Simultaneous determination of cyromazine and melamine in poultry eggs and meat with ultra-high performance liquid chromatography-tandem mass spectrometry
10.19485/j.cnki.issn2096-5087.2025.07.023
- Author:
ZHANG Xiang
;
WU Xiaoqiong
;
GE Miaohua
;
ZHOU Ying
;
OUYANG Nan
- Publication Type:Journal Article
- Keywords:
ultra-high performance liquid chromatography-tandem mass spectrometry;
cyromazine;
melamine
- From:
Journal of Preventive Medicine
2025;37(7):751-756
- CountryChina
- Language:Chinese
-
Abstract:
Objective:To establish an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method based on solid-phase extraction column purification for simultaneous determination of cyromazine and melamine in poultry eggs and meat.
Methods:Eggs, quail eggs, and chicken were collected from markets. After homogenization, the sample was extracted with 0.5% formic acid in acetonitrile, subjected to solid-phase extraction using an MCX cartridge, and eluted with 5% ammonia in methanol. The eluate was collected, evaporated to near dryness under nitrogen, and reconstituted in a 10% aqueous methanol solution. Separated using TSK gel Amide-80 column (2.0 mm×150 mm, 5 μm), cyromazine and melamine were simultaneously detected in positive ion multiple reaction monitoring mode via tandem mass spectrometry, with quantification achieved by isotope dilution internal standard methods. Efficiency was enhanced and matrix interference minimized by optimizing conditions such as sample extraction, solid-phase extraction cartridge selection, and instrumental parameters. Calibration curves were constructed, and detection limits, quantification limits, spiked recoveries, and relative standard deviations for (RSD) of cyromazine and melamine were calculated.
Results:After method optimization, matrix effects for cyromazine and melamine ranged from 0.97 to 1.04, indicating no significant matrix suppression or enhancement. Both cyromazine and melamine exhibited excellent linearity within the concentration range of 1.0-200.0 ng/mL, with correlation coefficients ≥0.999 5. The limits of detection were 0.3 μg/kg for cyromazine and 0.5 μg/kg for melamine, the quantification limits were 1.0 and 1.5 μg/kg, respectively. At spiked levels of 1.0, 20.0, and 150.0 μg/kg, the average recoveries ranged from 78.6% to 103.1%, with RSD between 3.5% and 6.3%. Among 95 samples tested, cyromazine was detected in 6 samples and melamine in 5 samples; neither cyromazine nor melamine was detected in chicken samples.
Conclusion:The UPLC-MS/MS method established in this study enables simultaneous detection and accurate quantification of cyromazine and melamine in poultry eggs and meat.
- Full text:2025110610503937149超高效液相色谱-串联质谱法同时检测禽蛋禽肉中灭蝇胺和三聚氰胺.pdf
