Validated ecofriendly chromatographic method for quantitative determination of anti‐migraine quaternary mixture

A novel ecofriendly, cost and time saving high‐performance thin‐layer chromatographic method was developed and validated for simultaneous determination of metoclopramide, ergotamine, caffeine, and paracetamol in bulk and pharmaceutical formulation. The separation was carried out on silica gel plates, using ethyl acetate:ethanol:ammonia (9:1:0.1, v/v/v) as a developing system. Ultraviolet detection was carried out at 272 nm. The resulting retention times were 0.15, 0.36, 0.49, and 0.74 min for metoclopramide, ergotamine, caffeine, and paracetamol, respectively. The greenness profile assessment was achieved to the proposed method to evaluate its greenness characters to the environment with acceptable results. Validation parameters were checked according to International Conference of Harmonization guidelines to achieve the international requirements for quality control analysis of the proposed drugs.     

Synthesis,characterization, and biological investigation of new mixed-ligand complexes

A novel series of mixed-ligand complexes of 5,5′-{(1E,1E′)-1,4-phenelynebis(diazene-2,1-diyl)}bis(quinolin-8-ol) (H₂L₁) as a primary ligand and 4-aminoantipyrine(L₂) as a secondary ligand with Mn(II) ion were prepared using two general formulae: [Mn₂(H₂L₁)₂(L₂)₂X₄].4Cl (X = OH₂( 1 ), ONO₂⁻( 2 ), Cl=nil; OAc( 3 ), Cl = nil) and [Mn₂(H₂L₁)(L₂)₂(O₂SO₂)₂]( 4 ). Free ligands and their complexes were characterized. Electronic absorption spectra of the mixed-ligand complexes indicate a distorted octahedral geometry around the central metal ion, and the anions X⁻ are in the axial positions for all compounds. The ligands behave in a neutral bidentate manner, through nitrogen atoms and oxygen atoms of the carbonyl group (L₂), whereas H₂L₁ coordinated through nitrogen and OH groups as a neutral bidentate ligand. All complexes do not contain coordinated water molecules, but complex ( 1 ) contains four water molecules. The water molecules are removed in a single step. The complexes exhibited magnetic susceptibility corresponding to five unpaired electrons. The antimicrobial activity of the Mn(II) mixed-ligand complexes ( 1–4 ) against two gram-positive bacteria, three local gram-negative bacteria, and three fungi species was tested. Mn(II) mixed-ligand complex ( 2 ) exhibited significant antibacterial activity against Bacillus cereus, Staphylococcus aureus, Escherichia coli, Klebsiella pneumoniae, and Pseudomonas sp. Mixed-ligand complex ( 2 ) exhibited a high potential cytotoxicity against the growth of human lung cancer cells.     

Volatiles and Antifungal-Antibacterial-Antiviral Activity of South African Salvia spp. Essential Oils Cultivated in Uniform Conditions

Spontaneous emissions of S. dentata Aiton and S. scabra Thunb., as well as the essential oil (EO) composition of the cited species, together with S. aurea L., were investigated. The chemical profile of the first two species is reported here for the first time. Moreover, in vitro tests were performed to evaluate the antifungal activity of these EOs on Trichophyton mentagrophytes, Microsporum canis, Aspergillus flavus, Aspergillus niger, and Fusarium solani. Secondly, the EO antibacterial activity against Escherichia coli, Staphylococcus aureus, and Staphylococcus pseudointermedius was examined, and their antiviral efficacy against the H1N1 influenza virus was assessed. Leaf volatile organic compounds (VOCs), as well as the EOs obtained from the arial part of Salvia scabra, were characterized by a high percentage of sesquiterpene hydrocarbons (97.8% and 76.6%, respectively), mostly represented by an equal amount of germacrene D (32.8% and 32.7%, respectively). Both leaf and flower spontaneous emissions of S. dentata, as well as the EO composition, showed a prevalence of monoterpenes divided into a more or less equal amount of hydrocarbon and oxygenated compounds. Interestingly, its EO had a non-negligible percentage of oxygenated sesquiterpenes (29.5%). S. aurea EO, on the contrary, was rich in sesquiterpenes, both hydrocarbons and oxygenated compounds (41.5% and 33.5%, respectively). S. dentata EO showed good efficacy (Minimal Inhibitory Concentration (MIC): 0.5%) against M. canis. The tested EOs were not active against E. coli and S. aureus, whereas a low inhibition of S. dentata EO was observed on S. pseudointermedius (MIC = 10%). Once again, S. dentata EO showed a very good H1N1 inhibition; contrariwise, S. aurea EO was completely inactive against this virus. The low quantity of S. scabra EO made it impossible to test its biological activity. S. dentata EO exhibited interesting new perspectives for medicinal and industrial uses.     

Synthesis and structure determination of a new layered zincophosphate: [H2N2C6H16]0.5[Zn2(PO4)(HPO4)(H2O)]·H2O

The synthesis and crystal structure of a new microporous zincophosphate are described. [H₂N₂C₆H₁₆]_0.5[Zn₂(PO₄)(HPO₄)(H₂O)]·H₂O crystallizes in the triclinic space group P1¯ with a = 8.822(4), b = 9.236(4), c = 8.451(3) Å, = 67.19(3), = 91.32(3), = 111.10(3)°, V = 586.7(4) ų and Z = 2. This new material consists of infinite two-dimensional anionic layers alternated with planes containing organic diprotonated templates, N, N, N, N-tetramethylethylenediamine [H₂N₂C₆H₁₆]²⁺ molecules. The framework structure is built up of ZnO₄, ZnO₃OH₂, PO₄, and PO₃OH tetrahedra, linked through oxygen vertices. The presence of terminal OH₂ and OH groups, leads to an open structure containing four- and eight-rings. The organic molecules are interconnected to the framework through hydrogen bonds.     

