Nestlé Research Centre, Nestec Limited, Vers-chez-les-Blanc, 1000 Lausanne 26, Switzerland.
J Agric Food Chem. 2010 Nov 24;58(22):11574-9. doi: 10.1021/jf102900k. Epub 2010 Nov 1.
As a consequence of the adulteration of infant formulas and milk powders with melamine (MEL) in China in 2008, much attention has been devoted to the analysis of MEL [and cyanuric acid (CA)] in dairy products. Several methods based on high-performance liquid chromatography (HPLC), liquid chromatography-tandem mass spectrometry (LC-MS/MS), nuclear magnetic resonance (NMR), or Raman spectroscopy have been described in the literature. However, no method is available for the simultaneous determination of MEL and CA in other raw materials, which are considered as high-risk materials for economically motivated adulteration. The present paper reports the results of an interlaboratory-based performance evaluation conducted with seven laboratories worldwide. The purpose was to demonstrate the ability of a cleanup-free LC-MS/MS method, originally developed for cow's milk and milk-powdered infant formula, to quantify MEL and CA in egg powder and soy protein. Limit of detection (LOD) and limit of quantification (LOQ) were 0.02 and 0.05 mg/kg for MEL in egg powder and soy protein, respectively. For CA, LOD and LOQ were 0.05 and 0.10 mg/kg in egg powder and 1.0 and 1.50 mg/kg in soy protein, respectively. Recoveries ranged within a 97-113% range for both MEL and CA in egg powder and soy protein. Reproducibility values (RSD(R)) from seven laboratories were within a 5.4-11.7% range for both analytes in the considered matrices. Horwitz ratio (HorRat) values between 0.4 and 0.7 indicate acceptable among-laboratory precision for the method described.
由于 2008 年中国婴儿配方奶粉和牛奶粉中三聚氰胺(MEL)的掺假事件,人们对乳制品中 MEL[和三聚氰酸(CA)]的分析给予了极大关注。文献中已经描述了几种基于高效液相色谱(HPLC)、液相色谱-串联质谱(LC-MS/MS)、核磁共振(NMR)或拉曼光谱的方法。然而,尚无方法可用于同时测定其他原材料中的 MEL 和 CA,这些原材料被认为是出于经济动机掺假的高风险材料。本文报告了在全球 7 个实验室进行的基于实验室间的性能评估的结果。目的是证明最初为牛奶和牛奶配方奶粉开发的无需净化的 LC-MS/MS 方法能够定量测定蛋粉和大豆蛋白中的 MEL 和 CA。在蛋粉和大豆蛋白中,MEL 的检测限(LOD)和定量限(LOQ)分别为 0.02 和 0.05mg/kg。对于 CA,在蛋粉中的 LOD 和 LOQ 分别为 0.05 和 0.10mg/kg,在大豆蛋白中的 LOD 和 LOQ 分别为 1.0 和 1.50mg/kg。在蛋粉和大豆蛋白中,MEL 和 CA 的回收率均在 97-113%范围内。在考虑的基质中,7 个实验室的重复性值(RSD(R))分别在 5.4-11.7%范围内。Horwitz 比值(HorRat)在 0.4 到 0.7 之间,表明该方法具有可接受的实验室间精密度。