cometadata/datacite-titles-descriptions-related-identifiers huggingface dataset:
DOI: 10.6084/m9.figshare.14304117.v1
title: Study of Inorganic Profiles of Street Cocaine Samples Using ICP-MS and ICP OES

description: Determining inorganic constituents in illicit drugs can indicate its purity and presence of adulterants. In this study, we analyzed 52 street cocaine samples, seized in three different regions of Espírito Santo, state of Brazil. Inductively coupled plasma optical emission spectrometry was used to determine Al, Ca, Cu, Fe, Mn, Mg, Zn concentrations and inductively coupled plasma mass spectrometry to determine Mo, Co, Pb and P concentrations. From analyte recovery tests, the accuracy was considered acceptable and the proposed method satisfactory. Most of the samples exhibited a relatively homogeneous inorganic profile with similar concentrations of investigated elements, however some samples had very discrepant concentrations. High concentrations of Al, Ca, Fe, Mg, Mn, and P were found, indicating that adulterants such as gypsum, marble powder, limestone, cement, and others must be used to increase the profitability of the illicit drug market.
DOI: 10.6084/m9.figshare.14304116.v1
title: Interaction of Suspended Particulate Material with Cd2+ and Pb2+ in a Brazilian Lagoon Estuarine System

description: The suspended particulate material (SPM) present in waters has fundamental importance for a better understanding of environmental behaviors of aquatic pollutants. This work determined the physicochemical parameters (pH, temperature, conductivity, total organic carbon and metals concentration) in water samples from Mundaú-Manguaba estuarine-lagoon system, Alagoas, Brazil. This work extracted and characterized the organic matter present in SPM in this estuary and studied the interaction of this organic matter with potentially toxic metals (Cd2+ and Pb2+). The results of the physical-chemical parameters evaluated showed influence of the tide and also of anthropic contributions close to the estuary. In fact, the lead concentrations determined (0.10-1.32 mg L-1) are well above that allowed by Brazilian legislation (&lt; 0.010 mg L-1). The organic matter present in the SPM showed a high degree of humification being similar to the organic matter extracted from water and showed strong interaction by Pb2+ ions.
DOI: 10.6084/m9.figshare.14304114.v1
title: Speciation of Antimony in Injectable Leishmanicidal Drugs by Lowering Citric Acid Concentration Used in Hydride Generation Atomic Absorption Spectrometry Analysis

description: This study proposes a procedure for speciation of antimony by hydride generation atomic absorption spectrometry in pentavalent antimony drugs. The SbIII content was determined by selective generation of SbH3 in medium with higher SbV concentration using 4 to 20-fold lower citric acid solutions than recommended in the available literature. The multivariate optimization of the methods was performed through factorial design followed by a central composite design (CCD). The limit of detection (LOD) and limit of quantification (LOQ) were calculated at 0.15 and 0.05 µg L-1 and 0.48 and 0.17 µg L-1, for total Sb and SbIII, respectively. The relative standard deviation (RSD) values ranged from 3.1 to 19.6% and 9.1 to 20.1%, while recovery ranged from 95.6 to 102.3% and 89.1 to 108.1%, for total Sb and SbIII, respectively. This method was applied for the analysis of meglumine antimoniate samples. Total Sb and SbIII concentrations ranged from 79.2 to 101.1 mg mL-1 and 0.08 to 0.41 mg mL-1, respectively.
DOI: 10.6084/m9.figshare.14304111.v1
title: Optimization of the Reaction Conditions for the Synthesis of Dihydrobenzofuran Neolignans

description: We have optimized the experimental conditions for the silver(I)-promoted oxidative coupling of methyl p-coumarate (I) and methyl ferulate (II), which is the most frequently used methodology to synthesize the bioactive dihydrobenzofuran neolignans 1 ((±)-trans-dehydrodicoumarate dimethyl ester) and 2 ((±)-trans-dehydrodiferulate dimethyl ester). Most of the tested conditions affected the conversion (i.e., the consumption of I and II) and the selectivity (i.e., the percentage of I and II that was converted into 1 and 2, respectively), so the optimized conditions were the ones that afforded the best balance between conversion and selectivity. Silver(I) oxide (0.5 equiv.) is the most efficient oxidant agent amongst the silver(I) reagents that were tested to convert methyl esters I and II into compounds 1 and 2, respectively. Acetonitrile, which has not yet been reported as a solvent for this reaction, provided the best balance between conversion and selectivity, besides being “greener” than other solvents that are more often employed (e.g., dichloromethane and benzene). Under the optimized conditions, the reaction time decreased from 20 to 4 h without significantly impacting the conversion and selectivity.
DOI: 10.6084/m9.figshare.14304110.v1
title: Direct Solid Sample Analysis of Medicinal Herbs for Determination of Ba, Cu, Ni, V and Zn by EDXRF

