cometadata/datacite-titles-descriptions-related-identifiers huggingface dataset:
DOI: 10.6084/m9.figshare.14303966.v1
title: Optimization and Validation of LLE-LTP and QuEChERS Methodologies for Determining 2,4-D in Water Samples

description: 2,4-Dichlorophenoxyacetic acid (2,4-D) has been one of the main herbicides used to control weeds, however, due to its high use it can promote episodes of environmental contamination. Therefore, this study aimed to optimize and validate the liquid-liquid extraction with low-temperature partition (LLE-LTP) and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) methods for determining 2,4-D in water samples by high performance liquid chromatography with diode array detector. The recovery percentages of the two methodologies were close to 100 ± 3%, and the limits of quantification were 2.0 and 3.1 µg L-1 for LLE-LTP and QuEChERS, respectively. The methodologies were selective and presented linearity from 2.0-26.0 and 3.1-40.6 µg L-1 for LLE-LTP and QuEChERS, respectively. The LLE-LTP was better than QuEChERS due to a smaller number of steps, lower reagent consumption, higher concentration factor and a lower limit of quantification. The real samples did not reveal any environmental contamination episodes by 2,4-D.
DOI: 10.6084/m9.figshare.14303964.v1
title: Effects of Temperature and Concentration on the Determination of PET Viscosity

description: This work describes the use of experiment planning to investigate the effects of the variables temperature and concentration of the polymer solution on the viscosity test of polyethylene terephthalate (PET). For this, the response surface methodology was based on a central composite rotatable design (CCRD) to optimize the combinations of the analytical conditions. With the analysis of the standard sample of PET with intrinsic viscosity of 0.630 ± 0.008 dL g-1 and 2-chlorophenol solvent, it was observed that the solution flow temperature and PET concentration caused significant effects on the results, while the storage temperature of the solvent was not statistically significant. With the results and the model developed, an industrial solid state polymerization process of PET was evaluated with simulations of the production of 30 tons of PET, demonstrating the importance of controlling the variables to guarantee the performance in quality control laboratories.
DOI: 10.6084/m9.figshare.14303963.v1
title: Synthesis, Characterization, Absorption and Fastness Properties of Novel Monoazo Dyes Derived from 1-Phenyl-3-amino-4-(2-thiazolilazo)pyrazol-5-one

description: Monosubstitute thiazolyl amines were diazotized in acetic acid, coupled to 1-phenyl-3-aminopyrazol-5-one (1a-1c) and acetylated to obtain the 2a-2c dyes. The dyes were characterized by elemental analysis and spectroscopic (Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR), ultraviolet (UV)) methods. The effects on the visible absorption spectra of the substituents present, solvents, pH, concentration and temperature were investigated in detail. Tautomerism of the dyes were investigated by spectroscopic methods. Fastness properties of dyes were studied using the standard method for the assessment of color fastness of textile.
DOI: 10.6084/m9.figshare.14303961.v1
title: Omega-3 and Omega-6 Determination in Nile Tilapia’s Fillet Based on MicroNIR Spectroscopy and Multivariate Calibration

description: Tilapia (Oreochromis niloticus) is the most cultivated fish species in Brazil. Studies have shown that fish consumption is related to the prevention of cardiovascular diseases due to its high contents of polyunsaturated fatty acids, as omega-3 (n-3) and omega-6 (n-6). In this sense, a new method to determine omega-3 and omega-6 by near-infrared (NIR) spectroscopy and multivariate calibration based on partial least squares (PLS) was proposed. Spectra of fillets of Nile tilapias packed under vacuum were obtained and compared to the reference method (gas chromatography) used for quantification of fatty acids. The outliers were evaluated in the models that were validated by calculation of the parameters for model performance estimation, showing promising results. The appropriate values achieved for accuracy, limits of detection and quantification, indicate that the NIR/PLS models can be an alternative to chromatography in the determination of omega-3 and omega-6 in fillets of Nile tilapia. Furthermore, the spectra acquisition on the vacuum-packed fillet contributes to the NIR/PLS method in terms of cost and quickness.
DOI: 10.6084/m9.figshare.14303959.v1
title: New Magnetic Fe Oxide-Carbon Based Acid Catalyst Prepared from Bio-Oil for Esterification Reactions

