Publications by authors named "Jairo Lisboa Rodrigues"

19 Publications

  • Page 1 of 1

Iron Oxide Nanomaterials for the Removal of Cr(VI) and Pb(II) from Contaminated River After Mariana Mining Disaster.

J Nanosci Nanotechnol 2021 03;21(3):1711-1720

Instituto de Ciência, Engenharia e Tecnologia, Universidade Federal dos Vales do Jequitinhonha e Mucuri, 39803-371 Teófilo Otoni, Minas Gerais, Brazil.

If not properly treated, water contaminated with chromium (Cr(VI)) and lead (Pb(II)) can cause severe damage to health due to the accumulation of those toxic metals in the human body. Therefore, in this work, three iron oxides, i.e., δ-FeOOH, cystine-functionalized δ-FeOOH (Cys-δ-FeOOH), and Fe₃O₄, were synthesized and used as adsorbents for Cr(VI) and Pb(II) in water. The results indicated that the Cr(VI) is best adsorbed on cys-δ-FeOOH followed by δ-FeOOH and Fe₃O₄. It was because of the enhanced interaction between Cr(VI) and the cysteine functional groups on the δ-FeOOH surface. The Cr(VI) adsorption capacity of cys-δ-FeOOH, δ-FeOOH, and Fe₃O₄ was 217, 14, and 8 mg g, respectively. On the other hand, Pb(II) was preferentially adsorbed directly on δ-FeOOH achieving a maximum Pb(II) adsorption capacity of 174 mg g. The Pb(II) adsorption capacity of cys-δ-FeOOH and Fe₃O₄ was 97 and 74 mg g, respectively. The Cr(VI) adsorption on cys-δ-FeOOH was best described by the Langmuir-Freundlich model, whereas Pb(II) adsorption on δ-FeOOH followed the Langmuir model. Both Cr(VI) and Pb(II) adsorption on the adsorbents was well-fitted to pseudo-second-order kinetics. The Cr(VI) was more quickly adsorbed by cys-δ-FeOOH ( = 0.10 mg g min) while the initial adsorption rate of Pb(II) onto δ-FeOOH was significantly faster ( = 16.34 mg g min). Finally, the synthesized adsorbents were efficient to remove Cr(VI) and Pb(II) from water samples of the Doce river after the environmental disaster of Mariana city, Brazil, thus showing its applicability to remediate real water samples.
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http://dx.doi.org/10.1166/jnn.2021.19089DOI Listing
March 2021

DLLME-SFO-GC-MS procedure for the determination of 10 organochlorine pesticides in water and remediation using magnetite nanoparticles.

Environ Sci Pollut Res Int 2020 Dec 12;27(36):45336-45348. Epub 2020 Aug 12.

Instituto de Ciência, Engenharia e Tecnologia, Universidade Federal dos Vales do Jequitinhonha e Mucuri, Teófilo Otoni, MG, 39803-371, Brazil.

There exists a high demand for fast, simple, and reliable methodologies for determining the presence of organochlorine pesticides (OCPs) on environmental samples. Moreover, the toxicity and accumulation of potential OCPs in several environments have led to the development of technologies that achieve their removal from contaminated waters. In this study, a novel method combining a dispersive liquid-liquid microextraction procedure based on the solidification of floating organic drop is developed and validated for the extraction, preconcentration, and determination of 10 OCPs: α-BHC, p,p'-DDE, δ-BHC, dieldrin, p,p'-DDT, endosulfan I, endosulfan sulfate, heptachlor, heptachlor epoxide (isomer B), and methoxychlor in water samples. The results show that the calibration curves were linear for all the studied compounds, and the coefficients of correlation higher than 0.99. The variation coefficient for precision and accuracy was lower than 10%, and the accuracy ranged from 93 to 105%. Low limit of detection and limit of quantification values ranging from 0.06-3.00 ng mL and 0.20-10 ng mL were obtained, respectively. The capability of the proposed method was confirmed using an analysis of the water samples before and after the degradation process; this was achieved by employing nanomaterials, while performing an analysis of 160 real samples that were sourced from a Brazilian river. A cobalt-doped magnetite was applied for the environmental remediation of the studied compounds, and it was verified that the novel material has the potential to be used in environmental remediation with a degradation efficiency exceeding 80% for the majority of the studied compounds.
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http://dx.doi.org/10.1007/s11356-020-10285-2DOI Listing
December 2020

Rapid, sensitive and simultaneous determination of 16 endocrine-disrupting chemicals (parabens, benzophenones, bisphenols, and triclocarban) in human urine based on microextraction by packed sorbent combined with liquid chromatography tandem mass spectrometry (MEPS-LC-MS/MS).

