Development and Validation of a High-Performance Thin-Layer Chromatographic Method,with Densitometry,for Quantitative Analysis of Tizoxanide (a Metabolite of Nitazoxanide) in Human Plasma

JPC – Journal of Planar Chromatography – Modern TLC - A new simple, rapid, and selective high-performance thin-layer chromatographic (HPTLC) method with metronidazole as the internal...     

Subbundles of maximal degree of the normal bundle of algebraic space curves almost complete intersection of special type

Summary LetX⊂P ³ be an irreducible smooth curve which is not a complete intersection. The main result of this paper shows that whenX is an a.c.i. of special type, i.e. its homogeneous ideal is generated by three polynomial of the same degreem, and additionallym>2, the subbundles of maximal degree of the normal bundle ofX inP ³ correspond to the singular points of maximal multiplicity of a plane curve which is the image ofX by a map (the linear system of the surfaces of minimal degree throughX). In particular this normal bundle is stable. The initial case of this family of curves, i.e. form=3, has been studied by E. Ballico-Ph. Ellia with different methods.

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Riassunto SiaX⊂P ³ una curva irriducibile e liscia che non è una completa intersezione. Il risultato principale di questa Nota mostra che quandoX è una almost completa intersezione di tipo speciale, cioè il suo ideale omogeneo è generato minimamente da 3 polinomi dello stesso gradom, e, inoltre,m>2, i sottofibrati di grado massimo del fibrato normale diX inP ³ corrispondono ai punti singolari di molteplicità massima di una curva piana che è l’immagine diX tramite una mappa (il sistema lineare delle superficie di grado minimo passanti perX). In particolare questo fibrato normale è stabile. Il caso iniziale di questa famiglia di curve, i.e. perm=3, è stato studiato da E. Ballico-Ph. Ellia con differenti metodi.

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This research is supported by GNSAGA (Italy).

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The main results of this paper have been the object of a talk at the meeting on ?Curves in Projective Space? held at Rocca di Papa in june 1985.     

Nickel-Ruthenium Mixed-Metal Carbonyl Clusters Syntheses and Solid State Structures of the Two Tetrahedral Clusters [PPh4][NiRu3(μ3 H)(CO)9(μ-CO)3] and [NEt4]2[NiRu3(CO)8(μ-CO)4]

Redox condensation of [Ru₃H(CO)₁₁]- with Ni(CO)₄, in tetrahydrofuran solution, under a nitrogen atmosphere, yields the tetranuclear anion [NiRu_H(CO)₁₁)-. Subsequent deprotonation with Bu'OK in acetonitrile solution leads to the formation of the related dianion. Both anions have been characterized by spectroscopic techniques, elemental analysis and single crystal X-ray diffraction. [PPh₄][NiRu₃H(CO)₁₂] crystallizes in the triclinic space group PI with unit cell dimensionsof a = 11.842(2) Å,b = 12.335(3) Å, c = 13.3080) Å,a = 91.89(2)°, = 93.35(1)°,y = 96.41(2)°, Z = 2, V= 1926.9(7) Å'. The NiRu₃, metal core of the molecule defines a distorted tetrahedron with nine terminal and three edge bridging carbonyl groups. The hydrido ligand was located by difference Fourier techniques and was found to bridge the NiRu₂ basal triangle at a distance of 0.88(6) A from this plane. Selected average distances and angles are: Ru-Ru = 2.839 Å, Ru-Ni = 2.640 Å, Ru-C, = 1.910 A,Ru-C _b = 2.084 Å, Ni-C _b = 2.022 Å, Ru-H = 1.77 Å, C-0, = 1.135 Å, C-O _b = 1.159 Å, M-C-O, = 176.3°,M-C--O _b = 139.3°;other distances are: Ni-C₁ = l.758(7) Å, Ni-H= 1.85(7) Å. [NEt₄]₂[NiRu₃(CO)₁₂] crystallizes in the orthorhombic space group Pnma (no. 62) with unit cell dimensions ofa=20.247(5) Å,b = 15.038(4)Å,c = 12.079(3) Å, Z=4, V=3678(2) A'. The molecule contains a tetrahedral NiRu₃ core with eight terminal and four edge bridging carbon monoxide groups which bridge the three Ni-Ru and one Ru-Ru bond. Average distances and angles are: Ru -Ru =2.3050A Ru-Ni 2.648 Å, Ru-C _t = 1.878 Å, Ru-C _b 2.045 Å, Ni-C _b = 2.055 Å, C-O _t = 1.145 Å, C-01,=1.157 Å, M-C-O,= 176.9°, M-C-O _b = 138.6°; other distance is: Ni-C _t = 1.754(10) Å,t = terminal,b = bridging.     

