Carbon-13 NMR Spectra Research Articles

Sonochemical synthesis, characterization, and ADMET studiesof Fe (II) and Cu (II) nano-sized complexes of trimethoprim

Nanoparticles exhibit distinct physical and chemical characteristics and are becoming increasingly significant in the production of innovative nanodevices for many applications in physics, biology, biomedicine, and pharmaceuticals. The aim of this research work is to synthesize Fe (II) and Cu (II) nano-sized complexes of trimethoprim (TMP) using the sonication method, characterize them using physical and spectroscopic methods, and carry out ADMET studies on the synthesized complexes. The spectroscopic and physical studies showed a change in colour and an increase in melting point due to coordination. The novel compounds were slightly soluble in water. The XRD tests revealed that the new nanocomplexes were crystalline. The Fe (II) nanocomplexes had a size of 57.56 nm and the Cu (II) nanocomplexes had a size of 69.88 nm. These values were found using Debye-Scherrer’s equation. The FTIR results of the TMP, Fe (II), and Cu (II) nanometal complexes showed a shift of the amino group band from 3317 to 3295 and 3202 cm?1 and the azomethine band from 1633 to 1625 and 1592 cm?1 in the complexes. In the complexes, the proton NMR spectra revealed an upfield shift of the amine proton. The carbon-13 NMR spectra showed that CH2 was involved in coordination with the metal ions. The spectra studies indicated that TMP coordinated with the metal ions through the methylene and amino groups. A trigonal bipyramid structure was proposed for the complexes. The results of the Rule of 5 studies indicated that the test compounds had a good drug-likeness prediction, with only one violation. The ADMET prediction showed that all of the compounds demonstrated improved pharmacokinetic characteristics and adhered to the RO5 requirement. These findings highlight the therapeutic potential of Fe (II) and Cu (II) nano-sized TMP complexes as bioactive compounds that warrant further investigation for pharmaceutical applications.

Synthesis, characterization, and investigation of catalytic properties of RuII complexes with Schiff bases based on 2-hydroxybenzaldehyde and 5-bromo-2-hydroxybenzaldehyde

Pursuing our recent interest concerning the catalytic activity of half-sandwich RuII complexes containing Schiff base ligands (L1 and L2), in this study new Schiff bases and their half-sandwich RuII complexes were prepared. The structures of these compounds were confirmed by a variety of spectral and physical methods such as microanalysis, FT-IR, electronic spectra, proton and carbon NMR, TGA and mass spectra. The catalytic activities of the RuII complexes toward the transfer hydrogenation of ketones to their corresponding alcohols were investigated using i-PrOH as a hydrogen source and solvent. The complexes showed high catalytic activities at catalyst concentrations of 0.01 mmol and were able to carry out transfer hydrogenation (TH) to a wide range of ketones in the presence of KOH. In general, Schiff bases recognition, the coordination chemistry, and the ketone substrates were found to influence the catalytic performance of these complexes.

Diisopropylammonium hydrogen squarate: Synthesis and comprehensive analysis of non-linear optical co-crystal using X-ray, Hirshfeld, mechanical, optical and DFT methods

This research successfully synthesized a single co-crystal of diisopropylammonium hydrogen squarate using prolonged vaporization for crystal growth. Single-crystal X-ray spectrometry confirmed its monoclinic structure, and morphological predictions were made. UV–visible spectroscopy revealed its optical transmittance with a direct optical energy band gap of 3.45 eV. Photoluminescence studies showed a strong violet emission at 402 nm when excited by a 260 nm source. Microhardness study examined the crystal's mechanical attributes portraying the normal indentation size effect followed by a qualitative overview of half-penny crack dynamics. FTIR study aided in the discernment of varied vibrational modes with NH stretching being observed at 3078 cm−1. Thermal examination further revealed the crystal's stability up till 244 °C. Proton and carbon-13 NMR spectra were analyzed to verify the presence of functional groups and the overall molecular integrity. Intermolecular interactions were analyzed using Hirshfeld surface and fingerprint mapping. The Z-scan technique demonstrated the crystal's applicative potential in its third harmonic generation capability. Theoretical calculations with Density Functional Theory (DFT) supported the experimental findings, offering insights into optimized geometries, frontier molecular orbitals, natural population and bond orbital distributions, hyperpolarizability, molecular electrostatic potentials, IR vibrational modes, and UV absorbance profiles.

