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2.
Talanta ; 266(Pt 2): 125084, 2024 Jan 01.
Artigo em Inglês | MEDLINE | ID: mdl-37598444

RESUMO

The persistence of active pharmaceutical ingredients in water bodies has lead to detrimental impacts on public health as well as deteriorated aquatic resources at breakneck pace. To address this, highly fluorescent chitosan capped ZnS QDs (CZS QDs) were integrated with nickel ferrite nanoparticles (NF NPs) through ultrasonic assisted method to yield a series of magnetically responsive CZS-xNF nanohybrids (x = 5, 10, 15 and 20 wt% of NF). The successful fabrication of nanohybrids were affirmed through various techniques such as Fourier transform infra-red spectroscopy (FT-IR), powder X-ray diffraction (XRD), X-ray photoelectron microscopy (XPS), high resolution transmission electron microscopy (HRTEM), vibrating sample magnetometer (VSM) and diffused reflectance spectroscopy (DRS). The dual applicability of CZS-xNF nanohybrid was witnessed for the detection of pharmaceutical waste by fluorescence sensing and their concomitant annihilation via visible light driven photodegradation reactions. The developed nanohybrid showed exceptional selectivity towards tetracycline antibiotics, with ultra-low limit of detection of 0.53 µM for tetracycline (TC) and 0.30 µM for minocycline (MC), respectively. The fluorescent sensor was also analysed for trace level detection of tetracyclines in real water samples that showed satisfactory recoveries of 90-106%, depicting practical applicability of sensor. Additionally, the excellent photocatalytic features of synthesized nanohybrid prompted their use in photodegradation of TC and MC and a superior photocatalytic performance was achieved in comparison to CZS QDs. The enhanced photocatalytic performance of CZS-xNF nanohybrid can be attributed to type-I charge transfer mechanism, which resulted in efficient charge separation and reduced photo-induced recombination rate of charge carriers. The nanohybrids were recyclable up to four cycles after being utilized in sensing and photocatalysis, thus offering a promising strategy for environmental remediation through synchronized sensing and extirpation of pharmaceutical waste.


Assuntos
Quitosana , Tetraciclina , Espectroscopia de Infravermelho com Transformada de Fourier , Antibacterianos , Minociclina , Corantes , Microscopia Eletrônica de Transmissão , Preparações Farmacêuticas , Água
3.
J Ethnopharmacol ; 318(Pt B): 116977, 2024 Jan 10.
Artigo em Inglês | MEDLINE | ID: mdl-37544341

RESUMO

ETHNOPHARMACOLOGICAL RELEVANCE: Oxalis corniculata L is a medicinal plant that belongs to the Oxalidaceae family. It is a little, slow-growing plant with a frail appearance typically found in mild temperate and tropical areas like Pakistan and India. This plant also includes many other bioactive substances, including alkaloids, flavonoids, terpenoids, cardiac glycosides, saponins, phlobatannins, and steroids. AIM OF THE STUDY: To investigate the anti-inflammatory effects of Compound diosmin, which is derived from Oxalis corniculata L, on VRV-PL-5 and VRV-PL-8a isolated from Vipera russelli. MATERIALS AND METHODS: Extraction, purification, and characterization of bioactive by TLC, HPTLC, FT-IR analysis, UV-Vis spectrophotometer, LC-MS/MS Analysis, NMR, XRD Analysis, In vitro evaluation, Circular dichroism spectroscopy, in vivo, and in silico studies. RESULTS: In this study, the extract of Oxalis corniculata was evaluated for its in vitro and in vivo anti-inflammatory effect against PLA2. The methanolic extract decreased hemolytic activity by about 60% at 1:75 w/w and neutralized the hemolytic activity completely at 1:100 w/w concentration. Diosmin inhibited VRV-PL-5 and VRV-PL-8a in a dose-dependent manner, with the extent of inhibition being about 56% for VRV-PL-5120 µM and VRV-PL-8a by 62% at the same concentration with IC50 concentrations of 87.08 µM for VRV-PL-5 and 82.08 µM for VRV-PL-8a, while at 75 µM. Diosmin inhibited the hemolytic activity of VRV-PL-5 by about 85%, and at the same concentration, VRV-PL-8a inhibited by about 75%. UV-CD spectra at the IC50 concentration of diosmin disrupted the secondary structure of VRV-PL-5 &VRV-PL-8a. In vivo, studies showed decreased myotoxicity and cardiotoxicity of the VRV-PL-5 &VRV-PL-8a, which was seen in the decrease in cytoplasmic markers LDH and CPK levels in the serum when incubated with diosmin. Furthermore, Histopathological studies of Muscles and lungs revealed that diosmin considerably protects against cellular abnormality caused by VRV-PL-5 & VRV-PL-8a. Molecular docking, MM/GBSA, and molecular dynamics simulation studies show that the diosmin is a potent inhibitor for VRV-PL-5 and VRV-PL-8a. CONCLUSION: This study shows that diosmin is a potentially effective VRV-PL-5 and VRV-PL-8a.


