RESUMO

Purslane (Portulaca oleracea) and spinach (Spinacea oleracea) are species with elevated levels of oxalic acid, an antinutrient that interferes in the bioaccessibility of minerals such as calcium and iron. Evaluating methods to determine oxalic acid content with reduced matrix interference, such as employing Flame Atomic Absorption Spectrometry (FAAS), can enhance the specificity of determinations. The different matrices of purslane (whole plant, leaves, and juice) and spinach (whole plant) were tested using three extraction methods (M1, M2, and M3). The oxalic acid content was evaluated by UV-vis spectrophotometry and FAAS (Flame Atomic Absorption Spectrometry). The absence of the precipitation step in M1 resulted in high levels of oxalic acid in the investigated matrices. The quantification of oxalic acid by FAAS for M2 (6M HCl for 1 hour at 100°C) and M3 (0.25N HCl for 15 minutes at 100°C) in the samples of purslane leaves and spinach whole plants yielded statistically similar results. However, the analysis by UV-vis spectrophotometry for M2 and M3 showed significant discrepancies in all evaluated samples, suggesting interference from colored compounds in the food matrix.•Comparison of methods of extraction•Comparison of UV-vis spectrophotometer and FAAS in the quantification of oxalic acid•Analysis of antinutrients in plant matrices.

RESUMO

BACKGROUND: Determining metals in complex biological samples, such as milk, typically involves dry or wet decomposition. However, these techniques have limitations, including low selectivity, risk of contamination, and the use of large reagent volumes. To solve these problems, solid-phase extraction (SPE) using multifunctional sorbents has been extensively explored. In this context, this work proposed synthesizing a new restricted double access ionic imprinted polymer (RAIIP-BSA), for online SPE and determination of Cu2+ from untreated milk samples via flow injection analysis and flame atomic absorption spectrometry (FIA-FASS). RESULTS: Firstly, the polymer was obtained by bulk polymerization using Cu2+ as a template, 4-vinyl pyridine as a functional monomer, and glycidyl methacrylate as a hydrophilic comonomer. Subsequently, it was covered with bovine serum albumin, creating the restricted double access barrier. The obtained material could exclude 97 % of the proteins from milk samples. RAIIP-BSA was chemically and physically characterized. The main extraction variables were optimized via multivariate optimization. The method showed good figures of merit, such as linearity ranging from 0.05 to 1.0 mg L-1, LoD and LoQ of 0.03 and 0.05 mg L-1, intra- and interday precision ranging from 0.73 to 4.14 % and 0.16-3.68 %, and an intra- and interday accuracy ranging from 97.0 to 115.0 % and 103.0-119.0 %, respectively. SIGNIFICANCE: The developed method demonstrates the effective extraction of Cu2+ from untreated milk samples, exhibiting selectivity, high extraction capacity, prolonged sorbent (RAIIP-BSA) durability, simplicity, and swift operation. This method holds promise as an alternative to conventional metal analysis approaches in complex matrices.

Assuntos

RESUMO

In this study, a miniaturized liquid-liquid extraction (LLE) method for pre-concentration of Na, K, Ca, and Mg in crude oil was proposed. Analytes in crude oil were quantitatively extracted to the aqueous phase, followed by flame atomic absorption spectrometry (FAAS) determination. The following parameters were evaluated: type of extraction solution, sample mass, heating temperature and time, stirring time, centrifugation time, and the use of toluene and chemical demulsifier. Accuracy was evaluated by comparing the results obtained by the proposed method (LLE-FAAS) with those obtained after high-pressure microwave-assisted wet digestion and FAAS determination (reference values). No statistical difference was observed between the reference values and those using the optimized conditions for LLE-FAAS: 2.5 g of sample; 1000 µL of 2 mol L-1 HNO3, 50 mg L-1 of chemical demulsifier in 500 µL of toluene, 10 min of heating at 80 °C, 60 s of stirring, and 10 min of centrifugation. Relative standard deviations were lower than 6%. The limits of quantification (LOQ) were 1.2, 1.5, 5.0, and 0.50 µg g-1 for Na, K, Ca, and Mg, respectively. The proposed miniaturized LLE method presents several advantages, such as ease-of-use, high throughput (up 10 samples can be processed per 1 h), uses a high sample mass reaching low LOQs. In addition, the use of a diluted solution for extraction reduces the amount of reagents (around 40 times) and consequently laboratory residue generation, becoming an environmental friendly method. Suitable LOQs were achieved for analyte determination at low concentration even using a simple and low-cost sample preparation system (miniaturized LLE method) and a relatively low-cost determination technique (FAAS), avoiding the use of microwave ovens and more sensitivity techniques, which are required for routine analyses.

