US EPA

1042742 

Journal Article 

Preparation of [13C3]-melamine and [13C3]-cyanuric acid and their application to the analysis of melamine and cyanuric acid in meat and pet food using liquid chromatography-tandem mass spectrometry 

Varelis, P; Jeskelis, R 

2008 

1 

Food Additives & Contaminants: Part A, Chemistry, Analysis, Control, Exposure & Risk Assessment
ISSN: 1944-0049
EISSN: 1944-0057 

25 

10 

1208-1215 

English 

18608503 

10.1080/02652030802101893 

WOS:000260408100005 

For the determination of melamine and cyanuric acid the labelled internal standards [(13)C(3)]-melamine and [(13)C(3)]-cyanuric acid were synthesized using the common substrate [(13)C(3)]-cyanuric chloride by reaction with ammonia and acidified water, respectively. Standards with excellent isotopic and chemical purities were obtained in acceptable yields. These compounds were used to develop an isotope dilution liquid chromatography/mass spectrometry (LC/MS) method to determine melamine and cyanuric acid in catfish, pork, chicken, and pet food. The method involved extraction into aqueous methanol, liquid-liquid extraction and ion exchange solid phase clean-up, with normal phase high-performance liquid chromatography (HPLC) in the so-called hydrophilic interaction mode. The method had a limit of detection (LOD) of 10 microg kg(-1) for both melamine and cyanuric acid in the four foods with a percentage coefficient of variation (CV) of less than 10%. The recovery of the method at this level was in the range of 87-110% and 96-110% for melamine and cyanuric acid, respectively. 

melamine; cyanuric acid; isotope dilution; tandem mass spectrometry; solid-phase extraction; hydrophilic interaction liquid chromatographic (HILIC)