Sonochemical synthesis and characterization of Fe(II) and Cu(II) nano-sized complexes of sulfamethoxazole

Nanoparticle drug delivery systems are precisely designed technologies that utilize nanoparticles to deliver therapeutic drugs to specific targets and regulate their release. In recent times, nanoparticles have garnered significant interest owing to their potential for efficient drug delivery. This work is aimed at synthesizing Fe(II) and Cu(II) nano-sized complexes of sulfamethoxazole (SMX) using the sonication method. The physical and spectroscopic studies showed a colour change from white to grey, and a decrease in melting points suggested the formation of the metal complexes. The nanometal complexes were insoluble in water. XRD analysis showed that the crystallite sizes of Fe(II) and Cu(II) nanometal complexes were determined to be 76.08 nm and 37.13 nm, respectively, using the Debye-Scherrer equation. The FTIR results of the SMX, Fe(II), and Cu(II) nanometal complexes showed a shift of the amine band from 3243 to 3191 cm^-1 and the sulfone band from 1154 to 1092 cm^-1 in both complexes. The proton NMR showed a shift of the amine proton from 6.100 ppm to 6.035 ppm in the spectra of the Cu(II) complex. The amine chemical shift was absent in the spectra of the Fe(II) complex, showing deprotonation. The carbon-13 NMR spectra showed a similar chemical shift. The spectra studies indicated that SMX coordinated with the metal ions through the amino and sulfone groups. A tetrahedral structure was proposed for the complexes. SMX coordinated as a bidentate ligand to Fe(II) and Cu(II) ions.

Spectroscopic (FT-IR, FT-Raman, NMR and UV–vis), quantum calculation, molecular structure, solvent interaction, ADME and molecular docking investigation on 4-oxo-4h-1-benzopyran-2-carboxylic acid

The present work, spectroscopic and quantum computational study has been carried out for the molecule 4-oxo-4H-1-benzopyran-2-carboxylic acid. The stable conformer of the title molecule was identified using Potential Energy Surface (PES) scan. The structural and geometrical parameters of the stable conformer of the molecule were determined by Density Functional Theory (DFT) using B3LYP method along with the basis set 6-311++G(d,p) through Gaussian 09 W software. The theoretical and experimental investigations such as Vibrational (FT-IR and FT-Raman), UV–visible and NMR analysis were done. The FT-IR were recorded in the region of (4000–400 cm−1) and FT-Raman in the region of (4000–100 cm−1), and the vibrational bands were compared with the theoretical values. Carbon NMR and Proton NMR spectra have been analyzed in DMSO solution. The theoretical chemical shift values were determined using Gauge Independent Atomic Orbital (GIAO) method. The intermolecular and intra-molecular bonding of orbitals and transfer of charge were studied using the Natural Bond Orbital (NBO) analysis. The respective transitional study was done through UV–vis's spectra and theoretical values predicted using TD-DFT (Time Dependent – DFT) method for both gas and solvent (ethanol) state. HOMO (Highest Occupied Molecular Orbital) – LUMO (Lowest Unoccupied Molecular Orbital) energy gap results prove the exchange of charges inside the molecule. Molecular Electrostatic Potential (MEP) is used to identify the nucleophilic and electrophilic sites of the molecule. To check the bioactive nature of the title molecule the drug-likeness was determined. Molecular docking is used to analyze the biological activity of the title molecule. The distribution of torsional angles in a protein structure is viewed by the Ramachandran plots of the molecules.

Electroporation Enhances the Anticancer Effects of Novel Cu(II) and Fe(II) Complexes in Chemotherapy-Resistant Glioblastoma Cancer Cells.

