Volume 22 Issue 2
Apr.  2009
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HONG MIAO, SAI FAN, YONG-NING WU, LEI ZHANG, PING-PING ZHOU, JING-GUANG LI, HUI-JING CHEN, YUN-FENG ZHAO. Simultaneous Determination of Melamine, Ammelide, Ammeline, and Cyanuric Acid in Milk and Milk Products by Gas Chromatography-tandem Mass Spectrometry[J]. Biomedical and Environmental Sciences, 2009, 22(2): 87-94.
Citation: HONG MIAO, SAI FAN, YONG-NING WU, LEI ZHANG, PING-PING ZHOU, JING-GUANG LI, HUI-JING CHEN, YUN-FENG ZHAO. Simultaneous Determination of Melamine, Ammelide, Ammeline, and Cyanuric Acid in Milk and Milk Products by Gas Chromatography-tandem Mass Spectrometry[J]. Biomedical and Environmental Sciences, 2009, 22(2): 87-94.

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

  • 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 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. 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.
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    沈阳化工大学材料科学与工程学院 沈阳 110142

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

Abstract: 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 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. 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.

HONG MIAO, SAI FAN, YONG-NING WU, LEI ZHANG, PING-PING ZHOU, JING-GUANG LI, HUI-JING CHEN, YUN-FENG ZHAO. Simultaneous Determination of Melamine, Ammelide, Ammeline, and Cyanuric Acid in Milk and Milk Products by Gas Chromatography-tandem Mass Spectrometry[J]. Biomedical and Environmental Sciences, 2009, 22(2): 87-94.
Citation: HONG MIAO, SAI FAN, YONG-NING WU, LEI ZHANG, PING-PING ZHOU, JING-GUANG LI, HUI-JING CHEN, YUN-FENG ZHAO. Simultaneous Determination of Melamine, Ammelide, Ammeline, and Cyanuric Acid in Milk and Milk Products by Gas Chromatography-tandem Mass Spectrometry[J]. Biomedical and Environmental Sciences, 2009, 22(2): 87-94.

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