RESUMO

The direct magnetic sorbent sampling flame atomic absorption spectrometry (DMSS-FAAS), recently proposed by our research group, was applied to determine the lead in soy-based juice, whole grape juice, reconstituted grape juice, and orange nectar samples. A dispersive solid phase extraction (d-SPE) of lead was carried out using a magnetic orange peel powder, developed and optimized by Gupta et al (2012), that was inserted into flame by FAAS with a magnetic probe. The limits of quantification (<4.6 µg L-1) were smaller than maximum residue limits established in Brazil. Good precisions and accuracies were obtained. DMSS-FAAS presented a sensitivity at least 14 times greater than the d-SPE followed by conventional FAAS analysis, wherein the analytes were extracted and desorbed, and the eluate was introduced in FAAS via nebulization system. Lead was easily quantified in juice samples at very low concentrations, with satisfactory figures of merit, and without the need of a mineralization step.

Assuntos

RESUMO

The buoyancy of eggs and embryos is associated with successful development in pelagic fish. Buoyancy is the result of oocyte hydration, which depends on the osmotic force exerted by free amino acids (FAA) generated by yolk proteolysis, and cathepsins are the main enzymes involved in this process. Seriola lalandi is a pelagic fish whose farming has been hampered by development failure that have been partially attributed to decreased buoyancy of embryos. Therefore, the aim of this study was to compare the mRNA expression and activity of cathepsins B, D, and L, as well as the FAA content in floating and low-floating embryos at different developmental stages. The chosen stages were eggs, morula, blastula, gastrula and 24 h embryos. Complementary assessments showed that there were no differences attributed to buoyancy status in embryo and oil droplet diameters, as well as the transcriptional status at any developmental stage. Cathepsin B did not show differences in mRNA expression or activity related to buoyancy at any stage. Cathepsin D displayed higher transcript and activity levels only in low-floating eggs compared with those floating. Cathepsin L showed higher expression in floating eggs and 24 h embryos compared with that of low-floating, but the activity of this enzyme was higher in floating eggs and morula. Total FAA content constantly decreased throughout development in floating embryos, but it was always higher than low-floating embryos until gastrula stage. In 24 h embryos floating and low-floating embryos share similar quantities of FAA. In summary, differences in the expression and activity of cathepsins between floating and low-floating embryos could be revealed at specific embryonic stages, suggesting different functions of these enzymes throughout development. Besides 24 h embryos, FAA content seems to be a decisive factor for buoyancy of embryos during early development of S. lalandi. Overall, considering the main role of cathepsins and FAA in buoyancy acquisition process and therefore in both embryo quality and viability, our study identifies good marker candidates to evaluate embryo quality in the farming of this species.

RESUMO

Lead (Pb) is a potentially toxic element with significant environmental interest. Simple and sensitive analytical methods are necessary to allow determination of this element at trace levels using sample preparation procedures related to green chemistry. For this, calcium alginate beads (CA-beads), a low-cost and environmentally friendly biopolymer, have been proposed for extraction and preconcentration of Pb2+ in river water samples and determination by flame atomic absorption spectrometry (FAAS). CA-beads were prepared and applied to extract and preconcentrate Pb2+ in river water samples, providing an enrichment factor (EF) of 50, enhancement factor (E) of 54, a detection limit of 2 µg L-1, and a relative standard deviation < 5%. The extraction of Pb2+ in CA-beads achieved good selectivity, with recoveries from 94.8 to 100.2% in real samples, demonstrating the good accuracy of the proposed method. The results were also compared to those obtained by ICP-MS. The reuse of CA-beads was evaluated for six cycles, and under these conditions, the extraction and preconcentration efficiency of Pb2+ were not significantly affected. The developed methodology was applied to determine Pb2+ in water samples from rivers that are part of the hydrographic areas of Tibagi and Pitangui Rivers, in which the Pb2+ concentration was less than 2 µg L-1, a concentration lower than that established by Brazilian legislation for class I and II rivers.

