RESUMO
BACKGROUND: Fraudulent practices used to distort the quality of milk and derivatives include the addition of formaldehyde. RESULTS: A formaldehyde sensor was developed based on the luminescence of newly proposed N-doped graphene quantum dots modified with silver (N-GQDs-Ag) that were prepared using a simple method. A microdroplet of the nanoparticle dispersion was used to collect formaldehyde vapor by headspace single-drop micro-extraction (HS-SDME). After, the microdroplet was diluted in water, the nanoparticle photoluminescence quenching, caused by the analyte, was measured. The strong luminescent quenching allowed a detection limit at 1.7 × 10-4% w/v. Response was selective towards formaldehyde. SIGNIFICANCE: The method was effective and a cost-effective method for screening analysis of milk samples with matrix interferences minimized due to the nature of nanoparticle (prepared using Tollen's reagent) and due to the probing at the headspace of the sample cell. Results were statistically similar to those obtained using liquid chromatography.
Assuntos
Grafite , Pontos Quânticos , Animais , Grafite/química , Pontos Quânticos/química , Prata/química , Nitrogênio/química , Leite , Água/química , FormaldeídoRESUMO
An Eu(III) ß-diketonate complex was produced and employed as a photoluminescent probe to determine methylmercury (CH3Hg+). To establish its molecular structure, the Eu(III) complex was characterized by elemental (CHNS) and thermogravimetric analyses and infrared spectroscopy. After establishing robust conditions to use the Eu(III) complex as an analytical probe, it was employed for the analysis of produced water (PW) samples with the analytical response based on the luminescence suppression proportional to the concentration of CH3Hg+ (a linear model after normalization of the response within the concentration range from 0.2 µg L-1 up to 2.0 µg L-1). Selectivity was guaranteed by a simple liquid-liquid extraction of the analyte in dichloromethane, which also allowed a 50 times pre-concentration factor. The instrumental limit of quantification of 0.2 µg L-1 is equal to the limit established in Brazilian resolution for total mercury content in waters, but pre-concentration (50 times factor) improved the overall method limit of quantification down to 4 ng L-1. Recovery results agreed with the ones achieved using cold vapor atomic absorption spectrometry.