Institute of Chemical Technology Prague, Faculty of Food and Biochemical Technology, Department of Food Chemistry and Analysis, Technická 5, 16628 Prague 6, Czech Republic.
J Chromatogr A. 2010 Jun 18;1217(25):4204-11. doi: 10.1016/j.chroma.2010.03.014. Epub 2010 Mar 18.
The use of fast semi-automated method employing direct analysis in real time (DART) ion source coupled to time-of-flight mass spectrometry (TOFMS) for analysis of melamine (MEL) and cyanuric acid (CYA) in milk powder and milk based products has been demonstrated in this study. Simple sample extraction procedure employing methanol-5% aqueous formic acid mixture, which enabled disruption of melamine-cyanurate complex, was followed by direct, high-throughput (30s per run) examination of sample extracts spread on a glass rod by mass spectrometry under ambient conditions, without any prior chromatographic separation. After optimization of instrument parameter settings, limits of detection (LODs) 170 and 450microgkg(-1) were achieved for MEL and CYA, respectively. In the final phase of study, the possibility of minimizing spectral interference, thus improving method performance characteristics through the use of ultrahigh resolving power offered by Orbitrap based mass analyzer is demonstrated.
本研究中展示了一种快速半自动分析方法，采用直接实时分析（DART）离子源与飞行时间质谱（TOFMS）联用，用于检测奶粉和奶基产品中的三聚氰胺（MEL）和三聚氰酸（CYA）。该方法采用甲醇-5%甲酸水溶液进行简单的样品提取，可破坏三聚氰胺-三聚氰酸复合物，然后在环境条件下通过质谱对直接、高通量（每次运行 30 秒）的玻璃棒上样品提取物进行分析，无需任何预先的色谱分离。在优化仪器参数设置后，MEL 和 CYA 的检测限（LOD）分别达到 170 和 450μgkg(-1)。在研究的最后阶段，通过使用基于轨道阱的质量分析仪提供的超高分辨率，证明了最小化光谱干扰的可能性，从而改善了方法的性能特征。