Assuntos

RESUMO

In the present study, Fe, Cu, Cr, Cd, Pb, Ni, and Al concentrations in Caiman latirostris and Testudines blood from the Tapacurá reservoir, Pernambuco, Brazil, were investigated. Blood was acid digested with HNO3, and metals were determined by ICP-OES and FAAS. Lead showed concentrations below the established limit of detection. Eighty animals were evaluated, forty from each group. The levels of all elements were statistically significant when compared between the two studied taxa (p < 0.05). In caimans, significant differences between young and adults were observed for chromium (p = 0.0539) and aluminum (p = 0.0515). Testudines showed no statistically significant differences for the variable age structure. Gender did not influence metal concentrations detected in the present study for either group. Differences between species of testudines were significant for Fe between Mesoclemmys tuberculata vs Phrynops geoffroanus (p = 0.0932) and Kinosternon scorpioides vs Phrynops geoffroanus (p = 0.063). The inter-elementary correlations showed statistically significant differences between the elements Cr vs Al (R2 = 0.52), Cr vs Cd (0.43), Cd vs Cu (R2 = 0.41), Ni vs Cu (R2 = 0.31), Ni vs Cr (R2 = 0.30), Al vs Cd (R2 = 0.27), and Cd vs Fe (R2 = 0.26). It is concluded that blood is an excellent predictor of metals in crocodilians and testudines in the Tapacurá reservoir, with statistically significant differences when correlated to concentrations such as size and species studied. In addition, it evidenced data that prove the exposure of these animals to metals, with strong inter-elementary correlations and opening doors for future studies that seek to understand possible biological effects caused in the studied taxa.

Assuntos

RESUMO

Excessive sodium (Na) consumption can lead to serious health problems such as hypertension, and cardiovascular and renal diseases. Therefore, the food industry in worldwide has been trying to reduce sodium levels in processed products. The aim of this study was to validate a method and quantify sodium in processed and packaged foods and to estimate its ingestion in the consumption. In the first step, for choose the adequate analytical procedure different samples preparations (mineralization) were evaluated as wet and dry ash mineralization, as well as CsCl concentration to suppress chemical interferences for apply FAAS technique. The best performance conditions were applied for the analytical method validation: mineralization by wet digestion and adding 0.1% CsCl, which characterized the method as simple and low cost. The method was validated and was applied in 12 different processed food matrices (5 brands, 3 batches), including products of vegetable and animal origins, different majority components and interferences for Na evaluation. The results showed that sausage, hamburger, ham, bread, tomato sauce, ketchup, mustard, mayonnaise and mashed potato were classified as high-sodium foods, with mean values above 460 mg 100 g-1. It was verified that 68% of the samples were regarded as having high sodium content and the maximum value found was 2851 mg 100 g-1 for a sample of mashed potatoes. In addition, it was found that 38% of the samples presented differences in Na concentration when compared to content declared on the label. It is also observed that is possible different sodium ingestion according the combinations of processed and packaged foods in the same meal and, in this case, the sodium consumption is above than the daily value as recommended by the regulatory agencies. It was concluded that the majority of processed and packaged foods presented high sodium concentration even with efforts of the food industry to reduce the levels of this mineral and its remains an important public health problem.

Assuntos

RESUMO

A new approach to the analysis of Cu, Fe, Mn and Zn in flaxseed was developed based on infrared-assisted acid digestion. Quantitation by flame atomic absorption spectrometry yields results in agreement with those arising from aggressive total decomposition using conventional microwave-assisted (MW) digestions. A full factorial design in two levels was applied to evaluate the impact of significant variables for all elements to determine optimal experimental conditions. A desirability function revealed these to be: 2.0g sample mass, 8mL of HNO3 and 8min of heating time in the IR system. Precision better than 10% (RSD) was obtained, superior to that of a combined IR-MW approach. Sample preparation based on IR-assisted digestion provides a rapid and inexpensive alternative to other conventional techniques for the analysis of complex samples and is able to accommodate relatively large masses of sample, alleviating potential homogeneity issues as well as enhancing detection power.