Schiff base ligand (L) was obtained by condensation reaction between 4-aminopyrimidin-2(1H)-one (cytosine) with 2-hydroxybenzaldehyde. The synthesized Schiff base was used for complexation with Cu(II) and Fe(II) ions used by a molar (2 : 1 mmol ration) in methanol solvent. The structural features of ligand, Cu(II), and Fe(II) metal complexes were determined by standard spectroscopic methods (FT-IR, elemental analysis, proton and carbon NMR spectra, UV/VIS, and mass spectroscopy, magnetic susceptibility, thermal analysis, and powder X-ray diffraction). The synthesized compounds (Schiff base and its metal complexes) were screened in terms of their anti-proliferative activities in U118 and T98G human glioblastoma cell lines alone or in combination with electroporation (EP). Moreover, the human HDF (human dermal fibroblast) cell lines was used to check the bio-compatibility of the compounds. Anti-proliferative activities of all compounds were ascertained using an MTT assay. The complexes exhibited a good anti-proliferative effect on U118 and T98G glioblastoma cell lines. In addition, these compounds had a negligible cytotoxic effect on the fibroblast HDF cell lines. The use of compounds in combination with EP significantly decreased the IC50 values compared to the use of compounds alone (p<0.05). These results show that newly synthesized Cu(II) and Fe(II) complexes can be developed for use in the treatment of chemotherapy-resistant U118 and T98G glioblastoma cells and that treatment with lower doses can be provided when used in combination with EP.

A simple study on vaporization enthalpy of taurine anion-based ionic liquid

Room temperature ionic liquids, as a new type of environmentally friendly “green solvents”, have many well-known and unique properties, which lay the foundation for their wide application in many fields. Two target products, 1-propyl-3-methylimidazolium taurine ionic liquid and 1- butyl −3- methylimidazolium taurine ionic liquid, were synthesized by conventional two - step synthesis method. Hydrogen and carbon NMR spectra were also used to verify the chemical structure of the target products. Isothermal thermogravimetric analysis was used to record the decreasing trend of the weight for two ionic liquids samples over time. According to Langmuir equation and Clausius-Clapeyron equation, vaporization enthalpies of two ionic liquids were obtained. For the study of thermodynamic properties, the vaporization enthalpy data of ionic liquid in a certain temperature range are very important and indispensable.

Evaluation of the ID number method for structure generation and complete assignment of NMR spectra of erythromycin A

The present paper describes the evaluation of the ID number method for the structure generation and complete assignments of proton and carbon NMR spectra of erythromycin A. This study revised the errors found in previous assignments of two carbon signals in the spectra of this compound.

Synthesis, Spectroscopic and Computational Studies of Some Metals Chelates with Chromene-2-one and Pyrazine-Based Ligands

The present paper deals with the synthesis of cobalt(II), nickel(II), copper(II) and cadmium(II) complexes with two bidentate ligands, L1 (3-(quinoxaline-2-yl)-coumarin) and L2 (2-methylene-2H-chromene-3-(methyl carbonimidic)thioanhydride). The L1 ligand was prepared by treating w-bromo-3-acetylcoumarin with 1,2-phenylenediamine whereas the ligand L2 was prepared through substitution reaction ofw-bromo-3-acetylcoumarin with potassium thiocyanate in ethanol medium. The confirmation of the structures for L1 and L2 were done by (C.H.N.S.) elemental analysis, FT-IR, NMR and mass spectra. The metal complexes of cobalt(II), nickel(II), copper(II) and cadmium(II), with L1 and L2, were prepared and isolated in the solid state then characterized by (C.H.N.M) elemental analysis, proton and carbon-13 NMR, FT-IR and mass spectra. Furthermore, the thermal analysis (TG-DSC) for some complexes assisted us in the elucidation of the suggested structures of complexes and confirmed their thermal stability. The results obtained from elemental analysis, magnetic susceptibility and thermal analysis confirmed that all metal complexes were formed in 2:1 molar ratio of ligand to metal with octahedral structures except cadmium(II) complexes which were in a tetrahedron geometry with 1:1 mole ratio. The complexes are found to be soluble in DMF and DMSO. The results obtained from TG-DSC analysis revealed that the metal complexes were thermally stable with point decomposition over 350 °C. The DFT/TDDFT calculations were carried out to provide the electronic structures and spectra of the compounds.

Ion exchange and binding in selenium remediation materials using DNP-enhanced solid-state NMR spectroscopy

Selenate-loaded selenium water remediation materials based on polymer fibres have been investigated by dynamic nuclear polarization (DNP) enhanced solid-state NMR. For carbon-13 a significant reduction in experiment time is obtained with DNP even when compared with conventional carbon-13 NMR spectra recorded using larger samples. For the selenium remediation materials studied here this reduction allows efficient acquisition of {1H}-77Se heteronuclear correlation spectra which give information about the nature of the binding of the remediated selenate ions with the grafted side chains which provide the required ion exchange functionality.