description: In this work, an analytical method for determination of Ba, Cu, Ni, V, and Zn, in medicinal herbs, through direct solid sample analysis by energy dispersive X-ray fluorescence spectrometry (EDXRF), was applied. Accuracy and precision (intra and inter day) of the analytical method were confirmed through analysis of certified reference material, tomato leaves (CRM NIST 1573a). Principal component analysis (PCA) and hierarchical cluster analysis (HCA) allowed to observe the formation of two groups. Group I was composed by highest levels of Cu and Zn, and the group II with highest concentrations of Ba, V, and Zn. Group I also was subdivided into two subgroups. The concentration of Ni in some samples exceeded the maximum allowed limit. In all samples, Cu and Zn concentration were below the maximum limit allowed by Brazilian legislation. However, for Ba and V, the evaluation was not possible, because there are no maximum limits in legislation.
DOI: 10.6084/m9.figshare.14304107.v1
title: Bergenin of Peltophorum dubium (Fabaceae) Roots and Its Bioactive Semi-Synthetic Derivatives

description: This work describes the isolation of pure bergenin from Peltophorum dubium roots with good yields and its further derivatization through Williamson synthesis. The alkyl derivatives of the bergenin were identified by nuclear magnetic resonance and mass spectrometry data analysis. Among them, three derivatives were reported for the first time herein, 8,10-dihexyl-bergenin, 8,10-didecyl-bergenin, and 8,10-ditetradecyl-bergenin, along with three previously reported ones (8,10-dimethylbergenin, 8-methylbergenin, 8,10-dioctyl-bergenin). Most derivatives of the bergenin displayed moderate cytotoxicity against Artemia salina, except the 8,10-dihexyl-bergenin (lethal concentration doses for 50% (LC50) = 70.55 µg mL-1). The antimicrobial assay showed that all derivatives selectively inhibited the Gram-positive bacteria Staphylococcus aureus, and two of them (8,10-dihexyl-bergenin and 8,10-didecyl-bergenin) had promising activities (minimum inhibitory concentration (MIC) = 5.1-6.2 µmol L-1). In addition, bergenin displayed interesting inhibition on acetylcholinesterase (half maximal inhibitory concentration (IC50) = 141.19 ± 0.41 µmol L-1), while its semi-synthetic derivatives displayed modest activity. Our results revealed that the antibacterial activity of bergenin could be greatly improved through its structural modification.
DOI: 10.6084/m9.figshare.14304102.v1
title: Identification of Potential Inhibitors of Severe Acute Respiratory Syndrome-Related Coronavirus 2 (SARS-CoV-2) Main Protease from Non-Natural and Natural Sources: A Molecular Docking Study

description: So far, there is neither a vaccine nor a specific antiviral drug to prevent or treat COVID-19 (coronavirus disease) infection. Recent studies have been done to investigate the capacity of human immunodeficiency virus type 1 (HIV-1) protease inhibitors be used in the treatment of COVID-19 patients. Some of those drugs have shown to be promising. Natural chemical substances from plants provide a good source of chemicals for the development of potential novel antiviral drugs against viral pathogens including HIV-1. In January 2020, a new promising target useful for structure-based drug design was elucidated and stored in the Protein Data Bank. In this context, the objective of this study was to determine whether and how a set of both non-natural and natural HIV-1 protease inhibitors could dock to that novel crystallized severe acute respiratory syndrome-related coronavirus 2 (SARS-CoV-2) main protease and, consequently, to identify potential lead compounds to treat COVID-19 infected patients. The results showed that two non-natural compounds, danoprevir and lopinavir, and one compound from plant, corilagin, produced strong interactions with the inhibitor binding site of SARS-CoV-2 main protease. It is expected that this work contributes to validate the use of HIV-1 protease inhibitors against SARS-CoV-2.
DOI: 10.6084/m9.figshare.14304098.v1
title: Determining Mercury in Sediment Samples by Extraction Using a Novel-Chelating Reagent Dithiothreitol (DTT) Followed by Cold Vapor Atomic Fluorescence Spectrometry (CV-AFS)

