[Determination of melamine and cyanuric acid in milk by gas chromatography-mass spectrometry].
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.
Li
Fengge
F
Technical Center of Xinjiang Entry-Exit Inspection and Quarantine Bureau, Urumqi 830063, China. ciqlfg@163.com
Yao
Weiqin
W
Su
Min
M
Li
Shiyu
S
Dou
Hui
H
Shang
Dejun
D
Zhu
Huiping
H
D000818:Animals; D002417:Cattle; D005506:Food Contamination / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D008892:Milk / Q000737:chemistry*; D014227:Triazines / Q000032:analysis*
D014227:Triazines; C004632:cyanuric acid; C011907:melamine