Assuntos
Diosmina , Oxalidaceae , Plantas Medicinais , Simulação de Acoplamento Molecular , Cromatografia Líquida , Espectroscopia de Infravermelho com Transformada de Fourier , Espectrometria de Massas em Tandem , Venenos de Víboras , Fosfolipases A2 , Anti-Inflamatórios/farmacologia
4.
Food Chem ; 431: 137138, 2024 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-37604001

RESUMO

This study aimed to elucidate how the Maillard reaction (MR) affects the flavor and bioactivities of Lentinula edodes hydrolysates (LEHs). Changes in flavor were investigated using non-targeted metabolomics techniques (GC-MS and LC-MS/MS) and sensory evaluation. Simultaneously, UV absorption, fluorescence, and FT-IR spectra were used to characterize the process of MR. We also evaluated the effects of MR on the antioxidant activity, hypoglycemic activity and antimicrobial activity of LEHs in vitro. The results revealed that MR produced many volatile aldehydes and ketones and decreased the content of most amino acids, sugars and flavonoids in the LEHs while increasing the content of l-theanine and succinic acid. MRPs had a strong caramel and like-meat flavor and an obvious improvement in umami, taste continuity, and total acceptability. Furthermore, MR improved the antioxidant and antimicrobial properties of LEHs. This research establishes a theoretical foundation for MR in the deep processing of edible mushrooms.


Assuntos
Reação de Maillard , Cogumelos Shiitake , Cromatografia Líquida , Espectroscopia de Infravermelho com Transformada de Fourier , Espectrometria de Massas em Tandem , Antioxidantes
5.
Food Chem ; 431: 137077, 2024 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-37611361

RESUMO

This study assessed the combined utility of ATR-FTIR spectroscopy and machine learning (ML) techniques for identifying and classifying pure njangsa seed oil (NSO), palm kernel oil (PKO), coconut oil (CCO), njangsa seed oil-palm kernel oil (NSOPKO) and njangsa seed oil-coconut oil (NSOCCO) margarine. Additionally, it quantified the degree of adulteration in each oil and margarine using ML regression models and sunflower oil and canola-flaxseed oil margarine as adulterants. Fingerprints of the oils and the margarines derived in the spectra region 4000-600 cm-1 were combined with ML models. The first two principal components explained 99.4% and 98% of the variance of pure oils and margarines and 90.1, 88.3, 88, 97.3 and 98.3% of adulterated PKO, NSO, CCO, NSOCCO and NSOPKO, respectively while enabling visualization. Pure margarines were classified accurately (100%) in all models. KNN was most effective in classifying pure oil at 97% followed by LR (93%), SVM (83%), LightGBM (53%) and DT (50%). The R2 obtained from all the models for adulterated PKO, NSO, CCO, NSOPKO and NSOCCO ranged from 59-99%, 55-99%, 45-94%, 69-98% and 59-94%, respectively. SVM and DT underperformed, while KNN was the best model.


Assuntos
Margarina , Sementes , Óleo de Coco , Espectroscopia de Infravermelho com Transformada de Fourier , Óleo de Brassica napus , Aprendizado de Máquina
6.
Talanta ; 266(Pt 1): 124959, 2024 Jan 01.
Artigo em Inglês | MEDLINE | ID: mdl-37516070