Use of Random forest in the identification of important variables

Random Forest (RF) technique has been shown to be promising in the supervised classification applied in different matrices. However, approaches to identifying significant variables that weight the model are scarce, in the classification problems. In this paper, we propose a methodology for the selection of variables of greater relevance in the construction of RF models. For the application of this methodology, classification models were developed to discriminating crude oil samples, about to their maximum pour point (MPP). In this sense, data from MPP (ASTM D5853) of 105 crude oil samples, their hydrogen (1H) NMR spectra and carbon (13C) NMR spectra were acquired. With MPP ranging from −54 °C to 39 °C, two classes were assigned: the first containing 43 samples with MPP value ≤ −9 °C, and, the second, 62 samples with MPP value > −9 °C. The 1H NMR models, with 90% accuracy, and 13C NMR, with 71% accuracy, were used in the selection of variable method. The results showed that the methodology proposed to select variables was effective in the distinction of the variables that best contributed to the discrimination of oils. Therefore, this new tool enabled a greater understanding of the interest chemical information, contained in the spectra and its relationship with the MPP property of the crude oil samples.

Synthesis, crystal growth, thermal and laser damage threshold properties of new Schiff base NLO material 4-Nitro-benzoic acid (3-ethoxy-2-hydroxy-benzylidene)-hydrazide

Novel organic Schiff base nonlinear optical material 4-Nitro-benzoic acid (3-ethoxy-2-hydroxy-benzylidene)-hydrazide (NEH) was synthesized and grown as single crystal by slow evaporation technique. The structure and unit cell parameter of NEH was confirmed by single crystal X-ray diffraction analysis and the crystal belongs to orthorhombic crystal system with noncentrosymmetric space group Pna21. Further both carbon and hydrogen NMR spectra confirm the formation of material and the presence of functional group was analyzed by Fourier Transform Infrared (FTIR) analysis. The optical absorption spectrum of the grown crystal shows the material has lower cut off wavelength at 320 nm. Thermal property of NEH was studied by TG/DTA analysis. The second harmonic nonlinear efficiency was accessed by Kurtz-Perry powder technique and it possesses an efficiency of 0.7 times that of standard KDP. The laser damage threshold of NEH crystal was found to be 3.22 GW/cm2.

Sensitivity-enhanced detection of non-labile proton and carbon NMR spectra on water resonances

Chemical exchange saturation transfer (CEST) experiments enhance the NMR signals of labile protons by continuously transferring these protons' saturation to an abundant solvent pool like water. The present study expands these principles by fusing into these experiments homonuclear isotropic mixing sequences, enabling the water-enhanced detection of non-exchangeable species. Further opportunities are opened by the addition of coupling-mediated heteronuclear polarization transfers, which then impose on the water resonance a saturation stemming from non-labile heteronuclear species like 13C. To multiplex the ensuing experiments, these relayed approaches are combined with time-domain schemes involving multiple Ramsey-labeling experiments imparting the frequencies of the non-labile sites on the water resonance, via chemical exchange. 13C and 1H NMR spectra were detected in this fashion with about two-fold SNR amplification vis-à-vis conventionally detected spectroscopies. When combined with non-uniform sampling principles, this methodology thus becomes a sensitive alternative to detect non-exchangeable species in biomolecules. Still, multiple parameters including the scalar couplings and solvent exchange rates, will affect the efficiency and consequently the practicality of the overall experiment.

Structural Properties and Isotopic Abundance Ratio Analysis of Magnesium Gluconate Treated with the Energy of Consciousness Using LC-MS and NMR Spectroscopy

