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
Objective To investigate the occurrence and concentrations of melamine and its analogues in tainted infant formula and to identify the etiologic factors for the urinary stones epidemic in infants and young children in...Objective To investigate the occurrence and concentrations of melamine and its analogues in tainted infant formula and to identify the etiologic factors for the urinary stones epidemic in infants and young children in China in 2008. Methods Sanlu infant formula samples were collected from families of the affected children in Gansu province, and markets in Gansu and Hebei provinces and Beijing city. Melamine and its analogues, including cyanuric acid, ammeline, and ammelide were measured by gas chromatography/tandem mass spectrometry. Results High prevalence and concentrations of melamine were found in Sanlu infant formula samples, with low concentrations of cyanuric acid, ammeline and ammelide. Melamine were detected in 87 out of 111 Sanlu infant formula samples with a range of 118 to 4 700 mg/kg, Conclusion The results provide strong evidence for melamine as the etiological factor for the urinary stones epidemic in infants and young children in China in 2008.展开更多
A rapid and sensitive LC-MS/MS method was established to analyze melamine and cyanuric acid in pet food and its ingredients.HILIC mechanism was utilized to separate small highly polar compounds such as melamine and cy...A rapid and sensitive LC-MS/MS method was established to analyze melamine and cyanuric acid in pet food and its ingredients.HILIC mechanism was utilized to separate small highly polar compounds such as melamine and cyanuric acid.In comparison with US FDA recognized GCMS and LC methods,it turned out that the current technique is superior with easy sample preparation,and the sensitivity and selectivity was found satisfactory.The LOD was 50 ng·L-1 for melamine and 1 μg·L-1 for cyanuric acid,respectively.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.
文摘Objective To investigate the occurrence and concentrations of melamine and its analogues in tainted infant formula and to identify the etiologic factors for the urinary stones epidemic in infants and young children in China in 2008. Methods Sanlu infant formula samples were collected from families of the affected children in Gansu province, and markets in Gansu and Hebei provinces and Beijing city. Melamine and its analogues, including cyanuric acid, ammeline, and ammelide were measured by gas chromatography/tandem mass spectrometry. Results High prevalence and concentrations of melamine were found in Sanlu infant formula samples, with low concentrations of cyanuric acid, ammeline and ammelide. Melamine were detected in 87 out of 111 Sanlu infant formula samples with a range of 118 to 4 700 mg/kg, Conclusion The results provide strong evidence for melamine as the etiological factor for the urinary stones epidemic in infants and young children in China in 2008.
文摘A rapid and sensitive LC-MS/MS method was established to analyze melamine and cyanuric acid in pet food and its ingredients.HILIC mechanism was utilized to separate small highly polar compounds such as melamine and cyanuric acid.In comparison with US FDA recognized GCMS and LC methods,it turned out that the current technique is superior with easy sample preparation,and the sensitivity and selectivity was found satisfactory.The LOD was 50 ng·L-1 for melamine and 1 μg·L-1 for cyanuric acid,respectively.