Chemosphere 2020 Feb 23;240:124951. Epub 2019 Sep 23.

Laboratório de Toxicologia e Essencialidade de Metais, Faculdade de Ciências Farmacêuticas de Ribeirão Preto, Universidade de São Paulo, 14049-903, Ribeirão Preto, SP, Brazil. Electronic address:

A high demand exists in human biomonitoring studies for reliable and straightforward methods that generate data faster and simultaneously. Thus, the present study combines microextraction by packed sorbent (MEPS) and liquid chromatography coupled to mass spectrometry (LC-MS/MS) for simultaneous extraction and determination of various classes of endocrine-disrupting chemicals (EDCs), including parabens, benzophenones, bisphenols, and the antimicrobial, triclocarban in human urine samples. Optimized MEPS conditions were: i) MEPS sorbent (C18), ii) pH of sample (3), iii) volume of sample (250 μL), iv) number of draws-eject cycles (5) and (vi) desorption solvent conditions (100 μL of CHOH:HO 80:20 v/v). The calibration curves were linear over the selected ranges for all studied compound, with correlation coefficients higher than 0.99. The variation coefficient for precision was lower than 20% at lower concentrations and lower than 15% at the higher concentrations studied. The accuracy ranged from 90% to 118%. The proposed strategy affords several advantages over currently published approaches, including simplicity of operation and reduction of sample and solvent volumes and time for matrix clean-up. Moreover, the analytical performance of each MEPS cartridge remained stable over the analysis of at least 70 samples (RSD < 10%). Thus, the current procedure may be an interesting high-throughput alternative for large routine human biomonitoring studies. Urinary geometric mean concentrations of EDCs obtained in this study were close than those previously reported for Brazilian children.
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http://dx.doi.org/10.1016/j.chemosphere.2019.124951DOI Listing
February 2020

Degradation of haloacetic acids with the Fenton-like and analysis by GC-MS: use of bioassays for monitoring of genotoxic, mutagenic and cytotoxic effects.

Environ Monit Assess 2019 Jul 26;191(8):513. Epub 2019 Jul 26.

Instituto de Ciência, Engenharia e Tecnologia, Universidade Federal dos Vales do Jequitinhonha e Mucuri, Teófilo Otoni, MG, 39803-371, Brazil.

In this study, a method was developed to evaluate the degradation of haloacetic acids (HAAs) in water by a heterogenous Fenton-like process catalyzed by cobalt-doped magnetite nanoparticles (FeCoO), extraction of the contaminants by liquid-liquid extraction (LLE), and analysis by gas chromatography-mass spectrometry (GC-MS). The developed method was efficient in the degradation of HAAs, with the following degradation values: 63%, 62%, 30%, 39%, 37%, 50%, 84%, 41%, and 79% for monochloroacetic acid, monobromoacetic acid, dichloroacetic acid, trichloroacetic acid, bromochloroacetic acid, dibromoacetic acid, bromodichloroacetic acid, dibromochloroacetic acid, and tribromoacetic acid compounds, respectively. Through the application of the Allium cepa test, the cytotoxicity, genotoxicity, and mutagenicity of HAAs were evaluated. The results confirm its genotoxic and mutagenic effects on Allium cepa meristematic cells. Through this study, it was possible to verify the effectiveness of the developed method and its potential as a proposal for environmental remediation.
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http://dx.doi.org/10.1007/s10661-019-7642-6DOI Listing
July 2019

Arsenic volatilization by Aspergillus sp. and Penicillium sp. isolated from rice rhizosphere as a promising eco-safe tool for arsenic mitigation.

J Environ Manage 2019 May 20;237:170-179. Epub 2019 Feb 20.

Centro de Ciências Naturais e Humanas, Universidade Federal do ABC, Avenida dos Estados 5001, 09210-580, Santo André, SP, Brazil. Electronic address:

Arsenic (As) is a non-threshold human carcinogenic. This element can be volatilized either by nature or anthropogenic sources. In the present study, the analytical performance of an As volatile species trapping system was evaluated to assess the As volatilization promoted by Penicillium sp. and Aspergillus sp., both isolated from rice rhizosphere, and Aspergillus niger sp. considered as a reference. The study was conducted for 60 days (sampling of volatile As species from 1st to 30 day and from 31st to 60 day). The efficiency of As-volatilization was associated with the fungal growth. The highest As volatilization occurred from 31st to 60 day. Penicillium sp., Aspergillus sp. and A. niger were capable of producing 57.8, 46.4, and 5.2% of volatile arsenic species, respectively. The speciation analysis has shown trimethylarsine (TMAs) as the main volatilized As-form, followed by mono- and dimethylarsine (MMAs and DMAs). The results are following the "Challenger pathway". Therefore, the tested fungi isolated from rice rhizosphere have shown promising properties concerning bio-volatilization with potential use for As-mitigation in paddy soils.
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http://dx.doi.org/10.1016/j.jenvman.2019.02.060DOI Listing
May 2019

Simple synthesis and characterization of l-Cystine functionalized δ-FeOOH for highly efficient Hg(II) removal from contamined water and mining waste.