description: A new analytical protocol has been developed for the determination of mercury in surface sediments using dithiothreitol (DTT) as a new chelating reagent for the extraction. This protocol requires a small sample mass (250 mg), 4.0 mL of a 0.1 M (pH = 9.0) aqueous DTT solution, and sonication for 30 min, followed by cold vapor atomic fluorescence spectrometry (CV-AFS). The limits of detection and quantification determined were 6 and 18 ng g−1, respectively. The method was validated using three standard reference materials, SRM NIST 1646a, PACS-2, and MESS-3, with recoveries in the range of 102-124%. The new analytical protocol was successfully applied in riverine surface sediments, revealing concentrations in the range of 220-340 ng g−1. The results obtained by CV-AFS were compared to those obtained by DMA-80 (direct mercury analyzer). The linear regression equation obtained was [CV-AFS] = (0.91 ± 0.07)[DMA-80] + (0.04 ± 0.02), revealing no systematic difference between the analytical methods. Hence, the proposed method does not require the complete digestion of the sediment, and was found to be comprehensive, simple, accurate and suitable to be employed for determination of mercury in sediment samples.
DOI: 10.6084/m9.figshare.14304096.v1
title: Multifunctionality of βCD/Ofloxacin and HPβCD/Ofloxacin Complexes: Improvement of the Antimicrobial Activity and Apoptosis Induction on Lung Adenocarcinoma A549 Cells

description: The ofloxacin (OFLOX) is a second-generation synthetic antibiotic that can be classified as a multifunctional drug, but is a poorly soluble drug, which influences its efficiency. The inclusion complexes of OFLOX with β-cyclodextrin (βCD) or hydroxypropyl-β-cyclodextrin (HPβCD) can improve the chemical characteristics of the drug; however, studies showing the biological activity of these inclusion complexes are still scarce. The present work aimed to investigate the multifunctionality of the OFLOX and their inclusion complexes. Thus, the 1:1 βCD/OFLOX or HPβCD/OFLOX were prepared and analyzed by Fourier transform infrared spectroscopy (FTIR), thermogravimetric and differential thermal analysis (TGA and DTA), 1H nuclear magnetic resonance (NMR) and isothermal titration calorimetry (ITC). The antitumor and antibacterial effects were assessed. The results confirm the formation of the inclusion complexes, which had lower minimum inhibitory concentration (MIC) values, higher cytotoxicity and promoted the apoptosis. The present study showed, for the first time, the promising effects of the inclusion complexes as antitumor, improving the biological activities of the uncomplexed ofloxacin.
DOI: 10.6084/m9.figshare.14304095.v1
title: Green Extraction Optimization of Bioactive Compounds from Rosemary (Rosmarinus officinalis L.) Using Response Surface Methodology

description: Rosemary (Rosmarinus officinalis L.) is known for its bioactive compounds with high antioxidant potential and pharmacological properties, such as antibacterial, antidepressant and anti-inflammatory. These properties are attributed to the presence of (poly)phenolic compounds. In the literature there is no extraction of these compounds with a totally non-toxic solvent, capable of applying the extract directly to the food. This work aimed to optimize the extraction conditions of bioactive compounds from the rosemary leaves using water as solvent. According to the analysis of variance parameters, a cubic model of high order of significance was obtained with adjusted R2 (R squared) &gt; 0.947. The optimal conditions of the antioxidant potential for conventional and ultrasonic agitation were: temperature 70 °C, 30 min of extraction and the solvent/solute ratio of 25, resulting in an antioxidant potential of 6861 and 7126 µmol L−1 Trolox, respectively. The electrospray ionization mass spectrometry (ESI(−)-MS/MS) analysis showed the presence of antioxidant compounds such as: carnosol (m/z 329.20), rosmanol (m/z 345.03) and rosmarinic (m/z359.14) acids. The response surface methodology evaluated the influence of the main parameters of the bioactive compounds extraction from rosemary using only water as solvent, in addition to the use of less time and sample mass, resulting in lower cost.
DOI: 10.6084/m9.figshare.14304093.v1
title: Method for Cleaning Back-Produced Water from Polymer Flooding Operations to Determine Polymer Molar Mass Using Size-Exclusion Chromatography

