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 metabolites in foods of animal origin.
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 1400psi 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 μgkg(-1), and limit of quantification (LOQ) was at 40 μgkg(-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 μgkg(-1) and 15 μgkg(-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.
MOA Key Laboratory of Food Safety Evaluation/National Reference Laboratory of Veterinary Drug Residues (HZAU), Huazhong Agricultural University, Wuhan, Hubei 430070, China.
Huan
H
Yu
Yanfei
Y
Tao
Dongmei
D
Chen
Yulian
Y
Wang
Zhaoying
Z
Liu
Yuanhu
Y
Pan
Lingli
L
Huang
Dapeng
D
Peng
Menghong
M
Dai
Zhenli
Z
Liu
Zonghui
Z
Yuan
D000818:Animals; D002417:Cattle; D002645:Chickens; D002851:Chromatography, High Pressure Liquid / Q000191:economics / Q000379:methods*; D005504:Food Analysis / Q000191:economics / Q000379:methods*; D057230:Limit of Detection; D008460:Meat / Q000032:analysis; D008892:Milk / Q000737:chemistry; D012756:Sheep; D053719:Tandem Mass Spectrometry / Q000191:economics / Q000379:methods*; D014227:Triazines / Q000032:analysis* / Q000378:metabolism
D014227:Triazines; C028704:cyromazine; C011907:melamine