description: In this work, bio-oil (an organic matrix rich in oxygen functionalities) was used to efficiently dissolve and disperse Fe3+ which upon thermal treatment produced a carbon containing dispersed and encapsulated Fe oxide magnetic nanoparticles. These materials were prepared by dissolution of 8, 16 and 24 wt.% Fe3+ salt in bio-oil followed by treatment at 400, 450, 500 or 600 ºC in N2 atmosphere. X-ray diffraction (XRD), scanning (SEM) and transmission electron microscopies (TEM), elemental analysis, thermogravimetric-mass spectrometry (TG-MS), potentiometric titration, Raman and Mössbauer spectroscopies showed that Fe3+ species in bio-oil is reduced to produce magnetic nanoparticles phases: magnetite Fe3O4 and maghemite γ-Fe2O3. At low temperatures, the iron phases were less protected, and the carbon matrix was more reactive, while in temperatures above 500 ºC, the iron phases were more stable, however, the carbon matrix was less reactive. Reaction of these magnetic carbon materials with concentrated H2SO4 produced surface sulfonic acidic sites (ca. 1 mmol g-1), especially for the materials obtained at 400 and 450 ºC. The materials were used as catalysts on esterification reaction of oleic acid with methanol at 100 ºC and conversions of 90% were reached, however, after 2 consecutive uses, the conversion decreased to 30%, being required more studies to improve the material stability.
DOI: 10.6084/m9.figshare.14303957.v1
title: Electroanalytical Method for Determination of Trace Metals in Struvite Using Electrochemically Treated Screen-Printed Gold Electrodes

description: We present an electroanalytical method using square-wave anodic stripping voltammetry on electrochemically-treated screen-printed gold electrodes to the simultaneous determination of lead(II), copper(II) and mercury(II) in struvite (natural fertilizer produced from urine). Electrochemical treatment via cyclic voltammetry of the working electrodes increased surface rugosity that improved the electroanalytical responses for the three metals. Under optimized conditions and using a deposition time of 90 s, the proposed method presented the following limit of detection values: 1.3 µg L-1 for lead(II), 2.0 µg L-1 for copper(II) and 0.9 µg L-1 for mercury(II). Struvite samples were easily dissolved in supporting electrolyte solution (0.05 mol L-1 HCl). Satisfactory recovery values between 91 and 111% were obtained for the analysis of spiked samples. Hence, we can infer that the proposed electroanalytical method is an effective alternative for the determination of trace metals, since it provides precise and accurate direct analyses, with rapid responses without interference from sample matrix and enabling in field analysis.
DOI: 10.6084/m9.figshare.14303955.v1
title: Accessing Basic Sites on Modified CoFe2O4 Nanoparticles: Addressing the Selective Oxidation of Benzyl Alcohol and Unraveling the Au:Pd Ratio Effects by XPS

description: AuPd nanoparticles have gained substantial attention due to their application in selective oxidation of alcohols. However, due to the radical nature of the oxidation of benzyl alcohol, under specific conditions, even without a catalyst, the reaction occurs and affects the selectivity of the system. Therefore, we aimed to develop a catalyst that enables the control of the oxidation leading to higher reaction selectivity. To accomplish this, we have prepared a catalytic support comprised of CoFe2O4 nanoparticles impregnated with Sr(OH)2 that presented a significant control of the reaction selectivity without any metal or external base addition. After the impregnation of AuPd nanoparticles in a specific ratio, the reaction reached a selectivity of &gt; 99% for benzaldehyde, in 3.5 h, with a recycle regime of five runs without loss of activity and selectivity. Our results show that the judicious choice of the ratio of the metals prevents the necessity of manipulating the reaction conditions to improve the performance of the system. Additionally, studies under N2 and O2 environments, with or without water, confirmed the role of the O2 in the system. Holding all this information, we propose a possible mechanism for the prepared system.
DOI: 10.6084/m9.figshare.14303948.v1
title: Phytochemical Analysis, Multi-Element Composition and Biological Activities of Extracts and Lupenone from Albizia inundata (Mart.) Barneby & J.W.Grimes

description: In this study, antimicrobial activity of extracts and lupenone from A. inundata (Fabaceae, Mimosoideae), were tested. In addition, the multi-element composition of the leaves, bark and stems (heartwood) of A. inundata was evaluated using inductively coupled plasma optical emission spectrometry (ICP OES). Lupenone was isolated in the petroleum ether extract of leaves, for the first time. Biological assays were conducted to evaluate the antimicrobial (antibacterial, antifungal and antiparasitic) of extracts, their fractions and lupenone. The results showed antimicrobial and antileishmanial activity of these compounds, which may be useful for obtaining a chemical composition and biological activity database on Albizia species. For multi-element composition, we found the mean concentrations (minimum-maximum) of Al, Ca, Cr, Cu, Fe, K, Mg, Mn, Ni, P, V and Zn in the samples ranged between 0.06 and 265.41 µg g-1. Concentration ranges of Cu, Fe, Mn and Zn are large, which makes these samples as additional sources of these macronutrients.
DOI: 10.6084/m9.figshare.14303945.v1
title: New Insights into the Partitioning of Phenothiazine Dyes in Aqueous Two-Phase Systems

