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    Marcos Bezerra

    A method was developed for determination of total antimony in hair samples from patients undergoing chemotherapy against Leishmaniasis based on the administration of pentavalent antimonial drugs. The method is based on microwave assisted... more
    A method was developed for determination of total antimony in hair samples from patients undergoing chemotherapy against Leishmaniasis based on the administration of pentavalent antimonial drugs. The method is based on microwave assisted digestion of the samples in a pressurized system, reduction of Sb5+ to Sb3+ with KI solution (10% w/v) in ascorbic acid (2%, w/v) and its subsequent determination by hydride generation atomic fluorescence spectrometry (HG-AFS). The proportions of each component (HCl, HNO3 and water) used in the digestion were studied applying a constrained mixtures design. The optimal proportions found were 50% water, 25% HNO3 and 25% HCl. Variables involved in the generation of antimony hydride were optimized using a Doehlert design revealing that good sensitivity is found when using 2.0% w/v NaBH4 and 4.4 mol L-1 HCl. Under the optimum experimental conditions, the method allows the determination of antimony in hair samples with detection and quantification limits ...
    Various factors have been described as phenotypic modulators of sickle cell disease, such as levels of fetal hemoglobin (Hb F), presence of alpha-thalassemia (thal), and haplotypes of the beta-globin genes. In order to characterize and... more
    Various factors have been described as phenotypic modulators of sickle cell disease, such as levels of fetal hemoglobin (Hb F), presence of alpha-thalassemia (thal), and haplotypes of the beta-globin genes. In order to characterize and determine the frequency of the betaS and betaC mutations and the prevalence of -alpha3.7-thal, 74 patients with sickle cell disease detected during neonatal screening in the State of Pernambuco, Brazil, were studied. The haplotypes of the beta gene and -alpha3.7-thal were determined using polymerase chain reaction (PCR), and specific restriction endonucleases were used to establish the polymorphic sites of the haplotypes. The results showed the high frequency of the Central African Republic (CAR) or Bantu haplotype in the State of Pernambuco, Brazil. The low frequency of the Benin haplotype recorded in this study, in comparison with other states in northeast Brazil, suggests the diversity of origins of Afro-Brazilians in this region.
    A procedure has been developed for the simultaneous determination of traces amounts of Cd, Cr, Cu, Mn, Ni and Pb from saline oil-refinery effluents and digested vegetable samples using inductively coupled plasma optical emission... more
    A procedure has been developed for the simultaneous determination of traces amounts of Cd, Cr, Cu, Mn, Ni and Pb from saline oil-refinery effluents and digested vegetable samples using inductively coupled plasma optical emission spectrometry (ICP OES). The procedure is based on cloud point extraction (CPE) of these metals as 2-(bromo-2-pyridylazo)-5-diethyl-amino-phenol (Br-PADAP) complexes into a micellar phase of octylphenoxypolyethoxyethanol (Triton X-114). Optimization of the procedure was performed by response surface methodology (RSM) using a Doehlert design. Principal components (PC) were used to simplify the multiple response analysis. A response surface for the first PC score is useful in determining the optimum conditions for the Cd, Cr, Cu, Mn and Pb determinations whereas the second PC is highly correlated with the Ni response. Improvement factors of 22, 36, 46, 25, 65 and 39, along with limits of detection (3sigma(B)) of 0.081, 0.79, 0.38, 0.83, 0.28 and 0.69 microg L(-...
    In the present paper, a system for on-line preconcentration and determination of copper by flame atomic absorption spectrometry (FAAS) was developed. It was based on solid phase extraction of copper(II) ions on a minicolumn of Amberlite... more
    In the present paper, a system for on-line preconcentration and determination of copper by flame atomic absorption spectrometry (FAAS) was developed. It was based on solid phase extraction of copper(II) ions on a minicolumn of Amberlite XAD-2 loaded with 2-(2-thiazolylazo)-5-dimethylaminophenol (TAM). The optimisation process was carried out using Doehlert designs. Four variables (sampling flow rate, SR; elution flow rate, buffer concentration, BC; and pH) were regarded as factors in the optimisation. The parameter "sensitivity efficiency (SE)" proposed in this paper, and defined as the analytical signal obtained for an on-line enrichment system for a preconcentration time of 1 min was used as analytical response in the optimisation process. Using the established experimental conditions, the proposed on-line system allowed determination of copper with detection limit (3sigma/S) of 0.23 mug l(-1), and a precision (repeatability), calculated as relative standard deviation (R...