Chemosphere 2019 Jan 13;215:422-431. Epub 2018 Oct 13.

Instituto de Ciência, Engenharia e Tecnologia, Universidade Federal dos Vales do Jequitinhonha e Mucuri, 39803-371 Teófilo Otoni, Minas Gerais, Brazil. Electronic address:

l-Cystine functionalized δ-FeOOH nanoparticles (Cys-δ-FeOOH) were prepared by a cheap and straightforward method for using as an adsorbent of Hg(II) in aqueous solution. X-ray diffraction (XRD), attenuated total reflectance infrared spectroscopy (ATR-IR), and Raman spectroscopy confirmed that Cys-δ-FeOOH was successfully synthesized. Cys-δ-FeOOH with 14 nm crystal size, 34 m g surface area, and 9 nm pore size were produced. The functionalization of the δ-FeOOH surface with cysteine decreases the point of zero charge of the iron oxyhydroxide from 8.4 in δ-FeOOH to 5.7 in Cys-δ-FeOOH, which is beneficial for the adsorption of Hg(II) near neutral pH. The maximum Hg(II) adsorption capacity of the δ-FeOOH and Cys-δ-FeOOH at pH 7 were found to be 35 mg g and 217 mg g, respectively. The kinetics data were best fitted by a pseudo-second-order model, suggesting chemical adsorption on the surface and pores of Cys-δ-FeOOH nanoparticles. Finally, δ-FeOOH and Cys-δ-FeOOH filters were constructed for purifying mercury-contaminated water. The filters were highly efficient to treat mercury-contaminated water from a Brazilian river, reducing the concentration of mercury in water to values below the allowed limits by the current legislation.
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http://dx.doi.org/10.1016/j.chemosphere.2018.10.072DOI Listing
January 2019

Removal of mercury(II) from contaminated water by gold-functionalised FeO magnetic nanoparticles.

Environ Technol 2020 Mar 4;41(8):959-970. Epub 2018 Oct 4.

Instituto de Ciência, Engenharia e Tecnologia, Universidade Federal dos Vales do Jequitinhonha e Mucuri, Teófilo Otoni, Brazil.

FeO nanoparticles were prepared by co-precipitation of Fe and Fe and then modified with Au to produce an effective adsorbent (FeO/Au) for aqueous Hg(II) in contaminated water. Rietveld refinement on the XRD pattern confirmed that the FeO/Au was synthesised. Mössbauer spectra exhibited broad and asymmetric resonance lines with two sextets which can be assigned to tetrahedral Fe; and octahedral Fe/Fe. The quantitative analysis of magnetite confirms that the sample shows around 3 wt.% Au and 97 wt.% partially oxidised FeO. High surface area: 121 m g, average pore sizes: 6.3 nm and pore volume: 1.64 cm g. The kinetics data were better fitted with a pseudo-second-order and Dubinin-Radushkevich isotherm suggests the Hg(II) adsorption onto FeO/Au nanoparticles was mainly by chemical adsorption forming complex with the Au metal immobilised on FeO surfaces. Adsorption capacity of 79.59 mg g. Ionic strength and co-existing ions had a slight influence on the adsorption capacity.
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http://dx.doi.org/10.1080/09593330.2018.1515989DOI Listing
March 2020

Agricultural use of Samarco's spilled mud assessed by rice cultivation: A promising residue use?

Chemosphere 2018 Feb 21;193:892-902. Epub 2017 Nov 21.

