Development of a high performance liquid chromatography method and a liquid chromatography–tandem mass spectrometry method with pressurized liquid extraction for simultaneous quantification and confirmation of cyromazine, melamine and its metabolit
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- 作者：Huan Yu ; Yanfei Tao ; Dongmei Chen ; Yulian Wang ; Zhaoying Liu ; Yuanhu Pan ; Lingli Huang ; Dapeng Peng ; Menghong Dai ; Zhenli Liu ; Zonghui Yuan
- 关键词：Cyromazine ; Melamine ; Pressurized liquid extraction ; High performance liquid chromatography ; Liquid chromatography– ; tandem mass spectrometry ; Food-producing animals
- 刊名：Analytica Chimica Acta
- 出版年：2010
- 出版时间：3 December 2010
- 年：2010
- 卷：682
- 期：1-2
- 页码：48-58
- 全文大小：907 K
文摘
Simple and sensitive methods have been developed for simultaneous detection of cyromazine, melamine and their metabolites (ammeline, ammelide and cyanuric acid) in samples of animal origins. These include a high performance liquid chromatography (HPLC) method and a liquid chromatography–tandem mass spectrometry (LC–MS/MS) method and are useful in regular monitoring and in toxicity studies of these molecules. Representative samples used in this study include muscles and livers of swine, bovine, sheep and chicken, kidneys of swine, bovine and sheep, and milk powder. A new sample preparation procedure with pressurized liquid extraction (PLE) at 1400 psi and 70 °C was investigated. Quantification of these five compounds by HPLC was achieved using an APS-2 column with UV detection at 230 nm. Limit of detection (LOD) was at 10 μg kg−1, and limit of quantification (LOQ) was at 40 μg kg−1. Recoveries of the five analytes in spiked samples ranged from 72.2 % to 115.4 % with RSD less than 12 % . Confirmatory analysis of the analytes was performed using LC–MS/MS in selected reaction monitoring (SRM) mode. The LOD and LOQ were 5 μg kg−1 and 15 μg kg−1, respectively. This is the first simultaneous analysis of cyromazine, melamine, ammeline, ammelide and cyanuric acid residues in complex tissue samples using PLE and HPLC. It is expected that these methods will find many practical applications in evaluating the safety of cyromazine, melamine and their metabolites.