    To determine the geographical distribution of hemoglobinopathies in the State of Pernambuco, to characterize the children with these diseases and to describe factors associated with their follow-up at the referral center during the period... more
    To determine the geographical distribution of hemoglobinopathies in the State of Pernambuco, to characterize the children with these diseases and to describe factors associated with their follow-up at the referral center during the period from 2003 to 2010. A retrospective, cross-sectional, descriptive study was carried out of 275 medical records from a total of 302 children with hemoglobinopathies diagnosed by the National Neonatal Screening Program in the State of Pernambuco in the study period. Microsoft Excel was used for data processing and analysis. The chi-square and the Fisher test were used for statistical analysis. The level of significance was set at 5%. Terra View software was used to analyze the geographical distribution of hemoglobinopathies in the State. A total of 8.9% of the cases of hemoglobinopathies detected in the period were not followed up at the referral center. For the mothers of children with diseases, this was their second or third or more pregnancy in 64....
    This paper proposes a preconcentration procedure for determination of nickel in saline aqueous waste samples by flame atomic absorption spectrometry (FAAS). It is based on cloud-point extraction of nickel(II) ions as... more
    This paper proposes a preconcentration procedure for determination of nickel in saline aqueous waste samples by flame atomic absorption spectrometry (FAAS). It is based on cloud-point extraction of nickel(II) ions as 2-(5-bromo-2-pyridylazo)-5-diethilaminophenol (Br-PADAP) complexes using octylphenoxypolyethoxyethanol (Triton X-114) as surfactant. The optimisation step was performed using a four-variable Doehlert design, involving the factors centrifugation time (CT) of system after addition of surfactant, solution pH, methanol volume (MV) added at micellar phase, and buffer concentration (BC). The analytical response used was absorbance, after volume correction. Using the established experimental conditions in the optimisation step the procedure enables nickel determination with a detection limit (3 delta/ S) of 0.2 microg L(-1), quantification limit (10 delta/ S) of 0.7 microg L(-1), and precision, calculated as relative standard deviation ( RSD) of 4.7 ( n=8) and 3.5% ( n=8) for ...
    Infectious complications represent the main cause of morbidity and mortality in chronic lymphocytic leukemia. It has been reported that polymorphisms of the mannosebinding lectin 2 (MBL2) genes are correlated with MBL protein serum levels... more
    Infectious complications represent the main cause of morbidity and mortality in chronic lymphocytic leukemia. It has been reported that polymorphisms of the mannosebinding lectin 2 (MBL2) genes are correlated with MBL protein serum levels and, consequently, are associated with the development of infectious diseases. The purpose of this study was to investigate the possible association between MBL2 gene polymorphisms and risk of infection in chronic lymphocytic leukemia patients. Peripheral blood samples from 116 chronic lymphocytic leukemia patients were collected; after genomic DNA extraction, real time polymerase chain reaction was used to determine the polymorphisms of the promoter region and exon 1 of the MBL2 gene. A high frequency of Binet stage A (p-value = 0.005) and absence of splenomegaly (p-value = 0.002) were observed in patients with no infection; however, variant alleles/ genotypes and haplotypes of this gene had no impact on the risk of infection. To the authors' knowledge, this is the first study describing the association between MBL2 polymorphisms and infectious disease in chronic lymphocytic leukemia. Although it was not possible to demonstrate any influence of MBL2 polymorphisms as a genetic modulator of infection in chronic lymphocytic leukemia, the authors believe that the present data are clinically relevant and provide the basis for future studies.
    This paper presents a study on the viability of the use of tissues of the Leptodactylus ocellatus species (Anura Leptodactylidae) as a bioindicator of metal pollution. The study is based on the determination and correlation of the... more
    This paper presents a study on the viability of the use of tissues of the Leptodactylus ocellatus species (Anura Leptodactylidae) as a bioindicator of metal pollution. The study is based on the determination and correlation of the concentrations of manganese, chromium, zinc, nickel, copper and iron in sediments and tissues (skin, muscles and viscera) of the frog Leptodactylus ocellatus collected in the middle region of the Contas River in Bahia, Brazil. The highest levels of the metals studied were found in the viscera of this animal. In this tissue, a higher correlation of the concentration of these metals with those found in sediments was also observed. The concentrations of elements found in the skin and muscles of these amphibians have revealed no correlation with the sediment where they were collected. According to the results obtained, the viscera of the L. ocellatus species presents itself as a good bioindicator of contamination by the metals studied.
