Determination of Melamine in Fresh Milk by Electrochemistry with Solid Phase Microextraction at Bismuthyl Chloride Modified Graphite Epoxy Composite Electrode
Melamine as an important chemical raw material and a harmful additive in foods has attracted many people’s attention. In the present paper, The graphite-epoxy composited solid phase electrode was modified with bismuth layer by cyclic voltammetric deposition of bismuth from Bi(NO3)3 aqueous solution including 0.10 M HNO3, and hydrolyzed into micro bismuthyl chloride on-sites. Melamine in fresh milk was extracted with solid phase micro-extraction on the bismuthyl chloride modified graphite-epoxy composited solid electrode. The adsorption of melamine on bismuthyl chloride particle surfaces follows a Freundlich adsorption model, and results in the decrease of the reduction peak current of bismuth in bismuthyl chloride, and determined by differential pulse voltammetry from fresh milk in a larger concentration range of 10–4 ? 10–12 M with detection limit of 2.5 ? 10–12 M and relative standard deviation of 2.7%. The method is sensitive, convenient and was applied in the detection of melamine in fresh milk with relative deviation of 4.2% in content of 0.45 mg/kg melamine in the fresh milk.
References
[1]
[1] S. V. Levchik and E. D. Weil, “Flame Retardancy of Thermoplastic Polyesters: a Review of the Recent Lit-erature,” Polymer International Vol. 54, No. 1, January 2005, pp. 11-35. doi:org/10.1002/pi.1663
[2]
Z. Wirpsza, “Achievements in the Use of Melamine as a Chemical Raw Material. Part I. General Review and Melamine-Based Coating Resins and Coatings,” Polimery,
Vol. 41, No. 5, June 1996, pp. 265-276.
[3]
H. Walch, A. Maier, W. M. Heckl and M. Lackinger, “Isotopological Supramolecular Networks from Melamine and Fatty Acids,” The Journal of Physical Chemistry C, Vol. 113, No. 3, March 2009, pp. 1014-1019.
doi:org/10.1021/jp8078474
[4]
M. Henriksson and L. A. Berglund, “Structure and Prop-erties of Cellulose Nanocomposite Films Containing Melamine Formaldehyde,” Journal of Applied Polymer Science, Vol. 106, No. 4, November 2007, pp. 2817-2824.
doi:org/10.1002/app.26946
[5]
U. Berger and W.Schnick, “Syntheses, Crystal Structures, and Vibrational Spectroscopic Properties of MgCN2, SrCN2, and BaCN2,” Journal of Alloys and Compounds Vol. 206, No. 2, May 1994,pp. 179-184.
doi:org/10.1016/0925-8388(94)90032-9
[6]
M. Groenewolt and M. Antonietti, “Synthesis of g-C3N4 Na-Noparticles in Mesoporous Silica Host Matrices,” Advanced Materials, Vol. 17, No. 14, July 2005, pp. 1789-1792. doi:org/10.1002/adma.200401756
[7]
E. Kroke and M. Schwarz, “Novel Group 14 Nitrides,” Coordination Chemistry Review, Vol. 248, No.5-6, 2004, pp. 493-532.
[8]
L. Licea-Jiménez and R. W. Rychwalski, “Novel Nano-composites Using Carbon Nanotubes and Melamine-For-
malde-Hyde,” Materials Science-Poland Vol. 23, No. 4, January 2005, pp. 909-913.
[9]
S. Bajia, R. Sharma and B. Bajia, “Solid-State Microwave Synthesis of Melamine-Formaldehyde Resin,” Solid State Microwave Synthesis, Vol. 6, No. 1, January 2009,
pp. 120-124.
[10]
A. K. Hau, T. H. Kwan and P. K. Li, “Melamine Toxicity and the Kidney,” Journal of American Society of Ne-phrology, Vol. 20, No.2, February 2009, 245-250.
doi:org/10.1681/ASN.2008101065
[11]
D. Meter and R. J. Hemley, “Low-Compressibility Carbon Nitrides,” Science, Vol. 271, No. 5245, January 1996, pp. 53-55.
[12]
S. Ehling, S. Tefera and I. Pho, “Rapid Nondestructive Screening for Melamine in Dried Milk by Raman Spec-troscop,” Food Additives and Contaminations, Vol. 24, No. 12, November 2007, pp. 1319-1325.
[13]
S. Mfiligenzi, B. Puschner and L. S. Aston, “Diagnostic Determination of Melamine and Related Compounds in Kidney Tissue by Liquid Chromatography/Tandem Mass Spectrometry,” Journal of Agricultural Food Chemistry, Vol. 56, No. 17, September 2008, pp. 7593-7599.
doi:org/10.1021/jf801008s
[14]
J. J. Litzau, G. E. Mercer and K. J. Mulligan, “GC-MS Screen for the Presence of Melamine, Ammeline, Am-melide and Cyanuric Acid,” US FDA Laboratory Infor-mation Bulletin, No. 4423, October 2008.
http://www.cfsan.fda.gov/~frf/ lib4423.
[15]
M. Smoker and A. J. Krynitsky, “Interim Method for Detemination of Melamine and Cyanuric Acid in Food Using LC/MS-MS,” Version 1.0. US FDA Laboratory Information Bulletin, No. 4422, October 2008.
http://www.cfsan.fda.gov/~frf/lib4422.
[16]
S. Turnipseed, C. Casey, C. Nochetto and D. N. Heller, “Determination of Melamine and Cyanuric Acid Residues in Infant Formula Using LC-MS/MS,” US FDA Laboratory Information Bulletin, No. 4421, October 2008.
http://www.cfsan.fda.gov/~frf/lib4421.
[17]
J. V. Sancho, M. Ibanez and S. Grimalt, “Residue Deter-mination of Cyromazine and Its Metabolite Melamine In Chard Samples by Ion-Pair Liquid Chromatography Cou-pled to Electrospray Tandem Mass Spectrometry,” Anay-ticall Chimica Acta, Vol. 530, No. 2, February 2005, pp. 237-243.
[18]
H. Ogasawara, K. Imaida and H. Ishiwata, “Urinary Bladder Carcinogenesis Induced by Melamine in F344 Male Rats: Correlation between Carcinogenicity and Urolith formation,” Carcinogenesis, Vol. 16, No. 11, November 1995, pp. 2773-2777.
[19]
N. Serrano, N. Martin, J. Diaz-Cruz, C. Arino and M. Esteban, “Bismuth Film Electrode in Metal Complexation Studies: Stripping Analysis of the Pb(II)-, Cd(II)-, and Zn(II)- Binding with Phthalate,” Electroanalysis, Vol. 21, No. 3-5, February 2009, pp. 431-438.
[20]
F. Torma, A. Grun, I. Bitter and K. Toth, “Calixarene/ Nafion-Modified Bismuth-Film Electrodes for Adsorptive Stripping Voltammetric Determination of Lead,” Electroanalysis, Vol. 21, No. 17-18, September 2009, pp. 1961-1969.
[21]
Solubility Products at 25?C, 11/28/2007
http://www.csudh.edu/Oliver/chemdata/data-ksp.
[22]
U. S Food and Drug Administration, “Interim Melamine and Analogues Safety/Risk Assessment,” 05/22/2009
http://www.fda.gov/ScienceResearch/SpecialToics/PeerReview of Scientific Information and Assessments/ucm 155012. htm.
[23]
J. T. Nwabanne and P. K. Igbokwe, “Kinetics and Equi-librium Modeling of Nickel Adsorption by Cassava Peel,” Journal of Engineering Applied Science, Vol. 3, No. 11, November 2008, pp. 829-834.
