Objective To 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 pro...Objective To 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）. Methods Melamine 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. Results The 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 tour 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. Conclusion This GC-MS/MS method for simultaneous determination of melamine, ammelide, ammeline, and cyanuric acid in milk and milk products is sensitive and specific.展开更多
文摘Objective To 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）. Methods Melamine 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. Results The 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 tour 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. Conclusion This GC-MS/MS method for simultaneous determination of melamine, ammelide, ammeline, and cyanuric acid in milk and milk products is sensitive and specific.