description: One of the methods used by the oil industry to increase production is to inject water, containing polymer, into the reservoir. The viscosity of the aqueous solution is primarily responsible for the efficiency of this method, and is achieved using polymers with high molar mass. However, polymer degradation can occur during pumping and fluid displacement in the porous medium, reducing the efficiency of the polymer flooding method. Therefore, it is important to monitor the molar mass of the polymer in the produced water. Size-exclusion chromatography (SEC) is a powerful method for determining average molar mass of polymers, but the impurities present in the produced water, such as salts and residual oil, can significantly affect the analysis. There is no method described in the literature for pretreating produced water before injecting it into the chromatograph. Therefore, the purpose of this work was to develop a reliable method for this pretreatment, without affecting the molar mass of the polymer. The results showed that an efficient method, which does not cause polymer degradation, must contain four steps: (i) heating, (ii) regular filtration, (iii) elution in poly(divinylbenzene) resin, and (iv) dialysis.
DOI: 10.6084/m9.figshare.14304092.v1
title: NMR in Analysis of the Nutritional Value of Lipids from Muscles and Livers of Wild Amazonian Fishes with Different Eating Habits Over Seasonal Variation

description: Endogenous and environmental factors can influence the lipid contents of fishes among which, in the Amazon River, seasonal dynamics influences stand out. Herein, nine most consumed Amazonian fish species had their lipid composition evaluated in terms of effects of tissue, season and eating habits. Higher amounts of lipids were obtained from fish livers than dorsal muscles. Statistical analysis has shown that Amazonian fishes presented different lipid profiles according to their eating habits, which mainly comprised saturated fatty acids to distinguish detritivorous livers, and linolenic acid, cholesterol, polar lipids for carnivorous and piscivorous fish muscles. Furthermore, in Amazonian fish, some very important lipids for human nutrition were found, such as w-3 and w-6 fatty acids whose availability depended on the tissue metabolism and fishes’ eating habit along with the seasonal periods. For example, our findings indicated that the piscivorous fish C. monoculus presented higher levels of linoleic acid for livers than linolenic acid and the opposite occurred for muscles. The w-6 and w-3 fatty acids ratio was influenced by the season dynamic of the Amazon River and availability of food according to each specific eating habit, pointing mainly to the piscivorous fishes as the healthiest fish for human consumption.
DOI: 10.6084/m9.figshare.14304090.v1
title: Identification of Flavonoids as Inhibitors of Plasmodium falciparum Enoyl-ACP Reductase by Hierarchical Virtual Screening

description: Malaria, a parasitic infection caused by Plasmodium falciparum, is a serious global public health problem. The enzyme enoyl-acyl carrier protein (ACP) reductase present in a limiting step in the biosynthesis of fatty acids type II was used to search for novel molecules with potential inhibitor by virtual screening techniques. A flavonoid library obtained in ChEMBL database (n = 4,008) was filtered through physico-chemical similarity using the Euclidean distance as a criterion. The selected molecules were subjected to molecular docking using the scoring function GridScore in the DOCK 6.5 software. The top 30 ranked molecules by molecular docking were submitted to the AuPosSOM 2.1 software with the aim of clustering molecules by means of intermolecular interactions in order to understand the patterns of these interactions with enoyl-ACP reductase from Plasmodium falciparum (PfENR). We observed the importance of flavonoid moiety to hydrophobic interactions with the active site of enzyme, this confirmed the choice to study this metabolite class as PfENR inhibitors. Moreover, it was possible to recognize which intermolecular interactions contribute to the molecular recognition process.
DOI: 10.6084/m9.figshare.14304089.v1
title: Synthesis and Antioxidant and Antimicrobial Properties of β-Hydroxy Sulfides, Sulfoxides, and Sulfones Derived from Cardanol and Glycerol Derivatives

description: Natural and synthetic sulfur-bearing organic compounds have many applications in medicinal chemistry. This article reports the preparation of amphiphilic β-hydroxy sulfides, sulfoxides, and sulfones derived from cardanol and glycerol. Thiolysis of cardanol epoxide 3 with various thiols (4a-4j) in ethanol or water yielded the corresponding β-hydroxy sulfides 5a-5j (61-95%). Treatment with 30% H2O2 in acetic acid at ambient temperature completely converted these products into β-hydroxy sulfoxides 6a-6j and sulfones 7a, 7c-7f, 7h-7j. The synthesized compounds were characterized by 1H nuclear magnetic resonance (NMR), 13C NMR, high-resolution mass spectroscopy (HRMS) and performed the in vitro evaluation antimicrobial activities against standard strains of Staphylococcus aureus and Escherichia coli. Compounds 5a, 5d-5f, and 5h-5j proved moderately active against S. aureus. None of the compounds were active against E. coli. β-Hydroxy-sulfides 5a-5j were also evaluated for antioxidant properties but failed to exhibit significant activity.
DOI: 10.6084/m9.figshare.14304086.v1
title: Multiresidue Determination of Endocrine Disrupting Compounds in Sewage Treatment Plants (SPE-HPLC-DAD)

