scholarly journals ISOLATION OF 2-CHLOROBENZIMIDAZOLE FROM MELIA DUBIA LEAF EXTRACT AND ITS STRUCTURAL CHARACTERISATION

2017 ◽  
Vol 9 (10) ◽  
pp. 67 ◽  
Author(s):  
G. Dayana Jeyaleela ◽  
S. Irudaya Monisha ◽  
J. Rosaline Vimala ◽  
A. Anitha Immaculate
Keyword(s):  
Mass Spectrometry ◽  
1H Nmr ◽  
Research Work ◽  
Proton Nuclear Magnetic Resonance ◽  
Resonance Spectroscopy ◽  
Ft Ir ◽  
Uv Visible ◽  
Isolated Compound ◽  
Promising Source

Objective: Natural products from medicinal plants, either as isolated compounds or as standardized plant extracts exhibit promising source of medicinal activity against various diseases. The aim of the present work was to make an attempt of isolation of bioactive principle and characterization of the isolated compound, from the medicinal plant Melia dubaiMethods: The extraction was done by a cold percolation method and the compound was separated and isolated by chromatography technique such as a thin layer chromatography (TLC), column chromatography and high-performance liquid chromatography (HPLC). The isolated compound was crystallized and the structural characterization of the isolated compound was made using UV-Visible, FT-IR, 1H-NMR, GC-MS and MS techniques which confirmed the structure of the isolated compound.Results: The separated and isolated compound was characterized by both physical and spectral methods like Ultraviolet-Visible spectroscopy (UV-Visible), Fourier transform infrared spectroscopy (FT-IR), Proton Nuclear Magnetic Resonance Spectroscopy (1H-NMR), Gas chromatography-mass spectrometry (GC-MS), and Mass spectrometry(MS). Based on the studies, organizational characteristics of one bioactive principle were deciphered. The results revealed that the isolated species is 2-chlorobenzimidazole and it agreed well with the reported value and spectra for 2-chlorobenzimidazole.Conclusion: The above results obtained in this research work clearly indicated the promising occurrence of 2-chlorobenzimidazole in Media dubia plant leaves. The future scope of these studies may guide us to view the biological activity of the isolated compound.

scholarly journals An Optimization of Liquid–Liquid Extraction of Urinary Volatile and Semi-Volatile Compounds and Its Application for Gas Chromatography-Mass Spectrometry and Proton Nuclear Magnetic Resonance Spectroscopy

Molecules ◽  
2020 ◽  
Vol 25 (16) ◽  
pp. 3651
Author(s):  
Natalia Drabińska ◽  
Piotr Młynarz ◽  
Ben de Lacy Costello ◽  
Peter Jones ◽  
Karolina Mielko ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Gas Chromatography ◽  
1H Nmr ◽  
Biomarker Discovery ◽  
Liquid Extraction ◽  
Proton Nuclear Magnetic Resonance ◽  
Gas Chromatography Mass Spectrometry ◽  
Resonance Spectroscopy ◽  
Liquid Liquid Extraction

Urinary volatile compounds (VCs) have been recently assessed for disease diagnoses. They belong to very diverse chemical classes, and they are characterized by different volatilities, polarities and concentrations, complicating their analysis via a single analytical procedure. There remains a need for better, lower-cost methods for VC biomarker discovery. Thus, there is a strong need for alternative methods, enabling the detection of a broader range of VCs. Therefore, the main aim of this study was to optimize a simple and reliable liquid–liquid extraction (LLE) procedure for the analysis of VCs in urine using gas chromatography-mass spectrometry (GC-MS), in order to obtain the maximum number of responses. Extraction parameters such as pH, type of solvent and ionic strength were optimized. Moreover, the same extracts were analyzed using Proton Nuclear Magnetic Resonance Spectroscopy (1H-NMR), to evaluate the applicability of a single urine extraction for multiplatform purposes. After the evaluation of experimental conditions, an LLE protocol using 2 mL of urine in the presence of 2 mL of 1 M sulfuric acid and sodium sulphate extracted with dichloromethane was found to be optimal. The optimized method was validated with the external standards and was found to be precise and linear, and allowed for detection of >400 peaks in a single run present in at least 50% of six samples—considerably more than the number of peaks detected by solid-phase microextracton fiber pre-concentration-GC-MS (328 ± 6 vs. 234 ± 4). 1H-NMR spectroscopy of the polar and non-polar extracts extended the range to >40 more (mainly low volatility compounds) metabolites (non-destructively), the majority of which were different from GC-MS. The more peaks detectable, the greater the opportunity of assessing a fingerprint of several compounds to aid biomarker discovery. In summary, we have successfully demonstrated the potential of LLE as a cheap and simple alternative for the analysis of VCs in urine, and for the first time the applicability of a single urine solvent extraction procedure for detecting a wide range of analytes using both GC-MS and 1H-NMR analysis to enhance putative biomarker detection. The proposed method will simplify the transport between laboratories and storage of samples, as compared to intact urine samples.