description: Aqueous two-phase systems (ATPSs) have proven to be efficient and environmentally safe methods for extracting chemical species. However, the driving forces behind the partition of solutes in these systems are still little understood. A complete thermodynamic partitioning of phenothiazine dyes was investigated in poly(ethylene oxide) (PEO) + salt + water ATPSs. Standard transfer parameters (Gibbs free energy change (ΔtrGº), enthalpy change (ΔtrHº) and entropy change (TΔtrSº)) were evaluated, and their dependence on the dye structure, electrolyte nature and tie line length (TLL). All phenothiazine dyes are concentrated predominantly in the polymer enriched phase, with ΔtrGº values ranging from -4.1 up to -13.4 kJ mol-1. Due to the dye-PEO attractive interactions that occur mainly via benzene condensed ring present in the structures of phenothiazine dyes, the partitioning of these dyes was enthalpically driven, with -11.4 ≥ ΔtrHº ≥ -52 kJ mol-1 and -4.93 ≥ TΔtrSº ≥ -38 kJ mol-1.
DOI: 10.6084/m9.figshare.14303943.v1
title: Expeditious Syntheses to Pharmochemicals 1,3-Dihydroxyacetone, 1,3-Dichloro-, 1,3-Dibromo- and 1,3-Diiodoacetone from Glycerol 1,3-Dichlorohydrin Using Homogenous and Heterogenous Medium

description: New efficient and reproductive routes to production of 1,3-dihydroxyacetone (1), 1,3-dichloroacetone (6), 1,3-dibromoacetone (7) and 1,3-diiodoacetone (8) from glycerol 1,3-dichlorohydrin (3) were developed. The synthesis of 1 was processed in three steps from glycerol 2 (1,3-selective chlorination of 2 to 3, oxidation of 3 to 6 and subsequent di-hydroxylation) in 51% overall yield. On the other hand, 7 and 8 were produced from3, via a trans-bromination and trans-iodination, respectively, followed by oxidation and hydroxylation steps, in 38-52% overall yield. It was used homogeneous media with different reagents (HCl/AcOH, pyridinium chlorochromate (PCC), PCC-HIO4) and heterogeneous media with reagents supported on polymer resins such as Amberlyst® A26-HCrO4– form, PV-PCC (polyvinyl-pyridinium chlorochromate) and Amberlyst® A26-OH- form or reagents supported on alumina such as KI/Al2O3, KBr/Al2O3, in solvent free conditions.
DOI: 10.6084/m9.figshare.14303942.v1
title: Mechanistic Investigation of DBU-Based Ionic Liquids for Aza-Michael Reaction: Mass Spectrometry and DFT Studies of Catalyst Role

description: 1,8-Diazabicyclo[5.4.0]undec-7-ene (DBU)-based ionic liquids (ILs) has exhibited a high catalytic activity in the aza-Michael reactions compared to conventional catalysts and with imidazole-based ILs. In the present work DBU-based ILs showed high catalytic potential for aza-Michael addition of aromatic amines to 2-cyclohexen-1-one under solvent-free condition. Electrospray ionization-mass spectrometry (ESI-MS) and density functional theory studies have been carried out to provide an effective activation mode of DBU-based ILs in aza-Michael addition. Our results show that both the presence of the acid hydrogen in the IL and the ability of the anion to carry out a hydrogen bond with the −NH2 group of the arylamine are fundamental for the reaction catalysis. The catalytic model proposed can be used for the rational development of new ILs with excellent catalytic properties.
DOI: 10.6084/m9.figshare.14303940.v1
title: Synthesis and Evaluation of Nematicidal Activity of Compounds Derived from Norbornadiene