Assuntos

RESUMO

The characterization of inorganic elements in the produced water (PW) samples is a difficult task because of the complexity of the matrix. This work deals with a study of a methodology for dissolved Fe quantification in PW from oil industry by flame atomic absorption spectrometry (FAAS) after cloud point extraction (CPE). The procedure is based on the CPE using PAN as complexing agent and Triton X-114 as surfactant. The best conditions for Fe extraction parameters were studied using a Box-Behnken design. The proposed method presented a LOQ of 0.010µgmL-1 and LOD of 0.003µgmL-1. The precision of the method was evaluated in terms of repeatability, obtaining a coefficient of variation of 2.54%. The accuracy of the method was assessed by recovery experiments of Fe spiked that presented recovery of 103.28%. The method was applied with satisfactory performance to determine Fe by FAAS in PW samples.

Assuntos

RESUMO

An ultrasound-assisted extraction procedure was evaluated for the multi-element determination of Cu, Mn, Ca, and Mg in alternative oilseed crops using flame atomic absorption spectrometry. The best results were obtained when 0.3g of samples were used to extract the mineral content using 10 mL of a 1.40 mol L(-1) HNO3 solution for 10 min at 25 °C. The accuracy and precision of the analysis were evaluated using two oilseed reference materials, and the results were in agreement with reference values at 95% confidence level (paired t-test). The method was used to analyze five oilseed samples and the results were in agreement with those obtained using a closed-vessel microwave-assisted acid digestion system for sample preparation. The relative standard deviations were 0.52-6.13% for all of the standard and sample measurements, and the limits of detection were 666.7, 416.7, 333.4 µg g(-1), and 3.5 mg g(-1) for Cu, Mn, Ca, and Mg, respectively.

Assuntos

RESUMO

A simple and fast ultrasound-assisted procedure for the determination of iron and zinc in infant formulas is presented. The analytical determinations were carried out by flame atomic absorption spectrometry. Multivariate experiments were performed for optimization; in addition, a comparative study was carried out using two ultrasonic devices. A method using an ultrasonic bath was selected because several samples can be prepared simultaneously, and there is less contamination risk. Analytical precision (sr(%)) was 3.3% and 4.1% for iron and zinc, respectively. Trueness was assessed using a reference material and by comparison of the results obtained analyzing commercial samples using a reference method. The results were statistically equivalent to the certified values and in good agreement with those obtained using the reference method. The proposed method can be easily implemented in laboratories for routine analysis with the advantage of being rapid and in agreement with green chemistry.

Assuntos

RESUMO

An assisted liquid-liquid extraction of copper, iron, nickel and zinc from vegetable oil samples with subsequent determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) was optimized by applying a full factorial design in two levels and the response surface methodology, Box-Behnken. The effects of the acid concentration and the amplitude, cycle and time of sonication on the extraction of the analytes, as well as their interactions, were assessed. In the selected condition (sonication amplitude = 66%, sonication time = 79 s, sonication cycle = 74%), using 0.5 mol L(-1) HCl as the extractant, the limits of quantification were 0.14, 0.20, 0.21 and 0.04 µg g(-1) for Cu, Fe, Ni and Zn, respectively, with R.S.D. ranging from 1.4% to 3.6%. The proposed method was applied for the determination of the analytes in soybean, canola and sunflower oils.

Assuntos

RESUMO

Introduction: The therapeutic monitoring of lithium, through concentration measurements, is important for individual dose adjustment, as a marker of treatment adherence and to prevent poisoning and side effects. Objectives: Validate and compare two methods - atomic emission and atomic absorption - for the determination of lithium in serum samples. Methodology: Parameters such as specificity, precision, accuracy, limit of detection (LOD) and linearity were considered. The atomic absorption spectrometer was used, operating in either emission or absorption mode. For the quantitative comparison of 30 serum samples from patients with mood disorder treated with lithium, the results were submitted to Student's t-test, F-test and Pearson's correlation. Results: The limit of quantification (LOQ) was established as 0.05 mEq/l of lithium, and calibration curves were constructed in the range of 0.05-2 mEq/l of lithium, using aqueous standards. Sample preparation time was reduced, what is important in medical laboratory. Conclusion: Both methods were considered satisfactory, precise and accurate and can be adopted for lithium quantification. In the comparison of quantitative results in lithium-treated patients through statistical tests, no significant differences were observed. Therefore the methods for lithium quantification by flame atomic absorption spectrometry (FAAS) and flame atomic emission spectrometry (FAES) may be considered similar...