scholarly journals Synthesis and characterization of mixed ligand catecholato-bis (diamine-mono-dithiocarbamato) vanadium (IV) complexes

2017 ◽  
Vol 52 (2) ◽  
pp. 89-96
Author(s):  
B Begum ◽  
A Sarker ◽  
AKM Lutfor Rahman ◽  
NC Bhoumik
Keyword(s):  
1H Nmr ◽  
Molar Conductance ◽  
Bidentate Ligand ◽  
Mixed Ligand ◽  
Vanadium Complexes ◽  
Spectroscopic Techniques ◽  
Physico Chemical ◽  
Ft Ir ◽  
Uv Visible

Diamine-mono-dithiocarbamates are mono-basic bidentate ligand forming stable complexes with transition metals. Mixed ligand catecholato-bis (diamine-mono-dithiocarbamato) vanadium (IV) complexes were synthesized and characterized using FT-IR, UV-visible and 1H-NMR spectroscopic techniques. The formation of vanadium complexes was con?rmed by the disappearance of ?S-H band in the complexes which was present in the ligands and incidence of ?V-S and ?V-O band in FT-IR spectra of the complexes. The mono-dithiocarbamate with one uncoordinated ?NH/NH2 group was indicated by the presence of ?N-H vibrational band in both the ligands and complexes. In the 1H-NMR spectra, the peak for –SH proton of ligands disappeared in the complexes suggest the formation of [VL2Cat] complex. Non-electrolytic nature of the synthesized complexes was established by their low molar conductance values. The +4 oxidation state of vanadium was con?rmed by the electronic spectra of the complexes. On the basis of all physico-chemical data, a six-coordinated octahedral structure has been suggested for catecholato-bis (diamine-mono-dithiocarbamato) vanadium (IV) complexes.Bangladesh J. Sci. Ind. Res. 52(2), 89-96, 2017

scholarly journals CARACTERIZACIÓN QUÍMICA Y FUNCIONAL DE METABOLITOS ANTIMICROBIANOS AISLADOS DE ASCIDIAN RHOPALAEA BIRKELANDI

2011 ◽  
Vol 3 ◽  
pp. 111
Author(s):  
Maribel Cordero ◽  
Henry Borbón ◽  
Félix R. Román ◽  
Luis Morell ◽  
Rigoberto Víquez ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Costa Rica ◽  
Magnetic Resonance ◽  
13C Nmr ◽  
Solid Phase ◽  
Proton Nuclear Magnetic Resonance ◽  
Gas Chromatography Mass Spectrometry ◽  
Spectroscopic Techniques ◽  
Ft Ir ◽  
Uv Visible