Pyridazine derivatives. Part 40: Reactivity of 5-alkynylpyridazin-3(2H)-ones toward hydrochloric acid

5-Alkynylpyridazin-3(2H)-ones or 5-(2-chloroalkenyl)pyridazin-3(2H)-ones were isolated during the cleavage of the methoxymethyl group in a series of 5-alkynyl-2-methoxymethylpyridazin-3(2H)-ones by treatment with hydrochloric acid. The efficient and selective cleavage of the methoxymethyl group in these compounds can be performed under mild conditions by employing aluminium chloride.     

Optical sensors based on hybrid DNA/conjugated polymer complexes

Single-stranded DNA (ss-DNA) can specifically bind to various targets, including a complementary ss-DNA, ions, proteins, drugs, and so forth. When binding takes place, the oligonucleotide probe often undergoes a conformational transition. This conformational change of the negatively charged ss-DNA can be detected by using a water-soluble, cationic polythiophene derivative, which transduces the complex formation into an optical (colorimetric or fluorometric) signal without any labeling of the probe or the target. This simple and rapid methodology has enabled the specific and sensitive detection of nucleic acids and human thrombin. This new biophotonic tool can easily be applied to the detection of various other biomolecules and is also useful in the high-throughput screening of new drugs.     

A Two‐Dimensional Coordination Compound as a Zinc Ion Selective Luminescent Probe for Biological Applications

A 2D coordination compound {[Cu₂(HL)(N₃)]?ClO₄}_∞ ( 1 ; H₃L=2,6‐bis(hydroxyethyliminoethyl)‐4‐methyl phenol) was synthesized and characterized by single‐crystal X‐ray diffraction to be a polymer in the crystalline state. Each [Cu₂(HL)(N₃)]⁺ species is connected to its adjacent unit by a bridging alkoxide oxygen atom of the ligand to form a helical propagation along the crystallographic a axis. The adjacent helical frameworks are connected by a ligand alcoholic oxygen atom along the crystallographic b axis to produce pleated 2D sheets. In solution, 1 dissociates into [Cu₂(HL)₂(H₃L)]?2H₂O ( 2 ); the monomer displays high selectivity for Zn²⁺ and can be used in HEPES buffer (pH 7.4) as a zinc ion selective luminescent probe for biological application. The system shows a nearly 19‐fold Zn²⁺‐selective chelation‐enhanced fluorescence response in the working buffer. Application of 2 to cultured living cells (B16F10 mouse melanoma and A375 human melanoma) and rat hippocampal slices was also studied by fluorescence microscopy.     

Darstellung und Eigenschaften von Chromtricarbonyl-Komplexen strukturisomerer Borazin-Derivate

The new hexaalkylborazine chromium tricarbonyls (n-Pr)₃B₃N₃Me₃Cr(CO)₃ (V), Me₃B₃N₃(n-Pr)₃Cr(CO)₃ (VI), (i-Pr)₃B₃N₃Me₃Cr(CO)₃ (VII) and Me₃B₃N₃(i-Pr)₃Cr(CO)₃ (VIII) have been prepared from fac-Cr(CO)₃(MeCN)₃ and the corresponding borazine in dioxane or without solvent. They are much more labile than the isomeric complex Et₃B₃N₃Et₃Cr(CO)₃ (IV) which can be readily obtained from Et₃B₃N₃Me₃Cr(CO)₃ and Et₃B₃N₃Et₃ by ring ligand exchange. The NMR., IR., UV. and Mass spectroscopic data of the complexes IV–VIII will be briefly discussed. The preparation of the borazine derivatives (n-Pr)₃B₃N₃Me₃ (IX) and Me₃B₃N₃(n-Pr)₃ (X) is also reported.     

Asymmetric synthesis by chiral ruthenium complexes : VI. Enantiomer-discrimination in the hydrogen transfer from racemic alcohols to prochiral ketones in the presence of H4Ru4(CO)8[(−)-diop]2

Hydrogen transfer from racemic alcohols to prochiral ketones in the presence of H₄Ru₄(CO)₈[(?)-DIOP]₂ has been examined. The enantiomer-discrimination is influenced by the structure of the reactants, temperature and the excess of phosphine present.     

Total synthesis of (±)-cyclooroidin

The first total synthesis of (±)-cyclooroidin, a member of the pyrrole-imidazole alkaloid family recently isolated from the sponge Agelas oroides in optically pure form, is described. The synthesis was achieved in nine linear steps, with an overall yield of 10%. Key step was a Wolff bromoketone synthesis performed on the intermediate longamide B.     

Mössbauer study of LaNiSn and NdNiSn compounds and their deuterides

Summary LaNiSn and NdNiSn compounds and their deuterides have been studied by variable temperature ¹¹⁹Sn M?ssbauer spectroscopy. The hyperfine parameters obtained experimentally are in good agreement with those derived from first principle calculations. The enlargement of quadrupole splitting observed for LaNiSn after deuteration confirms the lower symmetry of electron density around tin atoms indicated by the calculation of partial Sn-p density of states (DOS). Magnetic ordering is observed at low temperature in deuterided NdNiSn.