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Please use this identifier to cite or link to this item: http://repositorio.ufla.br/jspui/handle/1/13451

Title: Rapid extraction of melamine in powdered milk for direct electrospray ionization tandem mass spectrometry analysis
???metadata.dc.creator???: Domingo, Elisângela do Carmo
Tireli, Aline Auxiliadora
Nunes, Cleiton Antonio
Batista, Alexandre Vieira
Guerreiro, Mário César
Pinto, Sandra Maria
Keywords: Melamine extraction
Trichloroacetic acid precipitation
Milk - Adulteration
Ethyl acetate extraction
Extração de melamina
Precipitação de ácido tricloroacético
Leite - Adulteração
Extração de acetato de etilo
Publisher: Elsevier
Issue Date: 15-Jan-2015
Citation: DOMINGO, E. do C. et al. Rapid extraction of melamine in powdered milk for direct electrospray ionization tandem mass spectrometry analysis. Talanta, London, v. 132, p. 535-540, 15 Jan. 2015.
Abstract: A combination of a simple pretreatment for melamine extraction and direct analysis in electrospray ionization tandem mass spectrometry (ESI–MS/MS) is proposed. Three pretreatments were evaluated. The first was based on suppressing interference using acetonitrile. The second used sulphuric acid and trichloroacetic acid to suppress interference and for melamine extraction, respectively. The third used sulphuric acid to suppress milk interference, trichloroacetic acid for melamine precipitation, and ethyl acetate for melamine extraction. However, only the last pretreatment suppressed milk interference in melamine detection and a good linearity (R2=0.99) was obtained. The presence of MS/MS 85 on melamine fragmentation spectrum showed the selectivity of this method. The limit of detection and limit of quantification were 0.269 µg L−1 and 0.897 µg L−1, respectively. The recoveries and relative standard deviation (RDS) of method were lower than 114% and 7.86%, respectively. Further, the research was extended to elucidate the nature of the melamine in the extract through infrared spectroscopy and microscopy analyses. The precipitate was characterized as melaminium bis(trichloroacetate) dihydrate, which is generated through hydrogen bound formation in an interaction between melamine and trichloroacetic acid. Therefore, a simple, fast, and easy method for melamine extraction and direct ESI–MS/MS analysis was developed.
URI: http://www.sciencedirect.com/science/article/pii/S0039914014008297?via%3Dihub
http://repositorio.ufla.br/jspui/handle/1/13451
???metadata.dc.language???: en_US
Appears in Collections:DQI - Artigos publicados em periódicos
DCA - Artigos publicados em periódicos

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