Centro de Ciências Naturais e Humanas, Universidade Federal do ABC, 09210-170 Santo André, SP, Brazil. Electronic address:

Mining activity is one of the main responsible for accumulation of potentially toxic elements in the environment. These contaminants are absorbed by plants served as food that could be a risk to human health, such rice. Rice is a staple food with known accumulation of toxic elements. The recent collapse of a mining dam operated by Samarco Mining Company spilled around 50 million m of Fe-mining waste in the environment, including rivers and farming areas. In the present study, concentrations of As, Cd, Hg, Pb, Co, Zn, Mn, Cu, Fe, Al, Se, and Sr were determined in soils, roots and grains of rice plants cultivated in soil containing Samarco's residual mud (0, 16, 34 and 50%). Further, rice plant agronomic parameters (chlorophyll, carotenoids, grain yield, mass, height) were assessed. Rice cultivated at Samarco's residual mud produced grains with low levels of As, Cd and Pb. However, the excess of mud (50%) during the rice cultivation reduced roots' growth and grains yield. Chlorophyll (a and b) and carotenoids contents were significantly lower in all mud cultivations, mainly mud-50%. Our findings suggest that plant alterations induced by the mud were associated to the deficiency of nutrients and the physical properties of the mud. Soil fertilization by organic matter and top soil provided conditions for plant development. Therefore, considering the experimental conditions here used, we showed that is possible the use of the affected land for agriculture and reforestation after soil amendment.
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http://dx.doi.org/10.1016/j.chemosphere.2017.11.099DOI Listing
February 2018

A perspective of mitochondrial dysfunction in rats treated with silver and titanium nanoparticles (AgNPs and TiNPs).

J Trace Elem Med Biol 2018 May 31;47:63-69. Epub 2018 Jan 31.

Faculdade de Filosofia, Ciências e Letras de Ribeirão Preto, Departamento de Química, Universidade de São Paulo, Avenida do Café s/n°, CEP 14040-903, Ribeirão Preto, São Paulo, Brazil; National Institute for Alternative Technologies of Detection, Toxicological Evaluation and Removal of Micropollutants and Radioactives (INCT-DATREM), Unesp, Institute of Chemistry, P.O. Box 355, 14800-900 Araraquara, SP, Brazil.

Nanotechnology is a growing branch of science that deals with the development of structural features bearing at least one dimension in the nano range. More specifically, nanomaterials are defined as objects with dimensions that range from 1 to 100 nm, which give rise to interesting properties. In particular, silver and titanium nanoparticles (AgNPs and TiNPs, respectively) are known for their biological and biomedical properties and are often used in consumer products such as cosmetics, food additives, kitchen utensils, and toys. This situation has increased environmental and occupational exposure to AgNPs and TiNPs, which has placed demand for the risk assessment of NPs. Indeed, the same properties that make nanomaterials so attractive could also prove deleterious to biological systems. Of particular concern is the effect of NPs on mitochondria because these organelles play an essential role in cellular homeostasis. In this scenario, this work aimed to study how AgNPs and TiNPs interact with the mitochondrial respiration chain and to analyze how this interaction interferes in the bioenergetics and oxidative state of the organelles after sub-chronic exposure. Mitochondria were exposed to the NPs by gavage treatment for 21 days to check whether co-exposure of the organelles to the two types of NPs elicited any mitochondrion-NP interaction. More specifically, male Wistar rats were randomly assigned to four groups. Groups I, II, III, and IV received mineral oil, TiNPs (100 μg/kg/day), AgNPs (100 μg/kg/day), and TiNPs + AgNPs (100 μg/kg/day), respectively, by gavage. The liver was immediately removed, and the mitochondria were isolated and used within 3 h. Exposure of mitochondria to TiNPs + AgNPs lowered the respiratory control ratio, causing an uncoupling effect in the oxidative phosphorylation system. Moreover, both types of NPs induced mitochondrial swelling. Extended exposure of mitochondria to the NPs maintained increased ROS levels and depleted the endogenous antioxidant system. The AgNPs and TiNPs acted synergistically-the intensity of the toxic effect on the mitochondrial redox state was more significant in the presence of both types of NPs. These findings imply that the action of the NPs on mitochondria underlie NP toxicity, so future application of NPs requires special attention.
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http://dx.doi.org/10.1016/j.jtemb.2018.01.007DOI Listing
May 2018

Evaluation of distribution, redox parameters, and genotoxicity in Wistar rats co-exposed to silver and titanium dioxide nanoparticles.

J Toxicol Environ Health A 2017 11;80(19-21):1156-1165. Epub 2017 Sep 11.

a Faculdade de Ciências Farmacêuticas de Ribeirão Preto, Departamento de Análises Clínicas, Toxicológicas e Bromatológicas , Universidade de São Paulo , Av. do Café s/n, Bairro Monte Alegre, Ribeirão Preto , São Paulo , Brazil.