Marine ecosystems have a very large diversity of resources, most of them still partially unknown, and a few others exploited for development of new industrial and toxicological products. The objective of this investigation was to determine whether the acetone extract of the ascidia R. birkelandi from the Pacific coast of Costa Rica showed qualitative antimicrobial activity against the S. aureus bacteria and the G. candidum fungus, and to verify their main secondary metabolites in the active extract using chromatographic and spectroscopic techniques. Ascidians were collected at Tambor, Guanacaste, Costa Rica, between December 2007 and March 2008. Activity against the Gram positive bacteria and fungi was evaluated using ethanolic (95%) and acetonic extracts. Both extracts showed activity against G. candidum; however, only the acetonic extract showed activity against S. aureus. A coumarin and a hydroxyanthraquinone were isolated from a crude extract of R. birkelandi as metabolites present in the active fraction. Purification and isolation were performed by chromatographic techniques and solid phase extraction. Structural information was obtained by spectroscopic analyses: Ultraviolet (UV-Visible), Fourier Transform Infrared (FT-IR), Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS), Gas Chromatography Mass Spectrometry (GC/MS), Proton Nuclear Magnetic Resonance (1HNMR), and Carbon-13 Magnetic Resonance (13C-NMR). Further studies are recommended for characterization and quantification of the active components of this extract and the possible elucidation of the mechanisms of action. Los ecosistemas marinos poseen una gran cantidad de recursos, muchos de ellos todavía desconocidos y muy pocos de ellos explotados para el desarrollo de nuevos productos industriales y toxicológicos. Los objetivos de esta investigación fueron determinar si el extracto acetónico de la ascidia R. birkelandi de la costa pacífica de Costa Rica presenta actividad antimicrobial cualitativa contra la bacteria S. aureus y el hongo G. candidum, y determinar por técnicas cromatográficas y espectroscópicas los metabolitos secundarios principales presentes en el extracto activo. Se recolectó la ascidia en la zona de Tambor en la provincia de Guanacaste, Costa Rica, entre los meses de diciembre del 2007 y marzo del 2008. Se realizaron extractos crudos en acetona y etanol al 95% para evaluar la actividad contra una bacteria Gram positiva y un hongo. Ambos extractos presentaron actividad contra G. candidum, pero solo el extracto acetónico mostró actividad contra S. aureus. Se logró aislar y caracterizar una cumarina y una hidroxiantraquinona del extracto crudo de R. birkelandi como metabolitos presentes en la fracción responsable de la actividad biológica presentada. La purificación y el aislamiento fueron llevados a cabo con técnicas cromatográficas y de extracción en fase sólida. La información estructural fue obtenida por análisis espectroscópicos: Ultravioleta (UV-Visible), Infrarrojo con Transformada de Fourier (FT-IR), Cromatografía Líquida acoplada a Espectrometría de Masas (LC/MS/MS), Cromatografía de Gases acoplada a Masas (GC-MS), Resonancia Magnética Nuclear de Protón (1H-NMR) y Resonancia Magnética de Carbono 13 (13C-NMR). Se recomiendan estudios futuros para la caracterización y la cuantificación de los principios activos de este extracto y una posible elucidación de sus mecanismos de acción.

scholarly journals Synthesis of Lactic Acid-Based Thermosetting Resins and Their Ageing and Biodegradability

Polymers ◽  
2020 ◽  
Vol 12 (12) ◽  
pp. 2849
Author(s):  
Lara Lopes Gomes Hastenreiter ◽  
Sunil Kumar Ramamoorthy ◽  
Rajiv K. Srivastava ◽  
Anilkumar Yadav ◽  
Akram Zamani ◽  
...  
Keyword(s):  
Lactic Acid ◽  
1H Nmr ◽  
Proton Nuclear Magnetic Resonance ◽  
Resonance Spectroscopy ◽  
Scanning Calorimetry ◽  
Soil Burial ◽  
Chemical Structures ◽  
Macro Scale ◽  
Ft Ir ◽  
Oxidative Ageing