description: Nematode is a major problem in agriculture, the effective way to control this pest is through chemical control, but the efficient molecules present in the market have great toxicity to mammals and birds. Thus, there is a constant demand for the development of new nematicide molecules. This study describes the synthesis of 21 novel esters derived from norbornadiene and evaluation of their potential activity against Meloidogyne javanica. The esters 5-25 presented 50% mortality of the nematodes. The acid 3 and the ester 4 caused 96 and 93% mortality of the nematodes, respectively. The lethal concentration to kill 50% of the nematodes (LD50) were determined as being 11.8 µg mL-1 for the acid 3 and 99.4 µg mL-1 for the ester 4. According to the results obtained it is believed that polarity seems to be a key factor for the higher activity of compound 3 compared to structurally similar ester derivatives.
DOI: 10.6084/m9.figshare.14303939.v1
title: A Simple Fluorescent Chemosensor for Detection of Zinc Ions in Some Real Samples and Intracellular Imaging in Living Cells

description: A new designed fluorescent chemosensor TYMN ((E)-1-((thiazol-2-ylimino)methyl)naphthalen-2-ol) for highly sensitive and selective tracing of trace amount of Zn2+ ions in some real samples was synthesized and characterized. The sensor TYMN can detect Zn2+ ions via fluorescence enhancement with a high selectivity over a wide range of metal ions, especially Cd2+. The sensor showed large fluorescence enhancement upon complexation with Zn2+ and simultaneous color change from yellow to orange. The limit of detection was analyzed to be 0.0311 μM with a linear dynamic range 0.1-1.0 μM. The sensor could work in a pH span of 5.0-8.0. Based on the physicochemical and analytical methods like electrospray ionization (ESI)-mass, Job plot, 1H nuclear magnetic resonance (NMR) and theoretical calculations, the detection mechanism for Zn2+ was explained based on restriction of internal charge transfer (ICT) mechanism. TYMN sensor was potentially utilized for Zn2+ ions concentration evaluation in some real samples. Fluorescence microscopy experiments revealed that probe TYMN may have application as a fluorophore to detect the Zn2+ in living cells.
DOI: 10.6084/m9.figshare.14303937.v1
title: Copaifera multijuga, Copaifera pubiflora and Copaifera trapezifolia Oleoresins: Chemical Characterization and in vitro Cytotoxic Potential against Tumoral Cell Lines

description: Copaifera species (Fabaceae) comprises approximately 70 species of large trees, from which 16 can be found in Brazil. The oleoresins obtained from their trunk are widely used in Brazilian folk medicine, which display important antitumoral potential. Chemically, these oleoresins are mainly composed of a mixture of sesquiterpenes and diterpenes. In this paper we are describing the isolation and identification of 12 already known terpenes from oleoresins obtained from three different Copaifera species (C. multijuga, C. pubiflora and C. trapezifolia) and 2 novel diterpenes (ent-16-hidroxy-3,13 clerodadien-15,18-dioic acid and ent-labda-5,13-dien-15-oic acid) from C. trapezifolia. Both new compounds were identified by nuclear magnetic resonance (NMR) spectroscopic (1H and 13C NMR, correlation 1H-1H (COSY), heteronuclear multiple quantum coherence (HMQC) and heteronuclear multiple bond correlation (HMBC)) and by high-resolution electrospray ionization mass spectrometry (HR-ESIMS) analyses. The cytotoxic potential of these oleoresins, their main non-volatile compounds and their volatile compound fractions were evaluated against a panel of tumoral (MCF-7, ACP01, A549, HeLa) and normal cell lines (MCF-10A, GM07492-A) through XTT (tetrazolium salt) and SRB (sulforhodamine B) assays. The novel diterpene ent-labda-5,13-dien-15-oic acid displayed relevant cytotoxic effect against most of the cancer cell lines with mean inhibitory concentration (IC50) values ranging from 3.57 ± 1.12 to 22.56 ± 1.03 µg mL-1, and a high selectivity level in both assays.
DOI: 10.6084/m9.figshare.14303936.v1
title: Determination of Ethanol in Gel Hand Sanitizers Using Mid and Near Infrared Spectroscopy

description: Alcohol-based gel hand sanitizers became very popular during the COVID-19 (coronavirus disease 2019) pandemic. In Brazil, several irregular factories emerged requiring an efficient control by the police and regulatory agencies to guarantee product quality. This problem required a method to determine ethanol content, which led to the development of two methods employing mid and near infrared spectroscopy associated with chemometrics. Partial least squares (PLS) models were built and presented satisfactory results with mean absolute percentage error of prediction and root mean square error of prediction (RMSEP) of 1.12 and 0.76% (m/m), respectively, for mid-infrared (MIR) and 1.83 and 1.18% (m/m) for near-infrared (NIR). The analysis of commercial and seized samples of hand sanitizers showed that only 7 out of 34 samples had an ethanol content of 70% (m/m) or higher. This result reinforces the need for constant vigilance by authorities to ensure that the products have the required specifications.
DOI: 10.6084/m9.figshare.14303934.v1
title: A New Isoflavone and Other Constituents from Roots of Clitoria guianensis