The increasing production of silver nanoparticles (AgNPs) and titanium dioxide nanoparticles (TiONPs) has resulted in their elevated concentrations in the environment. This study was, therefore, aimed at determining the distribution, redox parameters, and genotoxic effects in male Wistar rats that were treated with either AgNP or TiONP individually, as well as under a co-exposure scenario. Animals were exposed via oral gavage to either sodium citrate buffer (vehicle), 0.5 mg/kg/day TiONP, 0.5 mg/kg/day AgNP or a mixture of TiONPs and AgNPs. Exposure lasted 45 days after which rats were sacrificed, and tissue biodistribution of Ag and Ti measured. The blood concentration of glutathione (GSH) and activities of glutathione peroxidase (GPx) and catalase (CAT) were determined while the genotoxicity was analyzed using the comet assay in peripheral blood and liver cells. The tissue concentrations of Ag followed the order; blood > liver > kidneys while for Ti the order was kidneys > liver > blood. There was no significant change in the measured redox parameters in animals that were exposed to TiONPs. However, there was a significant increase in GSH levels accompanied by a reduction in the GPx activity in AgNP-treated and co-exposed groups. The individual or co-exposure to TiONP and AgNP did not markedly induce genotoxicity in blood or liver cells. Data showed that TiONP did not produce significant oxidative stress or genotoxicity in rats at the dose used in this study while the same dose level of AgNPs resulted in oxidative stress, but no noticeable adverse genotoxic effects.
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http://dx.doi.org/10.1080/15287394.2017.1357376DOI Listing
November 2017

Carvedilol protects the kidneys of tumor-bearing mice without impairing the biodistribution or the genotoxicity of cisplatin.

Chem Biol Interact 2016 Feb 2;245:59-65. Epub 2016 Jan 2.

Departamento de Análises Clínicas, Toxicológicas e Bromatológicas, Faculdade de Ciências Farmacêuticas de Ribeirão Preto-USP, Av. do Café s/n, 14040-903, Ribeirão Preto, SP, Brazil. Electronic address:

Cisplatin (Cisp) is an effective antitumor drug; however, it causes severe nephrotoxicity. Minimization of renal toxicity is essential, but the interference of nephroprotective agents, particularly antioxidants, with the antitumor activity of cisplatin is a general concern. We have recently demonstrated that the anti-hypertensive and antioxidant drug carvedilol (CV) protects against the renal damage and increases the survival of tumor-bearing mice without impairing the tumor reduction by cisplatin. So far, reports on the antioxidant mechanism of CV are controversial and there are no data on the impact of CV on the antitumor mechanisms of cisplatin. Therefore, this study addresses the effect of CV on mechanisms underlying the tumor control by cisplatin. CV did not interfere with the biodistribution or the genotoxicity of cisplatin. We also addressed the antioxidant mechanisms of CV and demonstrated that it does not neutralize free radicals, but is an efficient chelator of ferrous ions that are relevant catalyzers in cisplatin nephrotoxicity. The present data suggest that oxidative damage and genotoxicity play different roles in the toxicity of cisplatin on kidneys and tumors and therefore, some antioxidants might be safe as chemoprotectors. Altogether, our studies provide consistent evidence of the beneficial effect of CV on animals treated with cisplatin and might encourage clinical trials.
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http://dx.doi.org/10.1016/j.cbi.2015.12.020DOI Listing
February 2016

Effect of diabetes on biodistribution, nephrotoxicity and antitumor activity of cisplatin in mice.

Chem Biol Interact 2015 Mar 7;229:119-31. Epub 2015 Feb 7.

Departamento de Análises Clínicas, Toxicológicas e Bromatológicas, Faculdade de Ciências Farmacêuticas de Ribeirão Preto - USP, 14040-903 Ribeirão Preto, SP, Brazil. Electronic address:

Both types of diabetes are associated with higher incidence of some types of cancer. Treating cancer in diabetic patients without aggravating diabetes-related complications is a challenge for clinicians. Additionally, little is known about how diabetes affects the treatment of cancer. One of the most effective chemotherapeutic drugs is cisplatin, which is nephrotoxic. Studies suggest that diabetes acts as a protective factor against the nephrotoxicity of cisplatin, but the mechanisms involved have not been elucidated yet. This renal protection has been attributed to decreased accumulation of cisplatin in the kidneys, which could be associated with deficient active transport of proximal tubular cells or to pharmacokinetic alterations caused by diabetes. However, it is uncertain if diabetes also compromises the antitumor activity of cisplatin. To address this issue, we developed a mouse model bearing cisplatin-induced nephrotoxicity, Sarcoma 180 and streptozotocin-induced diabetes. Four groups of treatment were defined: (i) control, (ii) diabetic, (iii) cisplatin and (iv) diabetic treated with cisplatin. The following parameters were evaluated: renal function, oxidative stress, apoptosis, renal histopathology, tumor remission, survival rate, genotoxicity and platinum concentration in tumor and several organs. Results indicate that diabetes protects against the renal damage induced by cisplatin, while also compromises its antitumor effectiveness. This is the first study to demonstrate this effect.
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http://dx.doi.org/10.1016/j.cbi.2015.01.027DOI Listing
March 2015

Contamination in a brazilian river: a risk of exposure to untreated effluents.