The present study was aimed to evaluate the impact of The Trivedi Effect® - Energy of Consciousness Healing Treatment (Biofield Energy Healing Treatment) on magnesium gluconate for the change in the structural properties and isotopic abundance ratio (PM+1/PM and PM+2/PM) using LC-MS and NMR spectroscopy. Magnesium gluconate was divided into two parts – one part was control, and another part was treated with The Trivedi Effect®- Biofield Energy Healing Treatment remotely by twenty renowned Biofield Energy Healers and defined as The Trivedi Effect® treated sample. The LC-MS analysis of both the control and treated samples revealed the presence of the mass of the protonated magnesium gluconate at m/z 415 at the retention time of 1.52 min with almost similar fragmentation pattern. The relative peak intensities of the fragment ions of the treated sample were significantly altered compared with the control sample. The proton and carbon signals for CH, CH2 and CO groups in the proton and carbon NMR spectra were found almost similar for the control and the treated samples. The isotopic abundance ratio analysis revealed that the isotopic abundance ratios of PM+1/PM (2H/1H or 13C/12C or 17O/16O or 25Mg/24Mg) and PM+2/PM (18O/16O or 26Mg/24Mg) were significantly decreased in the treated sample by 35.97% and 66.77%, respectively compared with the control sample. Briefly, 13C, 2H, 17O, and 25Mg contributions from (C12H23MgO14)+ to m/z 416; 18O and 26Mg contributions from (C12H23MgO14)+ to m/z 417 in the treated sample were significantly reduced compared with the control sample. Thus, The Trivedi Effect® treated magnesium gluconate could be valuable for designing better pharmaceutical and/or nutraceutical formulations through its changed physicochemical and thermal properties, which might be providing better therapeutic response against various diseases such as diabetes mellitus, allergy, aging, inflammatory diseases, immunological disorders, and other chronic infections. The Trivedi Effect® Treated magnesium gluconate might be supportive to design the novel potent enzyme inhibitors using its kinetic isotope effects.

NMR Spectroscopy as a Robust Tool for the Rapid Evaluation of the Lipid Profile of Fish Oil Supplements.

The western diet is poor in n-3 fatty acids, therefore the consumption of fish oil supplements is recommended to increase the intake of these essential nutrients. The objective of this work is to demonstrate the qualitative and quantitative analysis of encapsulated fish oil supplements using high-resolution 1H and 13C NMR spectroscopy utilizing two different NMR instruments; a 500 MHz and an 850 MHz instrument. Both proton (1H) and carbon (13C) NMR spectra can be used for the quantitative determination of the major constituents of fish oil supplements. Quantification of the lipids in fish oil supplements is achieved through integration of the appropriate NMR signals in the relevant 1D spectra. Results obtained by 1H and 13C NMR are in good agreement with each other, despite the difference in resolution and sensitivity between the two nuclei and the two instruments. 1H NMR offers a more rapid analysis compared to 13C NMR, as the spectrum can be recorded in less than 1 min, in contrast to 13C NMR analysis, which lasts from 10 min to one hour. The 13C NMR spectrum, however, is much more informative. It can provide quantitative data for a greater number of individual fatty acids and can be used for determining the positional distribution of fatty acids on the glycerol backbone. Both nuclei can provide quantitative information in just one experiment without the need of purification or separation steps. The strength of the magnetic field mostly affects the 1H NMR spectra due to its lower resolution with respect to 13C NMR, however, even lower cost NMR instruments can be efficiently applied as a standard method by the food industry and quality control laboratories.

Structural and Natural Isotopic Abundance Analysis of Magnesium Gluconate Treated with Energy of Consciousness (The Trivedi Effect®) Using LC-MS and NMR

The current research article was aimed to investigate the impact of The Trivedi Effect®- Energy of Consciousness Healing Treatment on the structural properties and isotopic abundance ratio (PM+1/PM and PM+2/PM) of magnesium gluconate using LC-MS and NMR spectroscopy. Magnesium gluconate was divided into two parts – one part was control, and another part was treated with The Trivedi Effect® remotely by eighteen renowned Biofield Energy Healers and defined as the Trivedi Effect® Treated sample. The liquid chromatogram of the control sample showed two peaks at Rt of 1.81 and 2.06 min, whereas the Trivedi Effect® Treated sample displayed these peaks at Rt of 1.79 and 2.03 min. The ESI-MS spectra of the control and the Trivedi Effect® Treated samples revealed the presence of the mass for magnesium gluconate ion in two forms at m/z 447 (adduct form with methanol) and 415 (protonated ion) in positive ionization mode. But, it showed the mass for the gluconate ion at m/z 195 in the negative ionization mode. The fragmentation pattern of magnesium gluconate in the treated sample was notably altered as compared to the control sample. The proton and carbon signals for CH, CH2 and CO groups in the proton and carbon NMR spectra were found almost similar for the control and the treated samples. The isotopic abundance ratio analysis revealed that the isotopic abundance ratio of PM+1/PM (2H/1H or 13C/12C or 17O/16O or 25Mg/24Mg) in two magnesium gluconate ion forms at m/z 447 and 415 in treated sample was significantly decreased by 59.82% and 55.44%, respectively compared with the control sample. The percentage change in the isotopic abundance ratio of PM+2/PM (18O/16O or 26Mg/24Mg) was remarkably decreased in the magnesium gluconate ion at m/z 447 in the treated sample by 78.26% compared with the control sample. Consequently, the isotopic abundance ratio of PM+1/PM (2H/1H or 13C/12C or 17O/16O) in gluconate ion in the treated sample was significantly increased by 37.35% with respect to the control sample. Thus, the Trivedi Effect® treated magnesium gluconate could be valuable for designing better pharmaceutical and/or nutraceutical formulations through its changed physicochemical and thermal properties, which might be providing better therapeutic response against various diseases such as diabetes mellitus, allergies, aging, inflammatory diseases, immunological disorders, and other chronic infections. The treated magnesium gluconate might be helpful to design the novel potent enzyme inhibitors by using its kinetic isotope effects.

