A novel mixed-mode solid phase extraction for simultaneous determination of melamine and cyanuric acid in food by hydrophilic interaction chromatography coupled to tandem mass chromatography.
J Chromatogr B Analyt Technol Biomed Life Sci
; 878(28): 2839-44, 2010 Oct 15.
Article
em En
| MEDLINE
| ID: mdl-20850393
ABSTRACT
Utilizing a solid phase extraction column (MCT) containing mixed hydrophilic functional gel and cation exchange sorbent, a sensitive and rapid HPLC-MS/MS method for simultaneously determining the residues of melamine (MEL) and cyanuric acid (CYA) in human foodstuffs was developed. MEL and CYA in egg, pork, liver, kidney and pork, shrimp, sausage casing, honey, soybean milk, soybean powder and dairy product were extracted using acetonitrile/water, defatted with hexane and isolated using MCT solid phase extraction column. The residues were separated upon a hydrophilic interaction liquid chromatography (HILIC) column and analyzed by electrospray ionization under negative-positive switched mode on a triplequadrupole mass spectrometry. The selected reaction monitoring was performed on [M+H](+) of m/z 127.9 to provide the transition of 127>85 and 127>68 (MEL) while the [M-H](-) of m/z 127.1 was selected as the precursor ion for CYA resulting in product ions m/z 85 and 42. Isotope labeled internal standard ((15)N(3)-MEL and (13)C(3)-CYA) and matrix-matched calibration were both used to observe the recovery to be 70.0-129.6% and 70.0-128.9% with RSD of 1.4-23.3% and 1.5-21.7% for MEL and CYA, respectively (n=6). All the LODs and LOQs of MEL and CYA were less than 39.4 and 99.1µgkg(-1), respectively, in 18 matrices, which were sensitive enough for quantitative analysis. This method has been proven effective in simultaneous determination of melamine and cyanuric acid when inspecting unknown and positive samples.
Texto completo:
1
Coleções:
01-internacional
Base de dados:
MEDLINE
Assunto principal:
Triazinas
/
Cromatografia Líquida
/
Espectrometria de Massas em Tandem
/
Extração em Fase Sólida
/
Análise de Alimentos
Tipo de estudo:
Diagnostic_studies
Limite:
Animals
Idioma:
En
Revista:
J Chromatogr B Analyt Technol Biomed Life Sci
Assunto da revista:
ENGENHARIA BIOMEDICA
Ano de publicação:
2010
Tipo de documento:
Article