description: A new isoflavone named pratensein-7-O-β-D-rutinoside [(-)-7-O-α-L-rhamnopyranosyl-(1→6)-β-D-glucopyranosyl-5,3’-dihydroxy-4’-methoxyisoflavone] and the known compounds biochanin A-7-O-β-D-rutinoside, 6-deoxyclitoriacetal 11-O-β-D-glucopyranoside, 6-deoxyclitoriacetal, (2S)-naringenin-6-C-β-D-glucopyranoside, (2R)-naringenin-6-C-β-D-glucopyranoside, tachioside, and koaburaside were isolated from the roots of Clitoria guianensis (Aubl.) Benth var. guianensis (Fabaceae), a subshrub found in the Brazilian Cerrado biome. The structures of the compounds were identified by physical and spectroscopic data measurements (specific rotation ([α]D), circular dichroism (CD), ultraviolet (UV), infrared (IR), 1D and 2D nuclear magnetic resonance (NMR), and mass spectrometry (MS)). The EtOAc fraction of the roots exhibited high toxicity against Artemia salina with median lethal dose (LD50) value of 8.53 mg L-1.
DOI: 10.6084/m9.figshare.14303932.v1
title: Chemical and Spectroscopic Characteristics of Anthrosol (Amazonian Dark Earth) and Surrounding Soil from the Brazilian Amazon Forest: Evaluation of Mineral and Organic Matter Content by Depth

description: The chemical and spectroscopic characteristics of soil organic matter (SOM) isolated from Amazonian dark earth (ADE) and surrounding soil (SR) were evaluated according to the soil depth. The results showed opposite trends for the soils. While ADE featured SOM with a greater aromatic condensation degree and greater hydrophobicity in the top layer, the SR showed more aliphatic and polar SOM. The SOM arrangement from ADE was less hydrophobic, aromatic, and more polar in depth. In contrast, the SOM from SR showed an increase in molecular weight and hydrophobicity. Besides the aromatic protection in the SOM from ADE, there was organo-mineral protection through binding to soil minerals. This suggested that the SOM from ADE was protected by its hydrophobicity and interaction with minerals compared with that from the SR, thereby showing that the combination of both characteristics is important to create new technologies for soil carbon storage.
DOI: 10.6084/m9.figshare.14303931.v1
title: Synthesis of ZnO Nanoparticles by the Sol-Gel Protein Route: A Viable and Efficient Method for Photocatalytic Degradation of Methylene Blue and Ibuprofen

description: The photocatalytic degradation of methylene blue dye and ibuprofen drug was studied in the presence of zinc oxide, synthetized by the protein sol-gel route. The catalyst, calcined at 1000 ºC, presented a tendentious morphology to filaments characteristic of ZnO crystalline, characterized by X-ray diffraction (XRD) and confirmed by the presence of Zn energy band in X-ray photoelectron spectrometer (XPS). The result of ultraviolet (UV) light photodegradation of this work is comparable to others that made use of more complex routes, considering the degradation of 97% of methylene blue dye solution and the solution of the ibuprofen drug reached 60% of degradation after 1 h of light incidence. In this research, it is possible to report good degradation results, and the research differential is a material made with a simple and less aggressive route, capable of generating a stable and efficient material.
DOI: 10.6084/m9.figshare.14303928.v1
title: New Synthetic Quinolines as Cathepsin K Inhibitors

description: Cathepsin K is a papain-like cysteine protease and is responsible for collagen degradation in bone tissue and thus represents an important target for the development of new therapies for treating diseases such as osteoporosis. Quinolines are an important class of heterocyclic molecular leads with a great pharmacological potential and represent a relevant scaffold to explore the chemical space of cathepsin K (CatK) inhibitors. This study presents the synthesis of nine 2,4-diphenylquinolines, including five phthalonitrile quinolines dyads, and the evaluation of their CatK inhibitory activity. Among the evaluated compounds, 4b was the most potent inhibitor with an IC50 (half-maximal inhibitory concentration) value of 1.55 µM (against Z-Phe-Arg-MCA substrate) acting in an uncompetitive inhibition mode. Molecular docking studies provided important information on the interaction of the inhibitor with the enzyme showing that these quinoline derivatives can play an important role as CatK inhibitors.