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2.
Talanta ; 205: 120148, 2019 Dec 01.
Article in English | MEDLINE | ID: mdl-31450468

ABSTRACT

Spent coffee grounds (SCG) immobilized in agarose gel are proposed as a novel binding agent for application in the Diffusive Gradients in Thin films (DGT) technique for the determination of Cd, Cu, Ni, Pb and Zn in waters. The SCG-agarose gel was characterized by Scanning Electron Microscopy, Energy Dispersive X-ray Spectrometry and Porosimetry by nitrogen adsorption. Elution of analytes from the binding agent was effectively performed with 2 mol L-1 HCl. The effects of key DGT parameters (e.g. immersion time, ionic strength and pH) were evaluated with a deployment of DGT devices (DGT-SCG) in synthetic solutions with ionic strengths between 0.005 mol L-1 and 0.1 mol L-1 and within a pH range of 3.5-8.0. The results were in excellent agreement with the predicted theoretical curve for mass uptake. Consistent results were found for solutions with ionic strengths between 0.005 mol L-1 and 0.1 mol L-1 and within a pH range of 3.5-8.0. The DGT-SCG performance was also evaluated in two spiked river water samples (Corumbataí and Piracicaba river) with satisfactory uptake values (CDGT-SCG/Csol) between 0.74 and 1.53. The proposed DGT-SCG opens opportunities for using residual biomass as binding phase in the DGT technique, showing low costs in production and complying with "green" technology approaches.

4.
Front Microbiol ; 9: 2930, 2018.
Article in English | MEDLINE | ID: mdl-30574128

ABSTRACT

Tuberculosis (TB) is an infectious, airborne disease caused by the bacterium Mycobacterium tuberculosis that mainly affects the lungs. Fortunately, tuberculosis is a curable disease, and in recent years, death rates for this disease have decreased. However, the existence of antibiotic-resistant strains and the occurrence of co-infections with human immunodeficiency virus (HIV), have led to increased mortality in recent years. Another area of concern is that one-third of the world's population is currently infected with M. tuberculosis in its latent state, serving as a potential reservoir for active TB. In an effort to address the failure of current TB drugs, greater attention is being given to the importance of bioinorganic chemistry as an ally in new research into the development of anti-TB drugs. Ruthenium (Ru) is a chemical element that can mimic iron (Fe) in the body. In previous studies involving the following heteroleptic Ru complexes, [Ru(pic)(dppb)(bipy)]PF6 (SCAR1), [Ru(pic)(dppb)(Me-bipy)]PF6 (SCAR2), [Ru(pic)(dppb)(phen)]PF6 (SCAR4), cis-[Ru(pic)(dppe)2]PF6 (SCAR5), and [Ru(pic)(dppe)(phen)]PF6 (SCAR7), we observed excellent anti-TB activity, moderate cell-toxicity, and a lack of oral bioavailability in an in vivo model of these complexes. Therefore, the objective of this study was to evaluate the toxicity and oral bioavailability of these complexes by loading them into a nanostructured lipid system. The nanostructured lipid system was generated using different ratios of surfactant (soybean phosphatidylcholine, Eumulgin®, and sodium oleate), aqueous phase (phosphate buffer with a concentration of 1X and pH 7.4), and oil (cholesterol) to generate a system for the incorporation of Ru(II) compounds. The anti-TB activity of the compounds was determined using a microdilution assay with Resazurin (REMA) against strains of M. tuberculosis H37Rv and clinical isolates resistant. Cytotoxicity assay using J774.A1 cells (ATCC TIB-67) and intra-macrophage activity were performed. The oral bioavailability assay was used to analyze blood collected from female BALB/C mice. Plasma collected from the same mice was analyzed via inductively coupled plasma mass spectrometry (ICP-MS) to quantify the number of Ru ions. The complexes loaded into the nanostructured lipid system maintained in vitro activity and toxicity was found to be reduced compared with the compounds that were not loaded. The complexes showed intra-macrophagic activity and were orally bioavailable.

5.
Anal Chim Acta ; 950: 32-40, 2017 Jan 15.
Article in English | MEDLINE | ID: mdl-27916127

ABSTRACT

Amberlite IRA-410 anionic exchange resin was evaluated as the binding layer for sampling V(V) by using Diffusive Gradients in Thin Films (DGT). V(V) was determined by inductively coupled plasma mass spectrometry (ICP-MS). Mass vs. time DGT deployments (ionic strength = 0.03 mol L-1 NaNO3, pH = 5.6 and T = 23.5 ± 0.5 °C) was characterized by excellent linear relationship (R2 = 0.9993) and a significant retention of V(V) by the binding layer. An exchange capacity of at least 40 µg V g-1 resin was achieved for the proposed binding layer. The diffusion coefficient obtained (7.13 ± 0.6 10-6 cm2 s-1) agrees with the literature. The accumulation rate of V(V) was not significantly affected by ionic strength of solutions up to 0.03 mol L-1 and for the entire studied pH range (from 3 to 9). Furthermore, when comparing the concentrations obtained using IRA-410-DGT and those obtained by direct measurement of the solution concentrations, the proposed approach provided a reduction of the 35Cl16O interference on V(V) determination by ICP-MS. Determination of V in normal mode (without collision cell) in solutions containing analyte:Cl- concentration ratio up to 1:500,000 was not affected by interference of 35Cl16O+ polyatomic ion even when normal mode ICP-MS was used. Potential interfering ions on sampling V(V) by DGT (PO43- and SO42-) showed no significant effects on the accumulation rate of V(V). Laboratory tests performed using synthetic samples, natural freshwater and acid drainage water showed an excellent performance (recoveries from 93% to 110%). For in situ deployment, measurements of V(V) by the proposed approach was not significantly different (95.5%) from the value of dissolved V concentration.

6.
Talanta ; 129: 417-21, 2014 Nov.
Article in English | MEDLINE | ID: mdl-25127614

ABSTRACT

In this work, a device based on diffusive gradients in thin films (DGT) was evaluated for the determination of Hg(II) in river water. The DGT device was assembled with a cellulose phosphate ion exchange membrane (P81 Whatman) as a binding phase and agarose gel 1.5% (m/v) as a diffusive layer. Laboratory deployments showed that the binding of Hg(2+) ([Hg(DGT)]/[Hg(solution)]) by P81 membrane was more effective (97%) than the Chelex 100 resin (80%).The effect of ionic strength, pH and potential interfering ions on Hg binding with DGT׳s was investigated. The results showed no significant effect on the binding of Hg(II) at pH range from 3.5 to 8.5 and at an ionic strength range from 0.0005 to 0.1 mol L(-1). Uptakes of 50 µg L(-1) Hg(II) by P81 membrane were not affected by Fe, Mn, Zn, Cu, Ca and Mg at the concentration range of 200-1800 µg L(-1). Finally, the DGT device using the P81 as the binding layer was applied for in situ measurements of Hg in river water. For in situ measurements, the labile Hg concentration (from <2 to 13 ng L(-1)) was lower than 10% of the dissolved fraction (from 155 to 446 ng L(-1)).


Subject(s)
Environmental Monitoring/methods , Mercury/analysis , Rivers/chemistry , Water Pollutants, Chemical/analysis , Cellulose/analogs & derivatives , Cellulose/chemistry , Chemistry Techniques, Analytical , Diffusion , Fresh Water/chemistry , Hydrogen-Ion Concentration , Ions , Osmolar Concentration , Resins, Synthetic/chemistry , Sepharose/chemistry
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