Simultaneous determination of melamine, ammelide, ammeline, and cyanuric acid in milk and milk products by gas chromatography-tandem mass spectrometry.
- Author:
Hong MIAO
1
;
Sai FAN
;
Yong-Ning WU
;
Lei ZHANG
;
Ping-Ping ZHOU
;
Jing-Guang LI
;
Hui-Jing CHEN
;
Yun-Feng ZHAO
Author Information
- Publication Type:Journal Article
- MeSH: Animals; Cattle; Chromatography, Gas; Flame Retardants; analysis; Food Contamination; Milk; chemistry; Molecular Sequence Data; Sensitivity and Specificity; Tandem Mass Spectrometry; Triazines; chemistry
- From: Biomedical and Environmental Sciences 2009;22(2):87-94
- CountryChina
- Language:English
-
Abstract:
OBJECTIVETo develop an analytical method for simultaneously qualitative and quantitative determination of melamine and triazine-related by-products including ammelide, ammeline, and cyanuric acid in milk and milk products by gas chromatography-tandem mass spectrometry (GC-MS/MS).
METHODSMelamine and triazine-related by-products namely ammelide, ammeline and cyanuric acid in the samples were extracted in a solvent mixture of diethylamine, water, and acetonitrile (10:40:50, V/V/V). After centrifugation, an aliquot of the supernatant was evaporated to dryness under a gentle stream of nitrogen gas, and then melamine and triazine-related by-products were derivatized using BSTFA with 1% TMCS. The derivatives of melamine and its analogues were determined by gas chromatography/tandem mass spectrometry using multiple reactional monitoring (MRM) with 2, 6-Diamino-4-chloropyrimidine (DACP) being used as an internal standard.
RESULTSThe linear detectable ranges were from 0.004 mg/kg to 1.6 mg/kg for melamine, ammelide, ammeline, and cyanuric acid with a correlation coefficient no less than 0.999. The recovery rates of the four compounds in spiked blank milk powder at concentrations 0.5, 1, 2 mg/kg were between 61.4%-117.2%, and the relative standard deviation was no more than 11.5% (n=6). The detection limits of melamine, ammelide, ammeline and cyanuric acid in milk powder were 0.002 mg/kg with a ratio of signal to noise of 3.
CONCLUSIONThis GC-MS/MS method for simultaneous determination of melamine, ammelide, ammeline, and cyanuric acid in milk and milk products is sensitive and specific.