J Environ Qual 2013 Sep;42(5):1596-601

Due to natural or anthropogenic activities, various chemical contaminants, such as toxic metals and organic compounds, enter water systems and can have multiple deleterious effects on many living organisms. The Todos os Santos River (TSR) in Brazil receives a high discharge of untreated effluents from various sources. The purpose of this study was to determine trace element concentrations in water samples from the TSR, evaluate the toxicological effects of these elements by using the (onion) test, and verify the physical-chemical parameters to establish the risk of exposure related to the contaminated river. The samples were taken in 2011 at six selected points (two upstream of an urban area, two in the urban area, and two downstream of the urban area) with physical-chemical parameters evaluated. The concentrations of Al (21.63-1688.84 μg L), P (38.59-1760.87 μg L), and Fe (478.9-8296.3 μg L) were above the maximum levels permitted under Brazilian law (and the World Health Organization); little dissolved O was observed. Based on the test, genotoxic and mutagenic effects may occur in the river and could be due to anthropogenic increases in metal content. These important results have serious implications for the ecosystem as well as the health of the people who use the water.
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http://dx.doi.org/10.2134/jeq2013.02.0068DOI Listing
September 2013

A fast ultrasound-assisted extraction procedure for trace elements determination in hair samples by ICP-MS for forensic analysis.

Forensic Sci Int 2009 Nov 8;192(1-3):88-93. Epub 2009 Sep 8.

Laboratório de Toxicologia e Essencialidade de Metais, Depto. de Análises Clínicas, Toxicológicas e Bromatológicas, Faculdade de Ciências Farmacêuticas de Ribeirão Preto-USP, Avenida do Café s/n, Monte Alegre, Ribeirão Preto-SP, Brazil.

An ultrasound-assisted extraction method is proposed for the determination of trace elements in hair samples by inductively coupled plasma-mass spectrometry (ICP-MS) for forensic investigation. Prior to analysis, 25mg of hair samples were accurately weighed into (15 mL) conical tubes. Then, 2 mL of 20% HNO(3) is added to the samples, sonicated at 2 min (50W, 100% amplitude), and then further diluted to 10 mL with Milli-Q water. Resulted diluted slurries are centrifuged and the analytes are directly determined in the supernatant. Calibrations against aqueous solutions were carried out with rhodium as internal standard. The method was successfully applied for the extraction of Al, As, Ba, Be, Cd, Co, Cr, Cu, Mn, Pb, Tl, U, V and Zn with a method detection limit (3s, n=20) of 0.1, 0.4, 0.2, 0.09, 0.08, 0.04, 0.1, 2.9, 1.0, 0.9, 0.04, 0.05, 0.1 and 4.2 ng/g, respectively. Method accuracy is traceable to Certified Reference Materials (CRMs) 85 and 86 human hair from the International Atomic Energy Agency (IAEA). Additional validation data are provided based on the analysis of hair samples from the trace elements intercomparison program operated by the Institut National de Sante' Publique du Quebec, Canada. The proposed method is very simple and can be applied for forensic purposes with the elimination of sample digestion step prior to analysis. Then, a considerable improvement in the sample throughput is archived with the use of the proposed method.
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http://dx.doi.org/10.1016/j.forsciint.2009.08.003DOI Listing
November 2009

Determination of trace elements in biological samples by inductively coupled plasma mass spectrometry with tetramethylammonium hydroxide solubilization at room temperature.

Anal Chim Acta 2009 Jul 21;646(1-2):23-9. Epub 2009 May 21.

Departamento de Análises Clínicas, Toxicológicas e Bromatológicas, Faculdade de Ciências Farmacêuticas de Ribeirão Preto, FCFRP, USP, Avenida do Café, s/n, Monte Alegre, 14040-903, Ribeirão Preto, SP, Brazil.

