title: Rapid extraction of melamine in powdered milk for direct electrospray ionization tandem mass spectrometry analysis.
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 (R(2)=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.
authors.affiliation: Department of Food Science, Federal University of Lavras, Lavras, Minas Gerais, Brazil. Electronic address: elisangela.domingo@posgrad.ufla.br.
authors.forename: Elisângela do Carmo
authors.initials: Edo C
authors.lastname: Domingo
authors.affiliation: Department of Chemistry, Federal University of Lavras, Lavras, Minas Gerais, Brazil.
authors.forename: Aline Auxiliadora
authors.initials: AA
authors.lastname: Tireli
authors.affiliation: Department of Food Science, Federal University of Lavras, Lavras, Minas Gerais, Brazil.
authors.forename: Cleiton Antonio
authors.initials: CA
authors.lastname: Nunes
authors.affiliation: Department of Food Science, Federal University of Lavras, Lavras, Minas Gerais, Brazil.
authors.forename: Alexandre Vieira
authors.initials: AV
authors.lastname: Batista
authors.affiliation: Department of Chemistry, Federal University of Lavras, Lavras, Minas Gerais, Brazil.
authors.forename: Mário César
authors.initials: MC
authors.lastname: Guerreiro
authors.affiliation: Department of Food Science, Federal University of Lavras, Lavras, Minas Gerais, Brazil.
authors.forename: Sandra Maria
authors.initials: SM
authors.lastname: Pinto
mesh_terms: D000085:Acetates / Q000737:chemistry; D000097:Acetonitriles / Q000737:chemistry; D000818:Animals; D002417:Cattle; D005506:Food Contamination / Q000032:analysis*; D057230:Limit of Detection; D008892:Milk / Q000737:chemistry*; D011208:Powders; D012117:Resins, Synthetic / Q000302:isolation & purification*; D052616:Solid Phase Extraction / Q000379:methods*; D021241:Spectrometry, Mass, Electrospray Ionization; D013464:Sulfuric Acids / Q000737:chemistry; D014227:Triazines / Q000302:isolation & purification*; D014238:Trichloroacetic Acid / Q000737:chemistry
chemical_list: D000085:Acetates; D000097:Acetonitriles; D011208:Powders; D012117:Resins, Synthetic; D013464:Sulfuric Acids; D014227:Triazines; D014238:Trichloroacetic Acid; C007650:ethyl acetate; C011907:melamine; C033158:sulfuric acid; C032159:acetonitrile
keywords: Adulteration; Ethyl acetate extraction; Melaminium bis(trichloroacetate) dihydrate; Trichloroacetic acid precipitation