Determination of melamine and cyanuric acid in milk by gas chromatography-mass spectrometry
Li, F.; Yao, W.; Su, M.; Li, S.; Dou, H.; Shang, D.; Zhu, H.
Se Pu 27(2): 233-236
2009
ISSN/ISBN: 1000-8713 PMID: 19626856 Document Number: 631779
A gas chromatography-mass spectrometry method was developed for the quantitative determination and confirmation of melamine and cyanuric acid in milk. The milk sample was extracted with diethylamine-acetonitrile-water solution. The extract was evaporated to dryness and derivatized with N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA) and chlorotrimethylsilane (TMCS), then analyzed using gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. The external standards were used for the quantitative determination. The linear range was from 0.025 to 2 mg/kg. The average recoveries were 84%-87% for melamine and 75%-102% for cyanuric acid, and the relative standard deviations were 5.7%-11.7% for melamine and 4.9%-7.8% for cyanuric acid in the spiked levels at 0.5, 1.0 and 2.5 mg/kg. The limits of detection of melamine and cyanuric acid were 0.05 mg/kg and 0.10 mg/kg, respectively. The method is suitable for the quantitative determination and confirmation of melainine and cyanuric acid residues in milk.