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1.
Talanta ; 123: 128-34, 2014 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-24725874

RESUMO

Experimental studies of the natural photoluminescence of melamine in aqueous solutions showed that its fluorescence intensity (at 250/365 nm) was appropriated for analytical purposes. The exploitation of such melamine property provided the basis of development of a new, simple, precise and accurate method based on high performance liquid chromatography with fluorescence detection (HPLC-Fluo) to determine melamine in kitchen plastic ware following aqueous extraction using a microwave oven. Optimization of analytical parameters such as solvent composition, pH and extraction conditions led to limits of detection and quantification of melamine of 0.0081 and 0.027 µg mL(-1), respectively, with a linear range up to 10 µg mL(-1). Sample extracts fortified with melamine at three concentration levels produced an average recovery of 98±6%, which was in agreement with the results achieved with a reference HPLC-UV method. Different samples of kitchen plastic ware analyzed by the developed and optimized method showed melamine concentrations in the aqueous extract up to 17 µg mL(-1), which corresponded to 86.0 mg kg(-1) in these utensils. The results obtained indicate that the use of kitchen plastic ware made of melamine can contaminate food with this compound after heating in a microwave oven.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Utensílios de Alimentação e Culinária , Plásticos/análise , Espectrometria de Fluorescência/métodos , Triazinas/análise , Contaminação de Alimentos/análise , Concentração de Íons de Hidrogênio , Luminescência , Micro-Ondas , Plásticos/química , Reprodutibilidade dos Testes , Solventes/química , Triazinas/química , Triazinas/isolamento & purificação
2.
Food Chem ; 141(4): 3649-55, 2013 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-23993532

RESUMO

The Kjeldahl method and four classic spectrophotometric methods (Biuret, Lowry, Bradford and Markwell) were applied to evaluate the protein content of samples of UHT whole milk deliberately adulterated with melamine, ammonium sulphate or urea, which can be used to defraud milk protein and whey contents. Compared with the Kjeldahl method, the response of the spectrophotometric methods was unaffected by the addition of the nitrogen compounds to milk or whey. The methods of Bradford and Markwell were most robust and did not exhibit interference subject to composition. However, the simultaneous interpretation of results obtained using these methods with those obtained using the Kjeldahl method indicated the addition of nitrogen-rich compounds to milk and/or whey. Therefore, this work suggests a combination of results of Kjeldahl and spectrophotometric methods should be used to screen for milk adulteration by these compounds.


Assuntos
Sulfato de Amônio/análise , Técnicas de Química Analítica/métodos , Contaminação de Alimentos/análise , Proteínas do Leite/análise , Leite/química , Espectrofotometria/métodos , Triazinas/análise , Ureia/análise , Animais , Bovinos , Proteínas do Soro do Leite
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