RESUMO

DNA evidence in sexual assault cases have proven increasingly difficult to obtain and analyse due to increased condom use. With more interest in alternatives to DNA evidence, prophylactic lubricants, spermicides and residues may be interesting prospects. Current interest in the analysis of prophylactic residues focuses on the evaluation and identification of lubricants and constituents, primarily through gas chromatography or Fourier transform infrared spectroscopy. Though cost-effective methods, extensive sample preparation and destructive modes of analysis remain an area for improvement. As a result, the focus has since shifted to ambient ionization methods that offer adequate sensitivity and reduced sample preparation. The Liquid Microjunction Surface Sampling Probe (LMJSSP) is a versatile ambient ionization source that employs a probe that supports a continuously flushing droplet that extracts analytes when placed in contact with a surface. The analytes are aspirated into the mass spectrometer with a Venturi pressure. In this work we use the LMJSSP to analyse the trace transfer of condom lubricant to different types of fabric (cotton, cotton-spandex, and denim). Furthermore, we examine the sensitivity and storage conditions for the direct analysis method on different swab types (cotton, silicone, and foam). Additionally, Principal Component Analysis (PCA) and Maximally Collapsing Metric Learning (MCML) are utilized for visualization of differentiability of commercially available condom brands including Durex™ and Trojan™, and product subtypes. The results present an interesting multi-disciplinary approach of using a direct liquid extraction ambient ionization technique and machine learning to improve the overall workflow for the analysis of lubricants, swabs and fabrics. Machine learning algorithms were able to differentiate between inherent differences of Durex™ and Trojan™ condoms.


Assuntos
Preservativos , Delitos Sexuais , Lubrificantes/análise , Espectrometria de Massas/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos
7.
Food Chem ; 432: 136852, 2024 Jan 30.
Artigo em Inglês | MEDLINE | ID: mdl-37657344

RESUMO

Capsanthin is a natural red pigment widely used in the food industry, but its pigment is severely lost during use and storage. Supramolecular chemistry-based macrocyclic hosts can encapsulate small molecule pigments to improve their stability and solubility. Herein, we synthesized two acyclic cucurbit[n]urils (ACBs, M1 and M2) as carriers for encapsulating capsanthin, and we expect this strategy to generate some positive improvements on the properties of capsanthin, extending its use by the food industry. Successful host-guest inclusion complexes (IC) formation was confirmed via 1H NMR, 2D-ROESY NMR, 13C NMR, XRD, and FT-IR. After encapsulation, the solubility of capsanthin was increased by 75.8 times and 62.3 times, respectively. Furthermore, the storage and utility of capsanthin was enhanced due to the phase transition from oil to solid powder. IC exhibited enhanced stability for capsanthin in challenging environments, such as high temperature, light exposure, acidity, metal ions, food additives, and extreme oxidation.


Assuntos
Antioxidantes , Aditivos Alimentares , Espectroscopia de Infravermelho com Transformada de Fourier , Xantofilas
8.
Food Chem ; 432: 137263, 2024 Jan 30.
Artigo em Inglês | MEDLINE | ID: mdl-37657340

RESUMO

This study aimed to fabricate novel nanocomplexes for delivery of anthocyanins (ACN) utilizing ovalbumin (OVA) and sulphated-polysaccharides with varying linear charge density (κ-,ι-, λ-carrageenan and dextran sulfate: κC < Î¹C < λC < DS). Influence of OVA-sulphated-polysaccharides on ACN stability, antioxidant capacity, and bioaccessibility was investigated. Fabricated nanoparticlecosmeticsed superior encapsulation efficiency (94.11-96.2%) and loaded capacity (9.05-9.54%) for ACN. OVA-DS displayed the smallest particle size and turbidity, while OVA-κC-ACN exhibited the largest ones. ζ-Potential of nanoparticles raised with increasing ester-sulfate level in sulphated-polysaccharides. FT-IR, Raman and OVA conformational alterations revealed existence of intermolecular-interactions between ACN and OVA-polysaccharides. DSC and TGA showed considerable thermo-stability of self-assembled (ACN-loaded) OVA-polysaccharides. Spheroid-nanoparticles size increased after ACN-loading in SEM and CLSM. Composite nanocomplexes enhanced ACN stability and antioxidant properties under accelerated degradation conditions and simulated digestion, particularly, OVA-DS-ACN and OVA-λC-ACN. We provide a choice for reinforcing stability of hydrophilic nutraceuticals and improving its applications.