    Previous studies on the role of inflammation in the pathophysiology of sickle cell disease (SCD) suggested that the CCR5Δ32 allele, which is responsible for the production of truncated C-C chemokine receptor type 5 (CCR5), could confer a... more
    Previous studies on the role of inflammation in the pathophysiology of sickle cell disease (SCD) suggested that the CCR5Δ32 allele, which is responsible for the production of truncated C-C chemokine receptor type 5 (CCR5), could confer a selective advantage on patients with SCD because it leads to a less efficient Th1 response. We determined the frequency of the CCR5Δ32 polymorphism in 795 Afro-Brazilian SCD patients followed up at the Pernambuco Hematology and Hemotherapy Center, in Northeastern Brazil, divided into a pediatric group (3 months-17 years, n = 483) and an adult group (18-70 years, n = 312). The adult patients were also compared to a healthy control group (blood donors, 18-61 years, n = 247). The CCR5/CCR5Δ32 polymorphism was determined by allele-specific PCR. No homozygous patient for the CCR5Δ32 allele was detected. The frequency of heterozygotes in the study population (patients and controls) was 5.8%, in the total SCD patients 5.1%, in the children 5.4%, in the adults with SCD 4.8%, and in the adult controls 8.1%. These differences did not reach statistical significance. Our findings failed to demonstrate an important role of the CCR5Δ32 allele in the population sample studied here.
    Recent developments and applications in the production of thermosprays directly into flame furnaces to improve the analytical sensitivity in atomic absorption spectrometry are reviewed in this manuscript. Principles, characteristics,... more
    Recent developments and applications in the production of thermosprays directly into flame furnaces to improve the analytical sensitivity in atomic absorption spectrometry are reviewed in this manuscript. Principles, characteristics, instrumentation, and applications of this analytical technique for trace elements determination in several matrices are discussed. The use of preconcentration procedures to allow low detection limits for ultra-trace levels using TS-FF-AAS is presented and current perspectives and future trends of this technique are also discussed.
    Abstract In the present paper a procedure for simultaneous preconcentration of Cd, Cu, and Pb using cloud point extraction (CPE) and multielemental sequential determination by thermospray flame furnace atomic absorption spectrometry... more
    Abstract In the present paper a procedure for simultaneous preconcentration of Cd, Cu, and Pb using cloud point extraction (CPE) and multielemental sequential determination by thermospray flame furnace atomic absorption spectrometry (TS‐FF‐AAS) is proposed. ...
    Page 1. Microchim Acta 154, 163–167 (2006) DOI 10.1007/s00604-005-0475-8 Original Paper A Pre-Concentration Procedure Using Cloud Point Extraction for the Determination of Uranium in Natural Water Hadla Sousa Ferreira1 ...
    ... Wagna Piler Carvalho Santos a , b , Jacira Teixeira Castro c , Marcos Almeida Bezerra d , Andréa Pires Fernandes a , Sérgio Luis Costa Ferreira a and Maria Graças Andrade Korn a , Corresponding Author Contact Information , E-mail The... more
    ... Wagna Piler Carvalho Santos a , b , Jacira Teixeira Castro c , Marcos Almeida Bezerra d , Andréa Pires Fernandes a , Sérgio Luis Costa Ferreira a and Maria Graças Andrade Korn a , Corresponding Author Contact Information , E-mail The Corresponding Author. ...
    In the present paper, an on-line preconcentration procedure for determination of cadmium, copper and zinc by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) is proposed. Amberlite XAD-4 functionalized with... more
    In the present paper, an on-line preconcentration procedure for determination of cadmium, copper and zinc by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) is proposed. Amberlite XAD-4 functionalized with 3,4-dihydroxybenzoic acid (XAD4-DHB) packed in a minicolumn was used as sorbent material. The metals were retained on the XAD-DHB resin, from which it could be eluted directly to the thermospray flame furnace system. The detection limits were 28 (Cd), 100 (Cu) and 77 ng L(-1) (Zn) for 60s preconcentration time, at a sample flow rate of 7.0 mL min(-1). Enrichment factors were 102, 91 and 62, for cadmium, copper and zinc, respectively. The procedure has been applied successfully to metal determination in biological standard reference materials.
    ... To optimize a procedure that satisfies an efficient simultaneous extraction of V and U, an approach developed by Derringer and Suich44 was used, which proposed application of desirability functions for the optimization of... more
    ... To optimize a procedure that satisfies an efficient simultaneous extraction of V and U, an approach developed by Derringer and Suich44 was used, which proposed application of desirability functions for the optimization of multi-response experiments. ...