Introdução: A monitorização terapêutica por meio da determinação sérica de lítio é importante para proporcionar o ajuste individual da dose, como marcador de adesão e para prevenir intoxicações. Objetivos: Validar e comparar duas metodologias, a de emissão e a de absorção atômicas, para determinação de lítio em amostras de soro. Metodologia: Foram determinados parâmetros de especificidade, precisão, exatidão, limite de detecção e linearidade a fim de validar as metodologias para determinação de lítio. Foi utilizado espectrômetro de absorção atômica, funcionando no modo de emissão ou de absorção. Para comparação das metodologias foram utilizados os testes estatísticos (teste t de Student, o teste F e a correlação de Pearson) nos resultados quantitativos de 30 amostras de soro sanguíneo de pacientes que faziam uso terapêutico de lítio para o controle do transtorno de humor bipolar (THB). Resultados: Foram estabelecidos um limite de quantificação de 0,05 mEq/l de lítio e curvas de calibração de 0,05 a 2 mEq/l de lítio, construídas utilizando padrões aquosos, com redução no tempo de preparo das amostras, principalmente para ser utilizado em laboratório de análises clínicas. Conclusão: Os dois métodos foram considerados satisfatórios, precisos e exatos e podem ser adotados para a quantificação do lítio. Na comparação dos dois métodos por testes estatísticos em amostras de pacientes tratados com o fármaco, não foram observadas diferenças significativas entre os resultados encontrados. Desta forma, os métodos para quantificação do lítio por espectrometria de absorção atômica em chama (FAAS) e espectrometria de emissão atômica em chama (FAES) podem ser considerados semelhantes...

Assuntos

RESUMO

A fast and accurate method based on ultrasound-assisted extraction in a cup-horn sonoreactor was developed to determine the total content of Cd, Co, Cr, Cu, Mn, Ni, Pb and Zn in organic fertilizers by fast sequential flame atomic absorption spectrometry (FS FAAS). Multivariate optimization was used to establish the optimal conditions for the extraction procedure. An aliquot containing approximately 120 mg of the sample was added to a 500 µL volume of an acid mixture (HNO3/HCl/HF, 5:3:3, v/v/v). After a few minutes, 500 µL of deionized water was added and eight samples were simultaneously sonicated for 10 min at 50% amplitude, allowing a sample throughput of 32 extractions per hour. The performance of the method was evaluated with a certified reference material of sewage sludge (CRM 029). The precision, expressed as the relative standard deviation, ranged from 0.58% to 5.6%. The recoveries of analytes were found to 100%, 109%, 96%, 92%, 101%, 104% and 102% for Cd, Cr, Cu, Mn, Ni, Pb and Zn, respectively. The linearity, limit of detection and limit of quantification were calculated and the values obtained were adequate for the quality control of organic fertilizers. The method was applied to the analysis of several commercial organic fertilizers and organic wastes used as fertilizers, and the results were compared with those obtained using the microwave digestion procedure. A good agreement was found between the results obtained by microwave and ultrasound procedures with recoveries ranging from 80.4% to 117%. Two organic waste samples were not in accordance with the Brazilian legislation regarding the acceptable levels of contaminants.

Assuntos

RESUMO

Arsenic is an element widely present in nature. Additionally, it may be found as different species in several matrices and therefore it is one of the target elements in chemical speciation. Although the number of studies in terrestrial plants is low, compared to matrices such as fish or urine, this number is raising due to the fact that this type of matrix are closely related to the human food chain. In speciation analysis, sample preparation is a critical step and several extraction procedures present drawbacks. In this review, papers dealing with extraction procedures, analytical methods, and studies of species conservation in plants cultivated in terrestrial environment are critically discussed. Analytical procedures based on extractions using water or diluted acid solutions associated with HPLC-ICP-MS are good alternatives, owing to their versatility and sensitivity, even though less expensive strategies are shown as feasible choices.