Assuntos
Antocianinas , Antioxidantes , Ovalbumina , Sulfatos , Espectroscopia de Infravermelho com Transformada de Fourier , Polissacarídeos , Ésteres
9.
Molecules ; 28(18)2023 Sep 06.
Artigo em Inglês | MEDLINE | ID: mdl-37764243

RESUMO

In order to investigate the antioxidant activity of Elaeagnus umbellata polysaccharides, the physicochemical characteristics of purified Elaeagnus umbellata polysaccharides (EUP, consisting of two fractions, EUP1 and EUP2) were investigated using UV spectrophotometry, high-performance liquid chromatography (HPLC), high-performance gel permeation chromatography (HPGPC), and Fourier transform infrared spectroscopy (FT-IR). This revealed that EUP1 and EUP2 were acidic polysaccharides with an average molecular weight (MW) of 63 and 38 kDa, respectively. EUP1 mainly consisted of L-rhamnose and D-galactose in a molar ratio of 2.05:1, and EUP2 consisted of D-mannose, L-rhamnose, D-galactose, and D-arabinose in a molar ratio of 2.06:1:2.78:1. Furthermore, EUP exhibited considerable antioxidant potential for scavenging hydroxyl, superoxide anion, DPPH, and ABTS radicals. Therefore, EUP can be developed as a potential antioxidant for the functional food or pharmaceutical field.


Assuntos
Antioxidantes , Elaeagnaceae , Antioxidantes/farmacologia , Galactose , Ramnose , Espectroscopia de Infravermelho com Transformada de Fourier , Polissacarídeos/farmacologia
10.
Molecules ; 28(18)2023 Sep 12.
Artigo em Inglês | MEDLINE | ID: mdl-37764361

RESUMO

To obtain the optimal process for the enzyme-assisted aqueous extraction of polysaccharides from Acanthopanax senticosus, and study the physicochemical properties of polysaccharides of different molecular weights, the extraction of Acanthopanax polysaccharides was optimized using the BBD response surface test. The polysaccharides with different molecular weights were obtained by ethanol-graded precipitation at 40%, 60%, and 80%, which were presented as ASPS40, ASPS60, and ASPS80. The polysaccharides were analyzed by HPGPC, ion chromatography, FT-IR, UV, SEM, TGA, XRD, Congo red, and I2-KI tests. The antioxidant assay was used to evaluate their antioxidant properties in vitro. The findings demonstrated that the recovery rate of Acanthopanax polysaccharide was 10.53 ± 0.682%, which is about 2.5 times greater compared to the conventional method of hot water extraction. Based on FT-IR, TGA, polysaccharides with different molecular weights did not differ in their structure or thermal stability. The XRD suggests that the internal structure of ASPSs is amorphous. Congo red and I2-KI showed that all three polysaccharides had triple helix structures with longer branched chains and more side chains. Furthermore, the antioxidant results showed the antioxidant activity of polysaccharides is not only related to the molecular weight size but also can be related to its composition and structure. These studies developed a green, and scalable method to produce polysaccharides from Acanthopanax senticosus and evaluated the properties of Acanthopanax polysaccharides of different molecular weights.


Assuntos
Eleutherococcus , Antioxidantes/farmacologia , Vermelho Congo , Peso Molecular , Espectroscopia de Infravermelho com Transformada de Fourier , Polissacarídeos , Água
11.
Molecules ; 28(18)2023 Sep 14.
Artigo em Inglês | MEDLINE | ID: mdl-37764394

RESUMO

Derivatives combining acridine, pyrrole, and thiazolidine rings have emerged as promising candidates in the field of antitumor drug discovery. This paper aims to highlight the importance of these three structural motifs in developing potent and selective anticancer agents. The integration of these rings within a single molecule offers the potential for synergistic effects, targeting multiple pathways involved in tumor growth and progression. Spiro derivatives were efficiently synthesized in a two-step process starting from isothiocyanates and 2-cyanoacetohydrazide. The thiourea side chain in spiro derivatives was utilized as a key component for the construction of the thiazolidine-4-one ring through regioselective reactions with bifunctional reagents, namely methyl-bromoacetate, dietyl-acetylenedicarboxylate, ethyl-2-bromopropionate, and ethyl-2-bromovalerate. These reactions resulted in the formation of a single regioisomeric product for each derivative. Advanced spectroscopic techniques, including 1D and 2D NMR, FT-IR, HRMS, and single-crystal analysis, were employed to meticulously characterize the chemical structures of the synthesized derivatives. Furthermore, the influence of these derivatives on the metabolic activity of various cancer cell lines was assessed, with IC50 values determined via MTT assays. Notably, derivatives containing ester functional groups exhibited exceptional activity against all tested cancer cell lines, boasting IC50 values below 10 µM. Particularly striking were the spiro derivatives with methoxy groups at position 3 and nitro groups at position 4 of the phenyl ring. These compounds displayed remarkable selectivity and exhibited heightened activity against HCT-116 and Jurkat cell lines. Additionally, 4-oxo-1,3-thiazolidin-2-ylidene derivatives demonstrated a significant activity against MCF-7 and HCT-116 cancer cell lines.