Evaluation of Isotopic Abundance Ratio and Structural Properties of Magnesium Gluconate After Treatment with the Energy of Consciousness Using LC-MS and NMR Spectroscopy

The current research work was aimed to investigate the impact of The Trivedi Effect® - Energy of Consciousness Healing Treatment (Biofield Energy Healing) on the structural properties and isotopic abundance ratio (PM+1/PM) of magnesium gluconate using LC-MS and NMR spectroscopy. Magnesium gluconate was divided into two parts. One part was denoted as the control, while the another part was defined as The Trivedi Effect® Treated sample, which received the Biofield Energy Healing Treatment remotely from eighteen renowned Biofield Energy Healers. The total ion chromatogram of the control sample showed two peaks at Rt of 1.81 and 2.06 min, whereas the treated sample displayed peaks at Rt of 1.79 and 2.04 min. The ESI-MS spectra of the control and the treated samples revealed the presence of the mass for magnesium gluconate ion in two forms at m/z 447 (adduct form with methanol) and 415 (protonated ion) in positive ionization mode. But, it showed the mass for the gluconate ion at m/z 195 in the negative ionization mode. The fragmentation pattern of magnesium gluconate in the treated sample was notably altered compared with the control sample. The proton and carbon signals for CH, CH2 and CO groups in the proton and carbon NMR spectra were found almost similar for the control and treated samples. The LC-MS based isotopic abundance ratio analysis indicated that the PM+1/PM (2H/1H or 13C/12C or 17O/16O or 25Mg/24Mg) in the treated magnesium gluconate ion at m/z 415 was significantly decreased by 79.24% compared with the control sample. Similarly, the isotopic abundance ratio of PM+1/PM (2H/1H or 13C/12C or 17O/16O) in the gluconate ion was decreased by 6.62% in the treated sample compared with the control sample. The treated magnesium gluconate might be beneficial in the nutraceutical and/or pharmaceutical industries for designing various forms of formulations, which could be providing better therapeutic response against various diseases such as diabetes mellitus, allergy, aging, inflammatory diseases, immunological disorders, and other chronic infections. Consequently, The Trivedi Effect® - Energy of Consciousness Healing Treated magnesium gluconate would be more helpful for understanding the enzymatic reactions as well as assist in the designing of the novel potent enzyme inhibitors by applying its kinetic isotope effects.

MOLECULAR DESIGN OF SUGAR-FREE MIGRACIN ANALOG MIGRACINAL THAT INHIBITS OVARIAN CANCER CELL MIGRATION AND INVASION

Introduction . Cancer metastasis consists of several steps including detachment from the primary tumor, migration, invasion, transport in the blood or lymphatic vessels, attachment at the secondary site, and growth of secondary tumor. Migration and invasion areinvolved in the mechanism of all types of cancer metastasis. We previously isolated novel cellular migration inhibitor migracin A and B from a culture filtrate of Streptomyces sp. Migracin A was shown to inhibit IGF-1-mediated cellular migration and invasion in ovarian carcinoma cells. However, it is difficult to prepare large amount of migracin A. Migracin A consists of substituted benzene and an alkylated sugar moiety. In the present research, we have designed and synthesized a simplified dialdehydederivative of migracin called migracinal having no sugar moiety. Material and methods. Migracinal was purchased from Techno Chem Co., Ltd., Tokyo, Japan. Migracinal was prepared from 2,4-dihydroxybenzaldehyde (2,4-DHBA). The structure was confirmed by proton and carbon NMR spectra and ESI mass spectroscopy. The antitumor activity of the new derivative was studied by standard tests under conditions in vitro. Results. Migracinal inhibited cellular migration and invasion in ovarian clear cell carcinoma ES-2 cells. It also inhibited IGF-1 expression as migracin A. Moreover, it induced anoikis rather than apoptosis in ES-2 cells. Conclusions. Migracinal is easier to prepare than migracins, and it may be useful for the mechanistic study and suppression of metastasis.