Assuntos

RESUMO

El Aloe vera (L.) Burm. f. (zábila) es una planta utilizada por sus propiedades medicinales, la parte utilizada de esta planta es su hoja, de ésta se extraen dos componentes: los cristales y el exudado. En esta investigación se estudió la concentración de macro elementos presentes en el exuda-do de hojas de zábila, a saber: sodio (Na), calcio (Ca), magnesio (Mg) y potasio (k) por espectrometría de absorción atómica en llama (FAAS). Las plantas estudiadas fueron cultivadas en la ciudad de Coro, estado Falcón. Las muestras compuestas de exudado se recolectaron en hojas ubi-cadas en las posiciones bajas, medias y superiores de las plantas. Luego se secaron por liofilización, y se mineralizaron: 0.25 g de muestra de exudado se sometieron a digestión ácida, con 1:2 HNO3 concentrado y H2O2 en plancha de calentamiento. Se utilizó material certificado NIST 1572, USA: Hojas de plantas cítricas, para evaluar la exactitud del método, no encontrándose diferencias estadísticamente significativas (p <0.05) entre los valores del material de referencia con los valores obtenidos con el método aplicado en esta investigación. El promedio de la desviación estándar relativa (RSD) fue de 1.41%, lo que certifica la precisión del método empleado. Las concentraciones de los macro elementos encontradas fueron: Na: 0.24 ± 0,03% p/p, k: 0.69 ± 0,13% p/p, Ca: 0.07 ± 0,01% p/p y Mg: 0.01 ± 0,00% p/p. El método empleado para determinar la concentración de Na, Ca, Mg y k en muestras de exudado de zábila por FAAS fue exacto, preciso y libre de interferencias.

The objective of this work was to determine the metals in Aloe vera (L.) Burm. f. (zabila). Theses metals are necessary in the human organism; namely: Na, k, Ca y Mg. It was digested for 1 hour in a hot plate at 70 ºC 0.25 g of lyo-philized exudate with 1:2 nitric acidic and hydrogen peroxi-de. It was no found significatives statistics differences at 95% of confidence between the standard calibration curve and the aqueous calibration curve, so no matrix effect was observed. The recovery studies was satisfactory, the mean value was 99.77 ± 2%. It was no found significatives statistics differences at 95% of confidence between the certificated values (NBS: Citrics leaves 1572) of studied metals and the values found with the applied methodology. The concentrations of these elements in the real composed samples were: Na: 0.24 ± 0,03% w/w; k: 0.69 ± 0,13% w/w; Ca: 0.07 ± 0,01% w/w; Mg: 0.01 ± 0,00% w/w. The method used to determine the determined elements was exact, pre-cise and free from interferences.

Assuntos

RESUMO

En esta investigacion se estudio la concentracion de microelementos tales como cobre, zinc, manganeso y hierro en el acibar de hojas de zabila, por espectrometria de absorcion atomica en llama (FAAS); asimismo, la concentracion de cromo por espectrometria de absorcion atomica electrotermica (ETAAS). Las plantas fueron cultivadas en la ciudad de Coro, estado Falcon, Venezuela. Las muestras de aci bar se recolectaron en hojas internas, medias y externas de la planta. Luego, se secaron por liofilizacion y se mineralizaron: 0,25 g de muestra de acibar se sometio a digestion humeda por 1 hora a 70 oC en una plancha de calentamiento, con 1:2 HNO3 y H2O2. No se encontro efecto de matriz, ya que no hubo diferencia estadisticamente significativa entre la pendiente de la curva de calibracion acuosa y la obtenida por adicion de estandar. El estudio de recuperacion fue satisfactorio, siendo el valor promedio 97,02 ± 4,65%. La exactitud del metodo se evaluo utilizando material certificado de la National Bureau of Standards (NBS) 1572, no encontrandose diferencias estadisticamente significativas entre los valores de los metales contenidos en el material de referencia con los valores obtenidos con el metodo aplicado en esta investigacion. Con relacion a la precision, el promedio de la desviacion estandar relativa fue de 1,26%, lo que certifica la precision del metodo empleado. Las concentraciones de metales (media poblacional ± intervalos de confianza) encontradas fueron las siguientes: Cu: 1.604 ± 0.296 mg/g, zn: 6.381 ± 0.974 mg/g, Fe: 14.609 ±3.161 mg/g, Mn: 5.058 ± 0.307 mg/g y Cr: 13.174 ± 3.046 mg/g. El metodo empleado fue exacto, preciso y libre de interferencias.

