摘要
目的:建立尿液中三聚氰胺和三聚氰酸的液相色谱-大气压化学离子化-串联质谱(LC-APCI-MS/MS)同时测定法。方法:尿液样品以三聚氰胺-15N3和三聚氰酸-13C3为内标,加乙腈稀释、离心、Waters XBridgeTMAmide色谱柱分离后,采用APCI源、正负离子切换、多反应监测模式(MRM)进行检测。结果:三聚氰胺和三聚氰酸均在20 ng/ml～1000 ng/ml范围内线性关系良好,相关系数均大于0.995,批内、批间精密度均小于10%,提取回收率和准确度均在89.9%～111.2%之间。结论:该方法前处理简便,检测灵敏、专属,可用于尿液中三聚氰胺和三聚氰酸的快速检测。
Objective：To establish a liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometric method（LC-APCI-MS/MS） for the determination of melamine and cyanuric acid in urine samples.Methods： Urine samples were mixed with isotopic labeled internal standards,15N3-melamine and 13C3-cyanuric acid,and diluted with acetonitrile.After centrifugation and separated on a Waters XBridgeTM Amide column,the analytes were detected by APCI-MS/MS with the multiple reaction monitoring（MRM） mode,positive for melamine and negative for cyanuric acid.Results： Calibration curves were linear in the range of 20 ng/ml～1000 ng/ml for melamine and cyanuric acid,both with the correlation coefficient better than 0.995.The intra and inter-batch precision（RSD） both less than 10%,and the accuracies and recoveries were both in the range of 89.9%～111.2%.Conclusion： The method is simple,sensitive and specific for the quantitative determination of melamine and cyanuric acid in the urine.
出处
《中国卫生检验杂志》
CAS
2010年第11期2701-2703,2706,共4页
Chinese Journal of Health Laboratory Technology
