound by weak C-H…π interactions and form layers in the (001) plane, alternating with each other. The structure of the coordination polyhedron of the described compound is similar to the structure of adducts of β-dicarbonyl complexes of d‑metals with pyridine. |
| first_indexed | 2026-04-09T01:00:16Z |
| format | Article |
| id | oai:ojs2.1444248.nisspano.web.hosting-test.net:article-767 |
| institution | Ukrainian Chemistry Journal |
| keywords_txt_mv | keywords |
| language | English |
| last_indexed | 2026-04-09T01:00:16Z |
| publishDate | 2026 |
| publisher | V.I.Vernadsky Institute of General and Inorganic Chemistry |
| record_format | ojs |
| spelling | oai:ojs2.1444248.nisspano.web.hosting-test.net:article-7672026-04-08T12:23:19Z VALIDATION OF HPLC METHOD FOR THE DETERMINATION OF RIVAROXABAN FOR COMPARATIVE EXTRACTION IN STUDYING THE DELIVERY OF THE DRUG VIA NASOGASTRIC TUBE IN VITRO. Yegorova , A. Sysenko , O. Skrypynets , Yu. Chebotarska , I. Aleksandrova , D. Kashutskуy , S. nickel, β-dicarbonyl complexes, cyclohexyl acetoacetate, N,N-diethylnicotinamide, crystal structure. A new coordination compound of Ni(II) with cyclohexylacetoacetate and N,N-diethylnicotinamide was synthesized and characterized by IR spectroscopy and X-ray analysis. The IR spectrum exhibits intense broad absorption bands corresponding to the stretching vibrations of the C=O and C=C bonds conjugated within the chelate ring (1625, 1502 cm⁻¹), as well as other absorption bands characteristic of β-dicarbonyl complexes, in particular a sharp band at 775 cm⁻¹ attributed to the out-of-plane bending vibration of the C–H bond in the chelate ring. In the high-frequency region of the spectrum, there are signals of stretching vibrations of the C-H bonds of alkyl groups (2855–2990 cm–1) and weak signals of stretching vibrations of the C-H of the pyridine ring (3080–3110 cm–1). The absorption bands of the amide group (νС=О 1620–1650 cm–1) and the pyridine ring (νС=С, νС=N 1500–1600 cm–1) of N,N‑diethylnicotinamide overlap with the vibration bands of the chelate rings and cannot be unambiguously assigned. The medium-intensity band at 1300 cm⁻¹, present in both the free ligand and the complex, is assigned to C–N stretching vibrations of the amide group. The low-intensity bands in the 600–400 cm⁻¹ region are assigned to Ni–N and Ni–O vibrations. According to X-ray data, the crystal system of NiL2NK2 complex is monoclinic, space group P21/с, a = 7.0360(15) Å, b = 13.233(4) Å, c = 23.619(5) Å, α = γ = 90º,  β = 93.301(12)º. The structure corresponds to the formula [Ni(C10H15O3)2(C10H14N2O)2] and represents a mononuclear complex located in a special position relative to the inversion center. The central Ni atom has a O4N2 distorted octahedral environment. The axial positions of the coordination polyhedron are occupied by the nitrogen atoms of the pyridine ring of N,N‑diethylnicotinamide. The molecules of chelating ligands, coordinated through oxygen atoms, occupy an equatorial position with a trans configuration relative to each other. In the crystal, the complex molecules are bound by weak C-H…π interactions and form layers in the (001) plane, alternating with each other. The structure of the coordination polyhedron of the described compound is similar to the structure of adducts of β-dicarbonyl complexes of d‑metals with pyridine. V.I.Vernadsky Institute of General and Inorganic Chemistry 2026-03-25 Article Article Аналітична хімія application/pdf https://ucj.org.ua/index.php/journal/article/view/767 Ukrainian Chemistry Journal; Vol. 92 No. 2 (2026): Ukrainian Chemistry Journal; 13-25 Украинский химический журнал; Том 92 № 2 (2026): Ukrainian Chemistry Journal; 13-25 Український хімічний журнал; Том 92 № 2 (2026): Ukrainian Chemistry Journal; 13-25 2708-129X 2708-1281 en https://ucj.org.ua/index.php/journal/article/view/767/401 |
| spellingShingle | Yegorova , A. Sysenko , O. Skrypynets , Yu. Chebotarska , I. Aleksandrova , D. Kashutskуy , S. VALIDATION OF HPLC METHOD FOR THE DETERMINATION OF RIVAROXABAN FOR COMPARATIVE EXTRACTION IN STUDYING THE DELIVERY OF THE DRUG VIA NASOGASTRIC TUBE IN VITRO. |
| title | VALIDATION OF HPLC METHOD FOR THE DETERMINATION OF RIVAROXABAN FOR COMPARATIVE EXTRACTION IN STUDYING THE DELIVERY OF THE DRUG VIA NASOGASTRIC TUBE IN VITRO. |
| title_full | VALIDATION OF HPLC METHOD FOR THE DETERMINATION OF RIVAROXABAN FOR COMPARATIVE EXTRACTION IN STUDYING THE DELIVERY OF THE DRUG VIA NASOGASTRIC TUBE IN VITRO. |
| title_fullStr | VALIDATION OF HPLC METHOD FOR THE DETERMINATION OF RIVAROXABAN FOR COMPARATIVE EXTRACTION IN STUDYING THE DELIVERY OF THE DRUG VIA NASOGASTRIC TUBE IN VITRO. |
| title_full_unstemmed | VALIDATION OF HPLC METHOD FOR THE DETERMINATION OF RIVAROXABAN FOR COMPARATIVE EXTRACTION IN STUDYING THE DELIVERY OF THE DRUG VIA NASOGASTRIC TUBE IN VITRO. |
| title_short | VALIDATION OF HPLC METHOD FOR THE DETERMINATION OF RIVAROXABAN FOR COMPARATIVE EXTRACTION IN STUDYING THE DELIVERY OF THE DRUG VIA NASOGASTRIC TUBE IN VITRO. |
| title_sort | validation of hplc method for the determination of rivaroxaban for comparative extraction in studying the delivery of the drug via nasogastric tube in vitro. |
| topic_facet | nickel β-dicarbonyl complexes cyclohexyl acetoacetate N,N-diethylnicotinamide crystal structure. |
| url | https://ucj.org.ua/index.php/journal/article/view/767 |
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