In this investigation was studied the concentration of microelements such as: Cu, zn, Fe and Mn in Aloe vera (L.) Burm. f. leaves exudates by atomic absorption spectrometry (FAAS), also the Cr concentration was determined by electrothermal atomic absorption spectrometry (ETAAS). The plants were cultivated in Coro city, Falcon state, Venezuela. The exudates samples were recollected from internal external and intermediate leaves of the plant. It was digested for 1 hour in a hot plate at 70 oC 0.25g of lyophilized exudates with 1:2 nitric acidic and hydrogen peroxide. It was no found significatives statistics difference at 95% of confidence between the standard calibration curve and the aqueous calibration curve, so no matrix effect was observed. The recovery studies was satisfactory, the mean value was 97.02 ± 4.65%. It was no found significatives statistics differences at 95% of confidence between the certificated values from The National Bureau of Standards (NBS) 1572 of studied metals and the values found with the applied methodology, so the method applied was accurate. The precision of the method was 1.26%. The concentrations of these elements in the real samples were: Cu: 1,604 ± 0,296 mg/g; zn: 6,381 ± 0,974 mg/g; Fe: 14,609 ± 3,161 mg/g; Mn: 5,058 ± 0,307 mg/g and Cr: 13,174 ± 3,046 mg/g. The method used to determine these elements was exact, precise and free from interferences.

Assuntos

RESUMO

INTRODUÇÃO: O cobre é um nutriente essencial para os humanos, e a manutenção dos seus níveis é importante, uma vez que seu metabolismo está envolvido com estresse oxidativo e patologias, como a Doença de Wilson. Neste trabalho, um método de espectrofotometria visível (espectrofotometria Vis) foi validado, aplicado em indivíduos jovens e comparado com espectrometria de absorção atômica com chama (EAA-chama). MÉTODOS: Concentrações séricas de cobre foram medidas por EAA-chama e por espectrofotometria Vis, através da reação de cobre com batocuproína, l = 484 nm. Curvas analíticas em solução aquosa e com adição de padrão foram efetuadas para verificar linearidade, recuperação e precisão do método espectrofotométrico. Amostras de sangue de 12 indivíduos (média de idade 22 anos) foram analisadas por ambos os métodos e comparadas entre si. Os resultados foram expressos em média ± desvio-padrão. RESULTADOS: As curvas com adição de padrão e aquosa (n = 5) apresentaram coeficientes de regressão superiores a 0,99 e de variação inter e intradia inferiores a 15 por cento. Os valores de cobre sérico encontrados para o método espectrofotométrico foram 1,17 ± 0,39 e 0,73 ± 0,14 mg/l para mulheres e homens, respectivamente. Para EAA-chama foram encontrados 1,13 ± 0,43 e 0,59 ± 0,13 mg/l para mulheres e homens, respectivamente. Os resultados mostraram correlação de Pearson significativa (r = 0,946; p < 0,05). Os níveis séricos de cobre foram significativamente maiores em mulheres do que em homens (p < 0,05). CONCLUSÃO: O método espectrofotométrico visível demonstrou ser linear, reprodutível e aplicável, oferecendo uma alternativa confiável à quantificação de cobre por EAA-chama. Além disso, é uma técnica simples, rápida e barata, que pode ser utilizada na rotina laboratorial clínica.

BACKGROUND: Copper is an essential nutrient for humans and maintenance of its adequate levels is important, since its metabolism is involved with oxidative stress and patolologies, such as Wilson's disease. In this work, a visible spectrophotometric method was validated, applied in young subjects and compared to flame atomic absorption spectrometry (FAAS) in serum copper levels determination. METHODS: Serum copper concentrations were measured by FAAS and by spectrophotometry, through copper reaction with bathocuproine, l = 484 nm. Aqueous curves and spiked serum curves were realized to verify linearity, recovery and precision of the visible spectrophotometric method. Blood samples from 12 subjects (mean 22 years) were analyzed in both methodologies and compared to each other. The results were expressed by mean ± standard deviation. RESULTS: Spiked serum and aqueous curves (n = 5) showed coefficient of regression superior to 0.99 and inter and intra-day coefficient of variation lower than 15 percent. The serum copper values found to Vis spectrophotometric method were 1.17 ± 0.39 and 0.73 ± 0.14 mg/l to women and men, respectively. To FAAS 1.13 ± 0.43 and 0.59 ± 0.13 mg/l were found to women and men, respectively. Both results showed a significant Pearson correlation (r = 0.946; p < 0.05). Besides, serum copper levels were significantly higher in women than in men (p < 0.05). CONCLUSION: The Vis spectrophotometric method demonstrated to be linear, reproducible and applied, offering a reliable alternative to FAAS copper quantification. Moreover, Vis spectrophotometry is a simple, quickly and not expensive technique, and it could be widely used as routine in clinical laboratory.

Assuntos