The present work is focused on the synthesis of bio-based thermoset polymers and their thermo–oxidative ageing and biodegradability. Toward this aim, bio-based thermoset resins with different chemical architectures were synthesized from lactic acid by direct condensation with ethylene glycol, glycerol and pentaerythritol. The resulting branched molecules with chain lengths (n) of three were then end-functionalized with methacrylic anhydride. The chemical structures of the synthesized lactic acid derivatives were confirmed by proton nuclear magnetic resonance spectroscopy (1H-NMR) and Fourier transform infrared spectroscopy (FT–IR) before curing. To evaluate the effects of structure on their properties, the samples were investigated by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and the tensile testing. The samples went through thermo-oxidative ageing and biodegradation; and their effects were investigated. FT-IR and 1H-NMR results showed that three different bio-based resins were synthesized using polycondensation and end-functionalization. Lactic acid derivatives showed great potential to be used as matrixes in polymer composites. The glass transition temperature of the cured resins ranged between 44 and 52 °C. Pentaerythritol/lactic acid cured resin had the highest tensile modulus and it was the most thermally stable among all three resins. Degradative processes during ageing of the samples lead to the changes in chemical structures and the variations in Young’s modulus. Microscopic images showed the macro-scale surface degradation on a soil burial test.

scholarly journals Novel Photosynthesis And Characterization of 4-(5,7- Dichloro-8ah-chromene-2-yl)-n, N-dimethylaniline from Its Chalcone Isomer

2020 ◽  
Vol 23 (2) ◽  
pp. 135-149
Author(s):  
Nirozh A. Chalabi ◽  
Ghazwan F. Fadhil
Keyword(s):  
Mass Spectrometry ◽  
Alcoholic Alkali ◽  
Schmidt Reaction ◽  
Flight Mass Spectrometry ◽  
Ft Ir ◽  
Uv Visible ◽  
Xenon Light ◽  
Layer Chromatography ◽  
Tof Ms

In the present study, trans-3-(2,4-dichlorophenyl)-1-(4-(dimethylamino)phenyl)prop-2-en-1-one (trans 2,4-dimethyl amino chalcone) was synthesized by Claisen-Schmidt reaction in the presence of aqueous alcoholic alkali solution by condensation of a substituted acetophenone with substituted benzaldehydes, Then, The photosynthesis of 4-(5,7-dichloro-8aH-chromen-2-yl)-N,N-dimethylaniline (2,4-dimethylamino chromene) was accomplished from the irradiation of the( trans 2,4-dimethyl amino chalcone) with xenon light. The products were characterized by UV-Visible, FT-IR, 1HNMR, thin layer chromatography Elemental analysis(CHNO) and liquid chromatography-quadrupole-time-of-flight mass spectrometry (LC-Q-ToF-MS).

scholarly journals Spot and Cumulative Urine Samples Are Suitable Replacements for 24-Hour Urine Collections for Objective Measures of Dietary Exposure in Adults Using Metabolite Biomarkers

2019 ◽  
Vol 149 (10) ◽  
pp. 1692-1700 ◽  
Author(s):  
Thomas Wilson ◽  
Isabel Garcia-Perez ◽  
Joram M Posma ◽  
Amanda J Lloyd ◽  
Edward S Chambers ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Dietary Intake ◽  
1H Nmr ◽  
Dietary Intervention ◽  
Dietary Exposure ◽  
Urine Samples ◽  
Proton Nuclear Magnetic Resonance ◽  
Resonance Spectroscopy ◽  
Spot Urine ◽  
Exposure Biomarkers

ABSTRACT Background Measurement of multiple food intake exposure biomarkers in urine may offer an objective method for monitoring diet. The potential of spot and cumulative urine samples that have reduced burden on participants as replacements for 24-h urine collections has not been evaluated. Objective The aim of this study was to determine the utility of spot and cumulative urine samples for classifying the metabolic profiles of people according to dietary intake when compared with 24-h urine collections in a controlled dietary intervention study. Methods Nineteen healthy individuals (10 male, 9 female, aged 21–65 y, BMI 20–35 kg/m2) each consumed 4 distinctly different diets, each for 1 wk. Spot urine samples were collected ∼2 h post meals on 3 intervention days/wk. Cumulative urine samples were collected daily over 3 separate temporal periods. A 24-h urine collection was created by combining the 3 cumulative urine samples. Urine samples were analyzed with metabolite fingerprinting by both high-resolution flow infusion electrospray mass spectrometry (FIE-HRMS) and proton nuclear magnetic resonance spectroscopy (1H-NMR). Concentrations of dietary intake biomarkers were measured with liquid chromatography triple quadrupole mass spectrometry and by integration of 1H-NMR data. Results Cross-validation modeling with 1H-NMR and FIE-HRMS data demonstrated the power of spot and cumulative urine samples in predicting dietary patterns in 24-h urine collections. Particularly, there was no significant loss of information when post-dinner (PD) spot or overnight cumulative samples were substituted for 24-h urine collections (classification accuracies of 0.891 and 0.938, respectively). Quantitative analysis of urine samples also demonstrated the relation between PD spot samples and 24-h urines for dietary exposure biomarkers. Conclusions We conclude that PD spot urine samples are suitable replacements for 24-h urine collections. Alternatively, cumulative samples collected overnight predict similarly to 24-h urine samples and have a lower collection burden for participants.