    To evaluate the long-term efficacy of concurrent radiotherapy with mitomycin-C (MMC)-based or cisplatin (CP)-based combinations in a cohort of patients with locally advanced anal canal carcinoma. Between 1988 and 2000, 179 patients with... more
    To evaluate the long-term efficacy of concurrent radiotherapy with mitomycin-C (MMC)-based or cisplatin (CP)-based combinations in a cohort of patients with locally advanced anal canal carcinoma. Between 1988 and 2000, 179 patients with locally advanced anal canal carcinoma were treated at the Instituto Nacional de Câncer with two cycles of chemotherapy during Weeks 1 and 5 of radiotherapy. 5-Fluorouracil (750 mg/m(2) 120-hour infusion or 1,000 mg/m(2) 96-hour infusion) plus CP (100 mg/m(2)) on the first day of each cycle or MMC (10-15 mg/m(2)) on the first day of Cycle 1 was administered concurrent with radiotherapy (total dose, 55-59.4 Gy). Of the 179 patients, 60% were included from a randomized trial initiated at the Instituto Nacional de Câncer in 1991 that compared concurrent chemoradiotherapy with MMC vs. CP. The median follow-up for the whole chemoradiotherapy group was 83 months. The median patient age was 58 years, 57% had Stage T3-T4 tumors, and 35% had N-positive disease. The 5-year cumulative colostomy rate was not significantly different between the CP group (22%) and MMC group (29%; p = .28). The actuarial 10-year overall survival and disease-free survival rate for the CP group was 54% and 49% and for the MMC group was 52% and 53%, respectively (p = .32 and p = .92, respectively). On multivariate analysis, male gender (p = .042) and advanced Stage T3-T4 disease (p <.0001) were statistically significant for worse disease-free survival. Stage T3-T4 (p = .039) and N+ (p = .039) disease remained independently significant for overall survival. Long-term follow-up has confirmed the good results of chemoradiotherapy with CP plus 5-fluorouracil, which seem to provide results equivalent to those with MMC plus 5-fluorouracil.
    This work presents the development of a procedure for the determination of Cr and Co from vegetal samples using graphite-furnace atomic absorption spectrometry after cloud-point extraction. The procedure is based on extraction of metals... more
    This work presents the development of a procedure for the determination of Cr and Co from vegetal samples using graphite-furnace atomic absorption spectrometry after cloud-point extraction. The procedure is based on extraction of metals from micellar media of octylphenoxypolythoxy-ethanol (Triton X-114) after complexing the metals with 2-(5-bromo-2-pyridylazo)-5-(diethylamino)-phenol [5-Br-PADAP]. A Doehlert design was used to optimize the pyrolysis and atomization temperatures and pyrolysis time in the determination of analytes trapped in the micellar phase. Ascorbic acid and palladium were used as chemical modifiers, allowing a higher pyrolysis temperature without analyte losses. Enrichment factors of 26.2 and 41.0, along with detection limits (3σB) of 23 and 12 ng L−1 for Cr and Co, respectively, were found. The precision expressed as relative standard deviation was 5.4 and 8.4% for metal concentrations of 0.5 µg L−1 (n = 8) for Cr and Co, respectively. The accuracy was evaluated through the analysis of the certified reference material NIST 1515 (apple leaves). The procedure developed in this study was applied to the determination of Cr and Co concentrations in vegetal leaf samples.
    ... DOI: 10.1080/03067310802592763 Luciane A. Escaleira a , Ricardo E. Santelli a , Eliane P. Oliveira a , Maria de Fátima B. de Carvalho b & Marcos A. Bezerra a c * pages 515-527. ... 2005. Anal. Chim. Acta , 545: 85 [CrossRef], [Web... more
    ... DOI: 10.1080/03067310802592763 Luciane A. Escaleira a , Ricardo E. Santelli a , Eliane P. Oliveira a , Maria de Fátima B. de Carvalho b & Marcos A. Bezerra a c * pages 515-527. ... 2005. Anal. Chim. Acta , 545: 85 [CrossRef], [Web of Science ®] View all references. ...