Assuntos
Acridinas , Antineoplásicos , Humanos , Pirróis/farmacologia , Tiazolidinas/farmacologia , Espectroscopia de Infravermelho com Transformada de Fourier , Antineoplásicos/farmacologia , Células HCT116
12.
Molecules ; 28(18)2023 Sep 17.
Artigo em Inglês | MEDLINE | ID: mdl-37764446

RESUMO

Non-small-cell lung cancer (NSCLC) is the main cause of cancer-related deaths worldwide, with a low five-year survival rate, posing a serious threat to human health. In recent years, the delivery of antitumor drugs using a nanostructured lipid carrier (NLC) has become a subject of research. This study aimed to develop an apigenin (AP)-loaded nanostructured lipid carrier (AP-NLC) by melt sonication using glyceryl monostearate (GMS), glyceryl triacetate, and poloxamer 188. The optimal prescription of AP-NLC was screened by central composite design response surface methodology (CCD-RSM) based on a single-factor experiment using encapsulation efficiency (EE%) and drug loading (DL%) as response values and then evaluated for its antitumor effects on NCI-H1299 cells. A series of characterization analyses of AP-NLC prepared according to the optimal prescription were carried out using transmission electron microscopy (TEM), differential scanning calorimetry (DSC), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). Subsequent screening of the lyophilization protectants revealed that mannitol could better maintain the lyophilization effect. The in vitro hemolysis assay of this formulation indicated that it may be safe for intravenous injection. Moreover, AP-NLC presented a greater ability to inhibit the proliferation, migration, and invasion of NCI-H1299 cells compared to AP. Our results suggest that AP-NLC is a safe and effective nano-delivery vehicle that may have beneficial potential in the treatment of NSCLC.


Assuntos
Carcinoma Pulmonar de Células não Pequenas , Neoplasias Pulmonares , Humanos , Carcinoma Pulmonar de Células não Pequenas/tratamento farmacológico , Apigenina/farmacologia , Projetos de Pesquisa , Espectroscopia de Infravermelho com Transformada de Fourier , Neoplasias Pulmonares/tratamento farmacológico , Excipientes
13.
Chemosphere ; 341: 140086, 2023 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-37678593

RESUMO

Both environment and human beings were menaced by the widespread application of radioactive uranium, high-performance and effective elimination of uranium from wastewater is of important meaning for development of environmental sustainability in the future. In this study, the water-stable MOF material and the highly crystalline COF were compounded by a mild hydrothermal strategy, which achieved efficient removal of U(VI) through the synergistic effect. The composites showed the characteristics of both COFs and MOFs, which will possess higher stability, larger surface area and faster adsorption efficiency that cannot be carried out by a single component. Batch experiments and characterizations (SEM, TEM, XRD, FT-IR, BET, XPS, etc.) indicated that UiO-66-NH2@LZU1 had more stable and multi-layer pore structure and rich active functional groups. The Langmuir model and the pseudo-second-order kinetics fitting was more suitable for the U(VI) elimination process. The greatest uranium adsorbing capacity of UiO-66-NH2@LZU1 (180.4 mg g-1) was observed to exceed the UiO-66-NH2 (108.8 mg g-1) and COF-LZU1 (65.8 mg g-1), which reached the excellent hybrid effects. Furthermore, FT-IR and XPS analyses confirmed that the most nitrogen-containing group from COF-LZU1 and oxygen-containing group of UiO-66-NH2 could be combined with U(VI). In addition, electrostatic interaction was also a mechanism during the removal process. This work displayed that UiO-66-NH2@LZU1 was a prospective hybrid material for radioactive waste remediation. The compound method and application mentioned in this work had provided a theoretical basis for designing and developing multi-functional composite adsorbents, which contributed to the development of new materials for radioactive wastewater treatment technologies.