Synthesis and Spectral Characterization of New S-Alkylated 1,2,4-Triazoles as Potential Biological Agents

2017 ◽  
Vol 68 (10) ◽  
pp. 2436-2439
Author(s):  
Stefania Felicia Barbuceanu ◽  
Laura Ileana Socea ◽  
Constantin Draghici ◽  
Elena Mihaela Pahontu ◽  
Theodora Venera Apostol ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Spectral Data ◽  
1H Nmr ◽  
Elemental Analysis ◽  
13C Nmr ◽  
Ethyl Bromide ◽  
Spectral Characterization ◽  
Basic Medium ◽  
Phenacyl Bromide

In the work we presented the behavior of 5-(4-(4-X-phenylsulfonyl)phenyl)-4-(n-propyl)-2H-1,2,4-triazole-3(4H)-thiones (X= Cl or Br) with some alkylation agents. Thus, new S-alkylated 1,2,4-triazole derivatives were synthesized by reaction of the corresponding 1,2,4-triazole-3-thione derivatives with different �-halogenated compounds (ethyl bromide, ethyl chloroacetate or phenacyl bromide), in basic medium. The structures of synthesized compounds were elucidated by spectral data (1H-NMR, 13C-NMR, mass spectrometry) and elemental analysis.

scholarly journals First Insight into Nutraceutical Properties of Local Salento Cichorium intybus Varieties: NMR-Based Metabolomic Approach

2021 ◽  
Vol 18 (8) ◽  
pp. 4057
Author(s):  
Chiara Roberta Girelli ◽  
Francesca Serio ◽  
Rita Accogli ◽  
Federica Angilè ◽  
Antonella De Donno ◽  
...  
Keyword(s):  
1H Nmr ◽  
Cichorium Intybus ◽  
Resonance Spectroscopy ◽  
Metabolic Profiles ◽  
Whole Plant ◽  
Different Content ◽  
Insight Into ◽  
Nutraceutical Properties ◽  
Metabolomic Approach

Background: Plants of genus Cichorium are known for their therapeutic and nutraceutical properties determined by a wealth of phytochemical substances contained in the whole plant. The aim of this paper was to characterize the metabolic profiles of local Salento chicory (Cichorium intybus L.) varieties (“Bianca”, “Galatina”, “Leccese”, and “Otranto”) in order to describe their metabolites composition together with possible bioactivity and health beneficial properties. Methods: The investigation was performed by 1H-NMR spectroscopy and Multivariate Analysis (MVA), by which the metabolic profiles of the samples were easily obtained and compared. Results: The supervised Partial Least Squares Discriminant Analysis (PLS-DA) analysis showed as “Bianca” and “Galatina” samples grouped together separated by “Leccese” and “Otranto” varieties. A different content of free amino acids and organic acids was observed among the varieties. In particular a high content of cichoric and monocaffeoyl tartaric acid was observed for the “Leccese” variety. The presence of secondary metabolites adds significant interest in the investigation of Cichorium inthybus, as this vegetable may benefit human health when incorporated into the diet. Conclusions: The 1H-NMR (Nuclear Magnetic Resonance Spectroscopy) based characterization of Salento chicory varieties allowed us to determine the potential usefulness and nutraceutical properties of the product, also providing a method to guarantee its authenticity on a molecular scale.

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