A Convenient Synthesis of Some New 1,3,4‐Thiadiazoles,Thiazoles, Pyrazolo[1,5‐a]pyrimidines,Pyrazolo[5,1‐c]triazine,and Thieno[3,2‐d]pyrimidines Containing 5‐Bromobenzofuran Moiety

1,3,4‐Thiadiazoles, pyrazolo[1,5‐a]pyrimidines, pyrazolo[5,1‐c]triazine, and thieno[3,2‐d]pyrimidines were synthesized from 1‐(5‐bromobenzofuran‐2‐yl)ethanone. The structures of the newly synthesized compounds were elucidated by elemental analysis, spectral data, chemical transformation, and alternative synthesis route whenever possible.     

Useful Precursors for Synthesis of Some New Azolo[3,4‐d]pyridiazines,Azolo[1,5‐a]pyrimidines,Azolo[5,1‐c]triazines,Pyrazoles, and Benzo[b][l,4]diazepine

Pyrazolo[3,4‐d]pyridazines, isoxazolo[3,4‐d]pyridazines, azolo[1,5‐a]pyrimidines, azolo[5,1‐c]triazines, pyrazoles, and benzo[b][l,4]diazepine were synthesized from the appropriate hydrazonoyl halides, hydroximoyl halides, heterocyclic amines, diazotized heterocyclic amines, arenediazonium chlorides, and o‐phenylenediamines with appropriate of sodium 3‐(5‐bromobenzofuran‐2‐yl)‐3‐oxoprop‐1‐en‐1‐olate or 1‐(5‐bromobenzofuran‐2‐yl)‐3‐(dimethylamino)prop‐2‐en‐1‐one. The newly synthesized compounds were elucidated by elemental analyses, spectral data, and alternative synthesis whenever possible.     

Purple subphthalocyanine-phthalocyanine dyad: Synthesis,photophysicochemical properties and DFT study

A new phthalocyanine-subphthalocyanine heterodyad ( 5 ) was prepared by Pd(0)-catalyzed Sonogashira coupling reaction between an asymmetrical phthalocyanine ( 3 ) bearing monoiodo and multiple triazolide moieties on its backbone and a subphthalocyanine ( 4 ) bearing axially propargyl group. The structure of this heterodyad ( 5 ) was subsequently confirmed by the conventional spectroscopic techniques. The photophysical and photochemical properties including; fluorescence and singlet oxygen generation of ( 5 ) along with its building chromophores ( 3 ) and ( 4 ) were also investigated. Interestingly, a purple colored solution was observed by this novel dyad which was significantly different from those colors (green or blue) obtained by phthalocyanine-subphthalocyanine conjugates. Based on steady state absorption spectroscopic data and transient absorption results, the synthesized dyad 5 was free of aggregation and there is good energy transfer occurs between Pc and subPc moieties. This result was confirmed using density functional theory (DFT) and time-dependent DFT (TDDFT) analyses: B3LYP exchange-correlation functional and the 6–31 + G(d) basis set.     

Salvia broussonetii Benth.: aroma profile and micromorphological analysis

The volatile profiles (VOC) and the essential oil (EO) composition from the aerial parts of Salvia broussonetii were analysed. Sesquiterpene hydrocarbons dominate the VOCs from leaves (95.7%) and flowers (67.6%), followed by monoterpene hydrocarbons (2.6 and 29.7%, respectively). The main common compounds are germacrene D, β-bourbonene, α-pinene, α-copaene and α-gurjunene, even if with divergent relative abundances. In the leaf EOs the sesquiterpenes prevail, even if not overwhelmingly (about 50.0%), followed by monoterpenes (23.0–35.0%) and by minor fractions of diterpene hydrocarbons and non-terpene derivates. The most abundant common compounds across the two sampling periods are α-pinene, β-pinene, isobornyl acetate, α-gurjenene, germacrene D and bifloratriene. A morphological characterisation of the trichomes responsible for the productivity in terpenes was also performed. Four different morphotypes were observed on the above ground organs of S. brussonetii: peltates and capitates of type II and III resulted the only producers of volatile substances.     

The liquid structure of the solvents dimethylformamide (DMF) and dimethylacetamide (DMA)

The liquid structure of the commonly used solvents dimethylformamide (DMF) and dimethylacetamide (DMA)were measured using state-of-the-art state neutron diffraction augmented with isotopic substitution (NDIS) and interpreted with empirical potential structure refinement (EPSR). Both solvents are found to develop rich local ordering with similar local packing densities, though with differences related to their three-dimensional molecular structure. While DMF’s dipole preferentially orientates anti-parallel to maximise hydrogen bonding, DMA favours parallel arrangement maximising non-directional dispersive forces. The highly-developed local orientational structure found in these solvents rationalises their ability to solvate a range of charged and neutral nanomaterials and highlights that the understanding of nanomaterial dispersions is a multi-body problem in which the geometry of the molecule, as well its dipole moment, must be incorporated.     

The solid state reaction between lanthanum oxide and strontium carbonate

The reaction between lanthanum oxide and strontium carbonate was studied non-isothermally between 350 and 1150 °C at different heating rates, intermediates and the final solid product were characterized by X-ray diffractometry (XRD). The reaction proceeds through formation of lanthanum oxycarbonate La₂O(CO₃)₂, lanthanum dioxycarbonate La₂O₂CO₃, and non-stoichiometric strontium lanthanum oxide La₂SrO_x (x = 4 + δ). La₄SrO₇ was found to be the final product which begins to form at ∼700 °C. Li⁺ doping enhances the formation of the final product as well as commencement of the reactions at lower temperatures.