Assuntos
Urânio , Humanos , Estudos Prospectivos , Espectroscopia de Infravermelho com Transformada de Fourier , Adsorção
14.
J Chromatogr A ; 1708: 464340, 2023 Oct 11.
Artigo em Inglês | MEDLINE | ID: mdl-37660561

RESUMO

Three structurally similar silane reagents with different terminal groups were prepared and bonded to silica to obtain three structurally similar stationary phases (Sil-Ph-COOH, Sil-Phe and Sil-Ph-NH2). The prepared stationary phases were characterized through elemental analysis (EA) and Fourier Transform Infrared Spectroscopy (FT-IR). These three stationary phases provided acceptable retention repeatability (relative standard deviations between 0.08% and 0.13%) and high column efficiency (7.3 × 104 plates/m for uridine on Sil-Phe). The retention behavior of the three columns was investigated under different chromatographic conditions including different mobile phase ratio, salt concentration, pH etc. The retention mechanisms were explored by linear solvation energy relationships and Van't Hoff plots. Applications in separation under reversed phase liquid chromatography (RPLC), hydrophilic interaction liquid chromatography (HILIC) and ion exchange chromatography (IEC) mode were investigated. The results showed that the retention capacity of the stationary phases with different terminal groups to the analytes is very different, especially for carboxylic acids, because the surface charges of amino groups and carboxyl groups under weakly acidic conditions produce different electrostatic effects with dissociated carboxylic acids. Finally, the Sil-Phe column was employed to detect ibuprofen extracted from pharmaceutical ibuprofen capsules and vitamins extracted from vitamin tablets.


Assuntos
Ibuprofeno , Vitaminas , Cromatografia Líquida de Alta Pressão , Espectroscopia de Infravermelho com Transformada de Fourier , Cromatografia Líquida , Ácidos Carboxílicos
15.
J Chromatogr A ; 1708: 464334, 2023 Oct 11.
Artigo em Inglês | MEDLINE | ID: mdl-37660560

RESUMO

A novel three-dimensional covalent organic framework (3D-COF) with content-tunable and active hydroxyl groups (OH) on the pore walls was developed and adopted for the high-performance capture of okadaic acid (OA) marine toxins. Using pore-surface engineering, the integration of linear building blocks (4,4'-diamino-3,3'-biphenyldiol, BD(OH)2 and benzidine, BD) with the 3D structural building block backbone (4,4',4'',4'''-methane-tetrayltetrabenzaldehyde, TFPM) was achieved. By adjusting the ratio of BD(OH)2, functional multicomponent-COFs [OH]x-BD-TFPM COFs (X = 25%) were synthesized, which offered ideal access to convert a conventional COF into a functional platform with multiple-mode interactions of hydrophobic and hydrophilic groups for OA capture. [OH]x-BD-TFPM was characterized using SEM, XRD, FT-IR, and BET. The adsorption features and analytical performance of OA were screened and evaluated. Optimization of dispersive solid-phase extraction using [OH]25-BD-TFPM was accomplished, and the method was verified for sensitive quantitative detection of OA in clam and mussel samples. Coupled with LC-MS/MS, the resultant [OH]25-BD-TFPM COF demonstrated the ability to analyze OA, and the limit of detection for OA in shellfish was determined to be 0.005 µg/kg. A significant improvement in trace OA detection was observed compared to previously reported SPE materials without adjustable hydrophilic interactions. The recoveries of OA in the fortified clam and mussel samples were in the ranges of 93.9‒105.1% and 96.7‒110.2%, respectively. This study highlights that OH-group surface engineering in channel walls is a facile and powerful strategy for developing functional 3D-COFs with multiple interactions for high-performance target capture.


Assuntos
Estruturas Metalorgânicas , Ácido Okadáico , Cromatografia Líquida , Espectroscopia de Infravermelho com Transformada de Fourier , Espectrometria de Massas em Tandem
16.
J Chromatogr A ; 1708: 464358, 2023 Oct 11.
Artigo em Inglês | MEDLINE | ID: mdl-37708671

RESUMO

Lakadong turmeric has been outlined for its high content of curcuminoids across the globe. Three significant molecular markers are widely present in turmeric viz, curcumin, desmethoxycurcumin, and bisdemethoxycurcumin, and they are present very high amount in Lakadong turmeric. Curcuminoids have been reported for structural and spectrum similarity of 3 to 4 nm (432, 434, and 436 nm, respectively). Current purification methods are based on recrystallisation where it is difficult to get highly pure material and preparative methods associated with tedious separation with high cost. Lakadong turmeric has not been explored commercially since long time. No reports are available in the literature with highly pure reference materials with in-depth characterization data and purity assessment. Curcumin, desmethoxycurcumin, and bisdemethoxycurcumin were characterized using different analytical techniques viz, UV-Visible Spectroscopy, Fourier Transform Infrared Spectroscopy (FT-IR), Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA), Proton Nuclear Magnetic Resonance (1HNMR), Carbon-13 Nuclear Magnetic Resonance (13CNMR), High-Resolution Mass Spectrometry (HR-MS) and Inductive Coupled Plasma Mass Spectrometry (ICP-MS). Purified 3 markers has shown High-Performance Liquid Chromatography-Diode Array Detector (HPLC-DAD) purity more than 99.5%. DSC the melting peaks of curcumin, desmethoxycurcumin and bisdemethoxycurcumin were observed at 168 °C, 165 °C, and 210 °C, respectively. These plant-based markers have high commercial potential as reference material for routine Quality Assurance and Quality Control (QAQC) in herbal industries.