    Various factors have been described as phenotypic modulators of sickle cell disease, such as levels of fetal hemoglobin (Hb F), presence of alpha-thalassemia (thal), and haplotypes of the beta-globin genes. In order to characterize and... more
    Various factors have been described as phenotypic modulators of sickle cell disease, such as levels of fetal hemoglobin (Hb F), presence of alpha-thalassemia (thal), and haplotypes of the beta-globin genes. In order to characterize and determine the frequency of the betaS and betaC mutations and the prevalence of -alpha3.7-thal, 74 patients with sickle cell disease detected during neonatal screening in the State of Pernambuco, Brazil, were studied. The haplotypes of the beta gene and -alpha3.7-thal were determined using polymerase chain reaction (PCR), and specific restriction endonucleases were used to establish the polymorphic sites of the haplotypes. The results showed the high frequency of the Central African Republic (CAR) or Bantu haplotype in the State of Pernambuco, Brazil. The low frequency of the Benin haplotype recorded in this study, in comparison with other states in northeast Brazil, suggests the diversity of origins of Afro-Brazilians in this region.
    We describe here two new unstable beta-globin variants, Hb Caruaru and Hb Olinda, found in northeastern Brazil, both associated with chronic haemolytic anaemia. Haemoglobin Caruaru is caused by a single base substitution at codon 122... more
    We describe here two new unstable beta-globin variants, Hb Caruaru and Hb Olinda, found in northeastern Brazil, both associated with chronic haemolytic anaemia. Haemoglobin Caruaru is caused by a single base substitution at codon 122 (TTC-->TCC), possibly originating from the germ line cells of the patient's grandmother. Haemoglobin Olinda is also a de novo mutation, caused by a 12 bp deletion leading to the removal of the 22nd to the 25th residues of the normal beta-globin chain.
    ... DOI: 10.1080/05704920802031341 Valfredo Azevedo Lemos a * , Leonardo Sena Gomes Teixeira b c , Marcos de Almeida Bezerra a , Antonio Celso Spínola ... diverse analytical techniques 11. Santelli, RE, Bezerra, MD,... more
    ... DOI: 10.1080/05704920802031341 Valfredo Azevedo Lemos a * , Leonardo Sena Gomes Teixeira b c , Marcos de Almeida Bezerra a , Antonio Celso Spínola ... diverse analytical techniques 11. Santelli, RE, Bezerra, MD, Sant'Ana, OD, Cassella, RJ and Ferreira, SLC 2006. ...
    Page 1. Cloud Point Extraction as a Procedure of Separation and Pre-Concentration for Metal Determination Using Spectroanalytical Techniques: A Review Marcos de Almeida Bezerra Universidade Federal da Bahia—UFBA ...
    This paper proposes a preconcentration procedure for determination of nickel in saline aqueous waste samples by flame atomic absorption spectrometry (FAAS). It is based on cloud-point extraction of nickel(II) ions as... more
    This paper proposes a preconcentration procedure for determination of nickel in saline aqueous waste samples by flame atomic absorption spectrometry (FAAS). It is based on cloud-point extraction of nickel(II) ions as 2-(5-bromo-2-pyridylazo)-5-diethilaminophenol (Br-PADAP) complexes using octylphenoxypolyethoxyethanol (Triton X-114) as surfactant. The optimisation step was performed using a four-variable Doehlert design, involving the factors centrifugation time (CT) of system after addition of surfactant, solution pH, methanol volume (MV) added at micellar phase, and buffer concentration (BC). The analytical response used was absorbance, after volume correction. Using the established experimental conditions in the optimisation step the procedure enables nickel determination with a detection limit (3 delta/ S) of 0.2 microg L(-1), quantification limit (10 delta/ S) of 0.7 microg L(-1), and precision, calculated as relative standard deviation ( RSD) of 4.7 ( n=8) and 3.5% ( n=8) for nickel concentration of 1 and 5 microg L(-1), respectively. The preconcentration factor, determined from the ratio of the slopes of the analytical curves with and without preconcentration, is 74. The recovery achieved for nickel determination in the presence of several cations demonstrated that this procedure could be applied for analysis of water samples. The robustness was checked by using saturated fractional factorial designs, centred on the established experimental conditions in the optimisation step. The results of these tests demonstrated that the variables centrifugation time and buffer concentration are robust for modification by 10% and that solution pH and methanol volume are robust for 5%. Accuracy was evaluated by using the certified material reference SLEW-3 estuarine water for trace metals. The procedure was used for determination of nickel in saline effluents from oil refinery samples. Recovery results (95-104%) indicate that the procedure has satisfactory accuracy for nickel determination in these samples.
    A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2... more
    A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L(-1) nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 microg L(-1), respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 microg L(-1). The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.