A simple method for sample preparation of biological samples for trace elements determination by inductively coupled plasma mass spectrometry (ICP-MS) is described. Prior to analysis, 75 mg of the biological samples were accurately weighed into (15 mL) conical tubes. Then, 1 mL of 50% (v/v) tetramethylammonium hydroxide (TMAH) solution was added to the samples, incubated at room temperature for 12 h and the volume made up to 10 mL with a solution containing 0.5% (v/v) HNO(3), 0.01% (v/v) Triton X-100 and 10 microg L(-1) of Rh. After preparation samples may be stored at -20 degrees C during 3 days until the analysis by ICP-MS. With these conditions, the use of the dynamic reaction cell was only mandatory for chromium determination. Method detection limits were 0.2145, 0.0020, 0.0051, 0.0017, 0.0027, 0.0189, 0.02, 0.5, 0.1, 0.0030, 0.0043, 0.0066, 0.0009, 0.020, 0.0043, 0.1794, 0.1 microg(-1) for Al, As, Ba, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Pb, Sb, Se, Sr, V and Zn, respectively. Validation data are provided based on the analysis of six certified reference materials (CRMs) purchased from the National Institute of Standards and Technology (NIST) and National Research Council Canada (NRCC). Additional validation was provided by the analysis of brain, kidney, liver and heart samples collected from rats and analyzed by the proposed method and by using microwave digestion.
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http://dx.doi.org/10.1016/j.aca.2009.05.022DOI Listing
July 2009

Elevated blood lead levels in a riverside population in the Brazilian Amazon.

Environ Res 2009 Jul 22;109(5):594-9. Epub 2009 Apr 22.

Laboratório de Toxicologia e Essencialidade de Metais, Departamento de Análises Clínicas, Toxicológicas e Bromatológicas, Faculdade de Ciências Farmacêuticas de Ribeirão Preto, Universidade de São Paulo, São Paulo, Brazil.

Lead (Pb) is recognized as one of the most toxic metals. Sources of Pb exposure have been widely documented in North America, and the removal of Pb additives from gasoline was reflected in a dramatic lowering of blood Pb concentration. In Latin America, the removal of Pb from gasoline resulted in decreased exposure, but Pb levels in many areas remain high due to occupational and environmental sources of exposure. While many of the Pb sources have been identified (mining, industries, battery recycling, lead-based paint, ceramics), new ones occasionally crop up. Here we report on blood Pb (B-Pb) levels in remote riverside communities of the Brazilian Amazon. Blood Pb (B-Pb) levels were determined in 448 persons from 12 villages of the Lower Tapajós River Basin, Pará, Brazil. Socio-demographic and dietary information, as well as occupational, residential and medical history was collected using an interview-administered questionnaire. B-Pb, measured by ICP-MS, showed elevated concentrations. Mean B-Pb was 13.1 microg/dL +/- 8.5, median B-Pb was 11.2 microg/dL and ranged from 0.59 to 48.3 microg/dL. Men had higher B-Pb compared to women (median: 15.3 microg/dL vs 7.9 microg/dL respectively). B-Pb increased with age for women, while it decreased for men. For both genders, B-Pb decreased with education. There were significant differences between villages. Exploratory analyses, using linear partition models, showed that for men B-Pb was lower among those who were involved in cattle-raising, and higher among those who hunted, farmed and fished. The distribution profile of B-Pb directed us towards artisanal transformation of manioc to flour (farinha), which requires heating in a large metal pan, with stirring primarily done by young men. In the village with the highest B-Pb, analysis of Pb concentrations (dry weight) of manioc (prior to transformation) and farinha (following transformation) from 6 houses showed a tenfold increase in Pb concentration (mean: 0.017 +/- 0.016 to 0.19 +/- 0.10 microg/g). This was confirmed in one of these villages where we sampled manioc paste (just before roasting) and the roasted farinha (0.05 microg/g vs 0.20 microg/g). While there may be other sources (ammunition, sinkers for fishing nets), the high concentrations in farinha, a dietary staple, assuredly makes an important contribution. Further action needs to reduce Pb sources in this region.
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http://dx.doi.org/10.1016/j.envres.2009.03.005DOI Listing
July 2009

Exploiting dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) for sequential determination of trace elements in blood using a dilute-and-shoot procedure.

Anal Chim Acta 2009 Apr 20;639(1-2):13-8. Epub 2009 Mar 20.

Departamento de Análises Clínicas, Toxicológicas e Bromatológicas, Faculdade de Ciências Farmacêuticas de Ribeirão Preto, USP, Avenida do Café, s/n, Monte Alegre, 14040-903 Ribeirão Preto, SP, Brazil.