Assuntos
Curcumina , Curcuma , Espectroscopia de Infravermelho com Transformada de Fourier , Diarileptanoides , Índia
17.
J Environ Manage ; 345: 118755, 2023 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-37716197

RESUMO

In this study, a number of leaching solutions (H2SO4, CuSO4 and NaCl) and an electrochemical method were used together for the separation of Cu from waste printed circuit boards. Secondly, the magnetic-MOF(Cu) was synthesized using the Cu recovered from waste printed circuit boards. Thereafter, TiO2/mag-MOF(Cu) composite was prepared and its photocatalytic activity was assessed in the photo degradation of two prominent organophosphorus pesticides, namely malathion (MTN) and diazinon (DZN). The catalytic structure of the MOF-based composite was fully characterized by various analyses such as XRD, SEM, EDAX, FT-IR, VSM and UV-vis. The obtained analyses confirmed the successful synthesis of TiO2/mag-MOF(Cu) composite. The synthesized composite exhibited highly efficient in the degradation of both pollutants under the following conditions: pH 7, contaminant concentration 1 mg/L, the catalyst dosage of 0.4 g/L, visible light intensity 75 mW/cm2 and reaction time of 45 min. First order kinetic model was best suited with the experimental results (R2: 0.97-0.99 for different MTN and DZN concentrations). Trapping studies revealed that superoxide radicals (O2•-) played an important role during the degradation process. Furthermore, the catalyst demonstrated a superb recovery as well as high stability over five cyclic runs of reuse. In addition, the total organic carbon (TOC) analysis showed over 83% and 85% mineralization for MTN and DZN, respectively. The combined system of TiO2/mag-MOF(Cu)/Vis also exhibited a great level of efficiency and feasibility in the treatment of tap water and treated wastewater samples. It is concluded that TiO2/mag-MOF(Cu) could be used as an excellent catalyst for the photodegradation of MTN and DZN in aqueous solution.


Assuntos
Nanocompostos , Praguicidas , Cobre , Compostos Organofosforados , Espectroscopia de Infravermelho com Transformada de Fourier , Metais , Diazinon , Malation , Luz
18.
Sci Rep ; 13(1): 15498, 2023 09 19.
Artigo em Inglês | MEDLINE | ID: mdl-37726341

RESUMO

Shape, size, composition, and function of the bones in the human body vary on the macro, micro and nanoscale. This can influence changes caused by taphonomy and post-mortem preservation, including DNA. Highly mineralised compact bone is less susceptible to taphonomic factors than porous trabecular bone. Some studies imply that DNA can be better preserved in trabecular bone, due to remnants of the soft tissue or bacteria better digesting organic matter while not digesting DNA. The aim of this study was to understand the differences between compact (diaphyses) and trabecular (epiphyses) bone on a molecular level and thus the reasons for the better preservation of the DNA in the trabecular bone. The powder obtained from epiphyses and diaphyses of metacarpals and metatarsals was analysed using ATR-FTIR spectroscopy and compared. Samples with poorest DNA preservation originated from diaphyses, predominantly of metatarsals. They were characterised by higher concentrations of phosphates and crystallinity, while lower collagen quality in comparison to samples with the best DNA preservation. Epiphyses presented higher concentrations of better-preserved collagen while diaphyses had higher concentrations of carbonates and phosphates and higher crystallinity. Due to better-preserved collagen in the epiphyses, the soft tissue remnants hypothesis seems more likely than the bacteria hypothesis.


