RESUMO
Formaldehyde is often added to foods as a preservative, but it is highly toxic to humans, having been identified as a carcinogenic substance. It has also been used for the adulteration of milk in order to diminish the bacteria count and increase the shelf life of the product. Herein, we present a green dispersive liquid-liquid microextraction procedure in a flow-batch system for the determination of formaldehyde in milk. Pulsed flows were exploited for the first time to improve the dispersion of the extractant in the aqueous phase. The Hantzsch reaction was used for the derivatization of formaldehyde and the product was extracted with the ionic liquid (IL) trihexyltetradecylphosphonium chloride with methanol as the disperser. The flow-batch chamber was made of stainless steel with the facility for resistive heating to speed up the derivatization reaction. Spectrophotometric measurements were directly carried out in the organic phase using an optical fiber spectrophotometer. The limit of detection and coefficient of variation were 100 µg L(-1) and 3.1% (n=10), respectively, with a linear response from 0.5 to 5.0 mg L(-1), described by the equation A=0.088+0.116CF (mg L(-1)) in which A is absorbance and CF is formaldehyde concentration in mg L(-1). The estimated recoveries of formaldehyde from spiked milk samples ranged from 91% to 106% and the slopes of the analytical curves obtained with reference solutions in water or milk were in agreement, thus indicating the absence of matrix effects. Accuracy was demonstrated by the agreement of the results with those achieved by the reference fluorimetric procedure at the 95% confidence level. The proposed procedure allows for 10 extractions per hour, with minimized reagent consumption (120 µL of IL and 3.5 µL acetylacetone) and generation of only 6.7 mL waste per determination, which contribute to the eco-friendliness of the procedure.
Assuntos
Contaminação de Alimentos/análise , Formaldeído/análise , Formaldeído/isolamento & purificação , Microextração em Fase Líquida/métodos , Leite/química , AnimaisRESUMO
The present work describes the development of a fast and robust sequential injection fluorimetric procedure for the determination of Sn in juices of canned fruits. The developed automatic methodology is based on the complexation of Sn with 8-hydroxyquinoline-5-sulfonic acid (HQSA) to form a fluorimetric product (lambda(exc)=354 nm; lambda(em)=510 nm). The influence of dimethylsulfoxide (DMSO) and cetylpyridinium bromide (CPB) on the sensitivity of the fluorimetric determination was evaluated. Linear calibration plots were obtained for Sn concentrations between 1 and 10 mg L(-1), with a detection limit of 0.38 mg L(-1). In each analytical cycle 0.006 mg of HQSA and 0.47 mg of CPB were consumed and 1.5 mL of effluent was generated. The developed methodology was applied to the determination of Sn in juices of canned fruits and the results complied with those furnished by an electrothermal atomic absorption spectrometry comparison procedure, with relative deviations lower than 5.2%. The automatic procedure exhibited good precision (R.S.D.<1.4%) and the sampling rate was about 70 determinations per hour.
Assuntos
Análise de Injeção de Fluxo/métodos , Fluorometria/métodos , Análise de Alimentos/métodos , Contaminação de Alimentos/análise , Conservação de Alimentos , Frutas/química , Estanho/análise , Cetilpiridínio/química , Dimetil Sulfóxido/química , Indicadores e Reagentes/química , Oxiquinolina/análogos & derivados , Oxiquinolina/química , Fatores de Tempo , Estanho/químicaRESUMO
A tubular gas diffusion PTFE membrane is exploited for non-invasive sampling in flow analysis, aiming to develop an improved spectrophotometric determination of ethanol in alcoholic beverages. The probe is immersed into the sample, allowing ethanol to diffuse through the membrane. It is collected into the acceptor stream (acidic dichromate solution), leading to formation of Cr(III), monitored at 600 nm. The analytical curve is linear up to 50% (v/v) ethanol, baseline drift is < 0.005 absorbance during four working-hours, and sample throughput is 30 h(-1), meaning 0.6 mmol K2Cr2O7 per determination. Results are precise (r.s.d.< 2%) and in agreement with an official procedure.
Assuntos
Bebidas Alcoólicas/análise , Cromatografia Gasosa/instrumentação , Etanol/análise , Difusão , Estudos de Viabilidade , EspectrofotometriaRESUMO
Uma membrana tubular de PTFE permeável a espécies gasosas foi empregada como sonda em sistemas de análises em fluxo visando a proposta de uma estratégia de amostragem não invasiva. Como aplicação, foi selecionada a determinação espectrofotométrica de etanol em bebidas alcoólicas. A sonda é imersa na amostra, permitindo que o analito se difunda através desta e seja coletado pelo fluxo aceptor (solução ácida de dicromato), levando à formação de Cr(III), o qual é monitorado a 600 nm. Linearidade da curva analítica é verificada até 50,0% (v/v) de etanol (r > 0,998; n = 8), derivas de linha base são menores do que 0,005 absorbância durante períodos de 4 horas de operação e a velocidade analítica é de 30 h-1 o que corresponde a 0.6 mmol K2Cr2O7 por determinação. Os resultados são precisos (d.p.r. < 2%) e concordantes com aqueles obtidos por um método oficial.