description: This work focuses on the validation and application of solid phase extraction followed by high-performance liquid chromatography (SPE-HPLC) analysis of important endocrine disruptors compounds (EDC) from different classes in highly complex wastewater matrix. The endocrine disruptors investigated included three different categories: pharmaceuticals (sulfamethoxazole (SMZ), trimethoprim (TMP) and diclofenac (DCF)), hormones (estrone (E1), 17α-ethinylestradiol (EE2) and 17β-estradiol (E2)) and plastic materials (bisphenol A (BPA)). The method involves pre-concentration by SPE using Strata-X extraction cartridges followed by HPLC coupled with diode array detector (DAD). As the assumption of homoscedasticity was met for analytical data, ordinary linear regression procedure was applied to the data. The method was considered validated for 7 EDC after consistent evaluation of the key analytical parameters. Recoveries were ranged from 52.3 to 179.6%. Limits of quantification were in the range 6.0-0.4 µg L−1. The described method was applied to evaluate the occurrence and removal efficiency of EDC in two biological sewage treatment plants (STPs). The influent mean concentrations of E1, E2 and EE2 hormones were 79.54; 175.09 and 102.19 µg L−1, respectively, while for SMZ, TMP, DCF and BPA were 215.17; 187.01; 218.97 and 87.12 µg L−1 for STP A, respectively. The efficiencies for the removal of EDCs ranged from 0 to 79.4%.
DOI: 10.6084/m9.figshare.14304084.v1
title: Activated Complex Approach to Describe Bovine Serum Albumin-Azure A and Bovine Serum Albumin-Azure B Intermolecular Interactions

description: Azure A (AZA) and azure B (AZB) phenothiazine dyes are used for clinical and medical purposes, and their functions can be altered via interactions with proteins. However, no kinetics information on the interactions between phenothiazine dyes and bovine serum albumin (BSA) is available. Surface plasmon resonance was used to determine the energetic and dynamic of the BSA-AZA and BSA-AZB complexes formation at pH 7.4. At temperature ≤ 16 °C, the formation of activated (DH‡a,12°C,AZA= -310.57 kJ mol-1 and DH‡a,12 °C,AZB= -256.37 kJ mol-1) and thermodynamically stable (DH°12°C,AZA= -314.56 kJ mol-1 and DH°12°C,AZB= -265.73 kJ mol-1) complexes was driven by enthalpy, while at temperature ≥ 20 °C, by entropy, (TDS‡a,28°C,AZA= 207.49 and TDS‡a,28°C,AZB= 190.69; TDS°28°C,AZA= 277.50 and TDS°28°C,AZB= 257.26 kJ mol-1). Hydrophobic interactions were fundamental to the complex stability and the increase in number of -CH3 groups in the dyes do not affect kinetic and thermodynamic parameters. Our results could help optimize the medical and pharmaceutical applications of phenothiazine dyes.
DOI: 10.6084/m9.figshare.14304081.v1
title: Determination of Total Antioxidant Capacity Using Thiamine as a Natural Fluorescent Probe

description: This work proposes a spectrofluorometric method for the determination of total antioxidant capacity (CAO) in beverage samples, based on inhibition of thiochrome formation (λex = 370 nm, λem = 440 nm); a product of thiamine (vitamin B1) oxidation from K3Fe(CN)6. In the development of the method, gallic acid (GA) was used as a reference, and inhibition of thiochrome formation (in percentage) was used as the analytical response. The selectivity of the method was evaluated using seven different compounds (gallic acid, ascorbic acid, quercetin, butylhydroxytoluene (BHT), 6-hydroxy-2,5,7,8-tetramethylchroman-2 (Trolox), cysteine, and glucose). As proof of concept, the proposed method was applied in the determination of CAO in different samples, such as teas and infusions, red wines, and white wines. The results were compared with the Folin-Ciocalteu (FC), 2,2’-azino-bis(3-ethylbenzothiazoline-6-sulfonate) (ABTS•+), and 2,2-diphenyl-1-picrylhydrazyl (DPPH•) methods using the linear correlation between the methods (at 95% confidence). We observed excellent agreement between the proposed method and FC (correlation coefficient (r) = 0.9768) and ABTS•+ (r = 0.9842), compared with DPPH• method (r = 0.8502). For the determination of total CAO in beverages, the proposed method developed proved to be fast, sensitive, simple, and the results were in agreement with established assays.