Inductively coupled plasma mass spectrometry with quadrupole (q-ICP-MS) and dynamic reaction cell (DRC-ICP-MS) were evaluated for sequential determination of As, Cd, Co, Cr, Cu, Mn, Pb, Se, Tl, V and Zn in blood. The method requires as little as 100 microL of blood. Prior to analysis, samples (100 microL) were diluted 1:50 in a solution containing 0.01% (v/v) Triton X-100 and 0.5% (v/v) nitric acid. The use of the DRC was only mandatory for Cr, Cu, V and Zn. For the other elements the equipment may be operated in a standard mode (q-ICP-MS). Ammonia was used as reaction gas. Selection of best flow rate of ammonium gas and optimization of the quadrupole dynamic band-pass tuning parameter (RPq) were carried out, using a ovine base blood for Cr and V and a synthetic matrix solution (SMS) for Zn and Cu diluted 1:50 and spiked to contain 1 microg L(-1) of each element. Method detection limits (3 s) for (75)As, (114)Cd, (59)Co, (51)Cr, (63)Cu (55)Mn, (208)Pb, (82)Se, (205)Tl, (51)V, and (64)Zn were 14.0, 3.0, 11.0, 7.0, 280, 9.0, 3.0, 264, 0.7, 6.0 and 800 ng L(-1), respectively. Method validation was accomplished by the analysis of blood Reference Materials produced by the L'Institut National de Santé Publique du Quebec (Canada).
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http://dx.doi.org/10.1016/j.aca.2009.03.016DOI Listing
April 2009

Trace element levels in whole blood of riparian villagers of the Brazilian Amazon.

Sci Total Environ 2009 Jun 29;407(13):4168-73. Epub 2009 Mar 29.

Laboratório de Toxicologia e Essencialidade de Metais, Departamento de Análises Clínicas, Toxicológicas e Bromatológicas, Faculdade de Ciências Farmacêuticas de Ribeirão Preto-USP, Avenida do Café s/n, Monte Alegre, Ribeirão Preto-SP, Brazil.

Monitoring the nutritional status of essential elements is of critical importance in human health. However, trace element concentrations in biological fluids are affected by environmental and physiological parameters, and therefore considerable variations can occur between specific population subgroups. Brazil is a large country with much food diversity. Moreover, dietary habits differ from north to south. As an example, the traditional populations of the Brazilian Amazon basin are heavily dependent on fish, fruits, vegetables and manioc for their daily sustenance. However, very few studies have examined to what extent these diets reflect adequate nutritional status for essential elements. Then, in the present study we have evaluated the levels of some trace elements (Cu, Co, Zn Sr, and Rb) in the whole blood of a riparian Brazilian Amazonian population and estimated the influence of age and gender on levels and inter-element interactions in the same population. For this, 253 subjects, aged 15 to 87, from 13 communities situated on the banks of the Tapajós, one of the major tributaries of the Amazon, were randomly selected. The values found for cobalt, copper and strontium in whole blood are in the same range as in other populations. On the other hand, the levels of rubidium and zinc may be considered higher. Moreover, gender was shown to influence Zn and Cu levels while age influenced the concentrations of Sr and Rb in men and Cu in women. Given the scarcity of studies examining nutritional status in traditional communities of the Amazon, our study is the first to provide relevant insight into trace element values in this region and inter-element interactions. This paper is also of particular importance for future studies looking at the possible protective effects of traditional Amazon riparian diets against mercury intake from fish consumption.
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http://dx.doi.org/10.1016/j.scitotenv.2009.02.041DOI Listing
June 2009

Flow injection spectrophotometric determination of Al in hemodialysis solutions.

J Pharm Biomed Anal 2005 Jan;36(5):1119-23

Departamento de Ciências Exatas, Escola de Farmácia e Odontologia de Alfenas-Centro Universitário Federal, Cep 37130-000 Alfenas, MG, Brazil.

A flow analysis (FA) system with spectrophotometric detection for Al determination in hemodialysis solutions was developed. The method was based on the reaction of Al with eriochrome cyanine R (ECR). The complex formed associated with cetyltrimethylammonium bromide (CTAB)--a cationic surfactant, which showed enough sensitivity to execute the direct analyte determination. All interferences were eliminated with the matrix matching calibration. The system presented the following analytic parameters: sensitivity (m) of 8.10 x 10(-4)L microg(-1), limit of detection (LOD) of 3.24 microg L(-1) (3sigma), linear correlation coefficient of 0.9966 and linear range response from 10.8 to 650 microg L(-1). The accuracy of the proposed method was checked by comparison with electrothermal atomic absorption spectrometry (ET-AAS) method. There were no differences among the results obtained from both methods, at a confidence level of 95% (paired t-test). Recovery tests were also made, values obtained were from 90.4 to 109 of recovery for Al-spiked samples.
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http://dx.doi.org/10.1016/j.jpba.2004.09.016DOI Listing
January 2005
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