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Published:Journal of Chromatographic Science, ISSN 0021-9665 Volume 47, Number 7, August 2009, pp. 581-584

High-Performance Liquid Chromatographic Method for the Determination of Cyromazine and Melamine Residues in Milk and Pork

Ruicheng Wei1, Ran Wang1, Qingfei Zeng2, Ming Chen1, and Tiezheng Liu1,
1Jiangsu Province Key Laboratory of Animal-Derived Food Safety, Jiangsu Academy of Agricultural Science, Jiangsu, Nanjing 210014, P.R. China;
2State Key laboratory of Lake Science and Environment, Nanjing Institute of Geography and Limnology and the Graduate School of Chinese Academy of Sciences, Nanjing 210008, P.R. China TP

A high-performance liquid chromatography method is described in this paper. The method uses NH2 column and 97% acetonitrile eluate to determine the insecticide cyromazine and metabolite melamine residues in milk and pork. Samples were treated with NaOH and extracted with acetonitrile containing 20% NH4OH. Target analytes of samples were cleaned up and concentrated by C18 column solid-phase extraction. A separation for cyromazine and melamine was achieved, and respective retention times were 8 and 12 min. The calibration curves for cyromazine and melamine were linear in a concentration range of 0.01–1.0 µg/mL, with correlation coefficients of 0.9999 and 0.9997, respectively. The limit of detection of both compounds was 0.2 ng, and the limit of quantitation was 0.02 mg/kg. Recoveries of cyromazine and melamine at fortified levels of 0.02, 0.05, and 0.1 mg/kg ranged from 84.5–90.8%, and 83.6–91.3%, respectively, with coefficient of variation of 3.1–7.8%.

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