Assuntos
Ossos Metacarpais , Ossos do Metatarso , Humanos , Osso Esponjoso , Espectroscopia de Infravermelho com Transformada de Fourier , DNA , Fosfatos , Proteínas Mutadas de Ataxia Telangiectasia
19.
J Mater Sci Mater Med ; 34(10): 47, 2023 Sep 21.
Artigo em Inglês | MEDLINE | ID: mdl-37735291

RESUMO

Numerous infections are linked to Pseudomonas aeruginosa. It is one of the major medical concerns because of virulence and antibiotic resistance. Antibiotic encapsulation in liposomes is a good strategy for controlling infections caused by this microorganism. Evaluation of anti-Pseudomonas aeruginosa effect of liposomal form of Imipenem/Cilastatin in vitro condition. By using the disk agar diffusion technique, the isolates' pattern of antibiotic resistance was identified. The antibiotic was placed into the nanoliposome after it had been made using the thin layer and ethanol injection techniques. SEM and DLS were used to determine the size, shape, and zeta potential of the encapsulated drug form and the empty nanoliposome. Additionally, Imipenem/Cilastatin encapsulation in nanoliposomes was studied using FT-IR spectroscopy. In the microbial assay experiments the MIC, MBC and MBEC of liposomal and free drug forms were determined. The nanoparticles were spherical, with a diameter ranging from 30 to 39 nm, and the EE% in the thin layer and ethanol injection procedures were 97 and 98, respectively. Imipenem/Cilastatin nanoliposomes showed peaks at 3009 cm-1 and 1650 cm-1, demonstrating the thermodynamic stability for the chemical structure of the drug enclosed and validating the encapsulation of antibiotic in the nanoliposomes. When compared to free drug forms, nanoliposomes had lower MIC and MBC values in the majority of the isolates and had a greater ability to eradicate the biofilm formation. It was shown that the two nanoliposome preparation techniques were more efficient in 80% of the isolates, which had outcomes that were consistent with those of numerous other investigations. Overall, we demonstrated that the antibacterial activity of nanoliposomes was higher than that of the free drug form based on the evaluation of their MIC and MBC. Pharmaceutical nanoliposome techniques provide an excellent future perspective on how to manage microbial infections that are resistant to antibiotics.


Assuntos
Antibacterianos , Pseudomonas aeruginosa , Espectroscopia de Infravermelho com Transformada de Fourier , Combinação Imipenem e Cilastatina , Antibacterianos/farmacologia , Etanol , Lipossomos , Biofilmes
20.
Int J Mol Sci ; 24(18)2023 Sep 19.
Artigo em Inglês | MEDLINE | ID: mdl-37762603

RESUMO

The present study investigates the relationship between the local structure, photocatalytic ability, and cathode performances in sodium-ion batteries (SIBs) and lithium-ion batteries (LIBs) using Ni-substituted goethite nanoparticles (NixFe1-xOOH NPs) with a range of 'x' values from 0 to 0.5. The structural characterization was performed applying various techniques, including X-ray diffractometry (XRD); thermogravimetry differential thermal analysis (TG-DTA); Fourier transform infrared spectroscopy (FT-IR); X-ray absorption spectroscopy (XANES/EXAFS), both measured at room temperature (RT); 57Fe Mössbauer spectroscopy recorded at RT and low temperatures (LT) from 20 K to 300 K; Brunauer-Emmett-Teller surface area measurement (BET), and diffuse reflectance spectroscopy (DRS). In addition, the electrical properties of NixFe1-xOOH NPs were evaluated by solid-state impedance spectroscopy (SS-IS). XRD showed the presence of goethite as the only crystalline phase in prepared samples with x ≤ 0.20, and goethite and α-Ni(OH)2 in the samples with x > 0.20. The sample with x = 0.10 (Ni10) showed the highest photo-Fenton ability with a first-order rate constant value (k) of 15.8 × 10-3 min-1. The 57Fe Mössbauer spectrum of Ni0, measured at RT, displayed a sextet corresponding to goethite, with an isomer shift (δ) of 0.36 mm s-1 and a hyperfine magnetic distribution (Bhf) of 32.95 T. Moreover, the DC conductivity decreased from 5.52 × 10-10 to 5.30 × 10-12 (Ω cm)-1 with 'x' increasing from 0.10 to 0.50. Ni20 showed the highest initial discharge capacity of 223 mAh g-1, attributed to its largest specific surface area of 174.0 m2 g-1. In conclusion, NixFe1-xOOH NPs can be effectively utilized as visible-light-activated catalysts and active cathode materials in secondary batteries.


Assuntos
Minerais , Nanopartículas , Espectroscopia de Infravermelho com Transformada de Fourier , Eletrodos
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