Organic Solvent-Free and Simple Method for Determining Cyromazine and Its Metabolite, Melamine, in Cow’s Milk

Abstract

This paper described an organic solvent-free, rapid, simple, and space-saving method of sample preparation followed by HPLC coupled photo-diode array (PDA) detector for simultaneous quantification of cyromazine (CYR) and its decy-cropropylated metabolite, melamine (MEL), in milk. The HPLC-PDA was performed on an Inertsil? HILIC column with an isocratic aqueous mobile phase. Analytes were extracted from the sample using water, and purified by Mono-Spin?-C18, a centrifugal monolithic silica spin mini-columns, and quantified within 20 min. The method, performed under 100% aqueous conditions, obtained average recoveries for CYR and MEL in the range of 93.2% - 99.1% with relative standard deviations ≤ 2.8%. The quantitation limits were 8.5 ng/mL for CYR and 10 ng/mL for MEL, respectively. No organic solvents were used at any stage of the analysis.

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N. Furusawa, "Organic Solvent-Free and Simple Method for Determining Cyromazine and Its Metabolite, Melamine, in Cow’s Milk," Journal of Analytical Sciences, Methods and Instrumentation, Vol. 2 No. 2, 2012, pp. 68-73. doi: 10.4236/jasmi.2012.22013.

Conflicts of Interest

The authors declare no conflicts of interest.

References

[1] FAO, Pesticide Management, JMPR Evaluation, List of Pesticides Evaluated by JMPR and JMPS, Cyromazine, JMPR No. 169, 2009 (R) Evaluation. http://www.fao.org/agriculture/crops/core-themes/theme/pests/pm/lpe/lpe-c/en/
[2] A. K. Hau, T. H. Kwan and P. K. Li, “Melamine Toxicity and the Kidney,” Journal of the American Society Nephrology, Vol. 20, 2009, pp. 245-250. doi:10.1681/ASN.2008101065 http://jasn.asnjournals.org/content/20/2/245.full.pdf+html
[3] MSDS, http://msds.chem.ox.ac.uk/index2.html
[4] International Chemical Safety Card, http://www.cdc.gov/niosh/ipcsneng/neng1154.html
[5] OSHA, “Chemical Sampling Information,” http://www.osha.gov/dts/chemicalsampling/data/CH_250440.html
[6] WHO, “Some Chemicals That Care Tumors of the Kidney or Urinary Bladder in Rodents and Some Other Substances,” http://en.wikipedia.org/wiki/Melamine#cite_note-melaminemsds-17
[7] H. D. Heck and R. W. Tyl, “The Induction of Bladder Stones by Terephthalic Acid, Dimethyl Terephthalate, and Melamine (2,4,6-Triamino-s-triazine) and Its Relevance to Risk Assessment,” Regulatory Toxicology and Pharmacology, Vol. 5, No. 3, 1985, pp. 294-313. doi:10.1016/0273-2300(85)90044-3
[8] FDA, “Protecting and Promoting Your Health,” http://www.fda.gov/Food/FoodSafety/FoodContaminantsAdulteration/ChemicalContaminants/Melamine/ucm 164520.htm
[9] WHO, Media Centre, International Experts Limit Melamine Levels in Food, http://www.who.int/mediacentre/news/releases/2010/melamine_food_20100706/en/index.html
[10] Codex, Resticide Residues in Food and Feed, Cyromazine, http://www.codexalimentarius.net/pestres/data/pesticides/details.html?id=169
[11] USDA FSIS, “Cyromazine and Melamine,” July 1991, Retrieved 27 April 2007. http://www.fsis.usda.gov/ophs/clg/Cyromazine.pdf
[12] S. Tittlemier, Health Canada, “Background Paper on Methods for the Analysis of Melamine and Related Compounds in Foods and Animal Feeds,” Ottawa, 1-4 December 2008. http://www.who.int/foodsafety/fs_management/Melamine_1.pdf
[13] H. A. Yu, Y. F. Tao, D. M. Chen, Y. L. Wang, Z. Y. Liu, Y. H. Pan, L. L. Huang, D. P. Peng, M. H. Dal, Z. L. Liu and Z. H. Yuan, “Development of a High Performance Liquid Chromatography Method and 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,” Analytica Chimica Acta, Vol. 682, No. 1-2, 2010, pp. 48-58. doi:10.1016/j.aca.2010.09.032
[14] S. S. Wang, D. M. Li, Z. D. Hua and M. P. Zhao, “Molecularly Imprinted Monolith Coupled On-Line with High Performance Liquid Chromatography for Simultaneous Quantitative Determination of Cyromazine and Melamine,” Analyst, Vol. 136, No. 18, 2011, pp. 3672-3679. doi:10.1039/c1an15086c
[15] H. W. Sun, L. X. Wang, N. Liu, F. X. Qiao and S. X. Liang, “SPE Then RP-LC for Simultaneous Analysis of Cyromazine and Its Metabolite Melamine in Liquid Milk and Egg,” Chromatographia, Vol. 70, No. 11, 2009, pp. 1685-1689. doi:10.1365/s10337-009-1355-x
[16] R. C. Wei, R. Wang, Q. F. Zeng, M. Chen and T. Z. Lui, “High-Performance liquid Chromatographic Method for the Determination of cyromazine and Melamine Residues in Milk and Pork,” Journal of Chromatographic Science, Vol. 47, 2009, pp. 581-584.
[17] P. T. Anastas, J. C. Warner, “Green Chemistry: Theory and Practice,” Oxford University Press, Oxford, 1998.
[18] T. Yoshimura, T. Nishinomiya, Y. Honda and M. Murabayashi, “Green Chemistry—Aim for the Zero Emission-Chemicals,” Sankyo Publishing Co. Ltd. Press, Tokyo, Japan, 2001.
[19] L. Huber (Ed.), “Validation and Quantification in Analytical Laboratories,” Interpharm Press, East England, 1998.
[20] ICH, “Work Products, ICH Guidelines, Quality Guidelines,” http://www.ich.org/products/guidelines.html
[21] AOAC International, “Method Validation, Guidelines & References,” http://www.aoac.org/vmeth/guidelines.htm
[22] FDA/CDER/CVM, “Guidelines for Industry—Bioanalytical Method Validation,” 2001. http://www.fda.gov/downloads/Drugs/GuidanceComplianceRegulatoryInformation/Guidances/UCM070107.pdf
[23] Codex Alimentarius Commission, ALINORM 01/23, Codex Committee on Methods of Analysis and Sampling, Joint FAO/WHO Food Standards Programme, the 23rd Section of the Codex Committee on Method of Analysis and Sampling. http://www.codexalimentarius.net/web/archives.jsp?year=01
[24] GL Sciences, Monolithic SPE Column for the Purification and Enrichment of Small Amount Sample, MonoSpin? Series. http://www.glsciences.com/products/monolithic_products/mono_spin.pdf

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