Details

Autor(en) / Beteiligte

• MIAO, Hong
• FAN, Sai
• WU, Yong-Ning
• ZHANG, Lei
• ZHOU, Ping-Ping
• CHEN, Hui-Jing
• ZHAO, Yun-Feng
• LI, Jing-Guang

Titel

Simultaneous Determination of Melamine, Ammelide, Ammeline, and Cyanuric Acid in Milk and Milk Products by Gas Chromatography-tandem Mass Spectrometry

Ist Teil von

• Biomedical and environmental sciences, 2009-04, Vol.22 (2), p.87-94

Ort / Verlag

China: Elsevier B.V

Erscheinungsjahr

2009

Quelle

Elektronische Zeitschriftenbibliothek (Open access)

Beschreibungen/Notizen

• 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.