LC-MS and NMR Based Structural Characterization and Isotopic Abundance Ratio Analysis of Magnesium Gluconate Treated with the Consciousness Energy Healing

Magnesium gluconate is widely used pharmaceutical/nutraceutical compound for the prevention and treatment of magnesium deficiency diseases. The present study was designed to explore the effect of The Trivedi Effect^® - Energy of Consciousness Healing Treatment (Biofield Energy Healing Treatment) on magnesium gluconate for the change in the structural properties and isotopic abundance ratio (P_M+1/P_M and P_M+2/P_M) using LC-MS and NMR spectroscopy. Magnesium gluconate was divided into two parts – one part was control, and another part was treated with The Trivedi Effect^® - Energy of Consciousness Healing Treatment remotely by twenty renowned Biofield Energy Healers and defined as The Trivedi Effect^® treated sample. The LC-MS analysis of both the control and Biofield Energy Treated samples indicated the presence of mass of the protonated magnesium gluconate at <i>m/z</i> 415 at the retention time of 1.52 min and fragmentation pattern of both samples were almost identical. The relative peak intensities of the fragment ions were significantly altered in the treated sample compared to the control sample. The proton and carbon signals for CH, CH₂ and CO groups in the proton and carbon NMR spectra of the control and treated samples were found same. The percentage change in the isotopic abundance ratio of P_M+1/P_M (²H/¹H or ¹³C/¹²C or ¹⁷O/¹⁶O or ²⁵Mg/²⁴Mg) was significantly decreased in the treated sample by 48.87% compared to the control sample. Subsequently, the isotopic abundance ratio of P_M+2/P_M (¹⁸O/¹⁶O or ²⁶Mg/²⁴Mg) in the treated sample was significantly increased by 29.18% compared with the control sample. In summary, ¹³C, ²H, ¹⁷O, and ²⁵Mg contributions from (C₁₂H₂₃MgO₁₄)⁺ to <i>m/z</i> 416; ¹⁸O and ²⁶Mg contributions from (C₁₂H₂₃MgO₁₄)⁺ to <i>m/z</i> 417 in the treated sample were significantly altered compared with the control sample. Thus, The Trivedi Effect^® Treated magnesium gluconate might be helpful to design the novel potent enzyme inhibitors using its kinetic isotope effects. Consequently, The Trivedi Effect^® Treated magnesium gluconate would be valuable for designing better pharmaceutical and/or nutraceutical formulations through its altered physicochemical and thermal properties, which might be providing better therapeutic response against various diseases such as diabetes mellitus, allergy, aging, inflammatory diseases, immunological disorders, and other chronic infections.

First structurally characterized anion exchange product of noval cyclohexane containing substituted thio piperazinium chloride [C6H11S(CH2)3C4H9N2C6H5Cl (L1Cl)]: Synthesis, crystal structure and supramolecularity of (L1NO3)

[C6H11S(CH2)3C4H9N2C6H5Cl (L1Cl)] has been synthesized by reaction of cyclohexyl thiol with 1-(chlorophenyl)-4-(3-chloropropyl) piperazine hydrochloride (P1) under dry nitrogen atmosphere. The L1Cl on reaction with Cd(NO3)2 forms a compound [L1NO3] having NHO hydrogen bonding. The single crystal structure of the compound L1NO3 is solved. The characteristic feature of these reactions is the retention of the piperazinium character from starting material (P1) to ligand formation (L1Cl) as well as in the formation of anion exchange product (L1NO3). L1Cl and L1NO3 are characterized on the basis of physico-chemical and spectral (ESI Mass, FT-IR, 1H, 13C and DEPT 135° 13C {1H} NMR) studies. The proton and carbon-13 NMR spectra of L1Cl and L1NO3 are characteristic. L1NO3 crystallizes in orthorhombic system with Pbca space group. Both piperazine and cyclohexane rings adopt the chair conformation with N1, N2 and C14, C17 out of plane. Geometry around quaternary nitrogen atom is distorted tetrahedral as revealed by the bond angles.