Effectiveness of Using Zn Powder and Spongy Cadmium As Reductor on Free Nitrite and Nitrate Analysis Method Validation in Bread Samples by UV-Vis Spectrophotometry

Yussi Pratiwi, Elsa Vera Nanda, Aisyah Kistani

Abstract

This research had been carried out on the analysis of nitrite and nitrate in bread by UV-Vis spectrophotometry through a diazotization reaction. The research began by determining the optimum conditions for nitrite analysis while nitrate needs to be reduced using Zn powder or spongy cadmium so it can be analyzed by UV-Vis spectrophotometry. Ionic interference could affect nitrite analysis using UV-Vis spectrophotometry, then both nitrite and nitrate analysis methods were validated based on the method validation parameters. The diazotization reaction produced an azo compound which have λmax 546 nm. The validation results showed that the linearity of nitrite and nitrate has R2 = 0.9990 in the range 0-1 mg L-1 with a molar absorptivity value for nitrite without a reduction process was 3.37 × 104 L mol-1 cm-1, meanwhile 2.91 × 104 L mol-1 cm-1 and 3.83 × 104 L mol-1 cm-1 was shown for the reduced nitrite of Zn powder and spongy cadmium. The detection limits were 4.29 × 10-3, 9.34 × 10-3 ,and 7.58 × 10-3 mg L-1 .The %RSD results were 0.31-1.83% with recovery percentage of nitrite and nitrate in the range of 83.2-104.4%. The strongest ionic interference was shown by Fe2+ and Fe3+ ions at concentrations < 10 mg L-1. WHO has confirmed that the daily intake for nitrate that is acceptable to be consumed by human is 0-3.7 mg/kg.

Keywords

nitrite; spongy cadmium; UV-Vis spectrophotometry; Zn powder; validation method

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References

[1] S. Setiowati, R. Roto, and E. T. Wahyuni, “Monitoring Kadar Nitrit Dan Nitrat Pada Air Sumur Di Daerah Catur Tunggal YOGYAKARTA Dengan Metode Spektrofotometri Uv-vis (Monitoring of Nitrite and Nitrate Content in Ground Water of Catur Tunggal Region of YOGYAKARTA by Uv-vis Spectrophotometry),” J. Mns. dan Lingkung., vol. 23, no. 2, pp. 143–148, 2016.
doi: https://doi.org/10.22146/jml.18784

[2] T. T. Mensinga, G. J. A. Speijers, and J. Meulenbelt, “Health implications of exposure to environmental nitrogenous compounds,” Toxicol. Rev., vol. 22, no. 1, pp. 41–51, 2003.
doi: 10.2165/00139709-200322010-00005

[3] H. Kodamatani, S. Yamazaki, K. Saito, T. Tomiyasu, and Y. Komatsu, “Selective determination method for measurement of nitrite and nitrate in water samples using high-performance liquid chromatography with post-column photochemical reaction and chemiluminescence detection,” J. Chromatogr. A, vol. 1216, no. 15, pp. 3163–3167, 2009.
doi: 10.1016/j.chroma.2009.01.096

[4] C. Merusi, C. Corradini, A. Cavazza, C. Borromei, and P. Salvadeo, “Determination of nitrates, nitrites and oxalates in food products by capillary electrophoresis with pH-dependent electroosmotic flow reversal,” Food Chem., vol. 120, no. 2, pp. 615–620, 2010.
doi: https://doi.org/10.1016/j.foodchem.2009.10.035

[5] K. M. Miranda, M. G. Espey, and D. A. Wink, “A rapid, simple spectrophotometric method for simultaneous detection of nitrate and nitrite,” Nitric oxide, vol. 5, no. 1, pp. 62–71, 2001.
doi: https://doi.org/10.1006/niox.2000.0319

[6] P. Nagaraja, J. S. Prakash, and B. L. Bhaskara, “Rapid Spectrophotometric Determination of Trace Amounts of Nitrate-Nitrogen Using Dapsone and α-Naphthol,” E-Journal Chem., vol. 3, no. 3, pp. 146–153, 2006.
doi: https://doi.org/10.1155/2006/945747

[7] M. Pandurangappa and Y. Venkataramanappa, “Quantification of nitrite/nitrate in food stuff samples using 2-aminobenzoic acid as a new amine in diazocoupling reaction,” Food Anal. Methods, vol. 4, no. 1, pp. 90–99, 2011.
doi: https://doi.org/10.1007/s12161-010-9138-4

[8] S. Wang, K. Lin, N. Chen, D. Yuan, and J. Ma, “Automated determination of nitrate plus nitrite in aqueous samples with flow injection analysis using vanadium (III) chloride as reductant,” Talanta, vol. 146, pp. 744–748, 2016.
doi: 10.1016/j.talanta.2015.06.031

[9] M. N. Jones, “Nitrate reduction by shaking with cadmium: alternative to cadmium columns,” Water Res., vol. 18, no. 5, pp. 643–646, 1984.
doi: 10.1016/0043-1354(84)90215-X

[10] S. Duckett, Foundation of Spectroscopy. Oxford University Press, 2000. ISBN: 978-0198503354
Available: googlescholar

[11] J. C. Greever, “Organic Chemistry, (Fessenden, Ralph J.; Fessenden, Joan S.).” ACS Publications, 1995.
Available: googlescolar

[12] M. R. Yazdanbakhsh and A. Mohammadi, “Synthesis, substituent effects and solvatochromic properties of some disperse azo dyes derived from N-phenyl-2, 2′-iminodiethanol,” J. Mol. Liq., vol. 148, no. 1, pp. 35–39, 2009.
doi: 10.1016/j.molliq.2009.06.001

[13] B. Narayana and K. Sunil, “A spectrophotometric method for the determination of nitrite and nitrate,” Eurasian J. Anal. Chem., vol. 4, no. 2, pp. 204–214, 2009.
Available: googlescholar

[14] A. Satheshkumar et al., “Anion induced azo-hydrazone tautomerism for the selective colorimetric sensing of fluoride ion.,” Spectrochim. Acta. A. Mol. Biomol. Spectrosc., vol. 128, pp. 798–805, Jul. 2014,
doi: 10.1016/j.saa.2014.02.200.

[15] Y. H. Liou, C. J. Lin, I. C. Hung, S. Y. Chen, and S. L. Lo, “Selective reduction of NO3− to N2 with bimetallic particles of Zn coupled with palladium, platinum, and copper,” Chem. Eng. J., vol. 181, pp. 236–242, 2012.
doi: https://doi.org/10.1016/j.cej.2011.11.071

[16] M. Kumar and S. Chakraborty, “Chemical denitrification of water by zero-valent magnesium powder,” J. Hazard. Mater., vol. 135, no. 1–3, pp. 112–121, 2006. doi: 10.1016/j.jhazmat.2005.11.031

[17] V. Rosca, M. Duca, M. T. de Groot, and M. T. M. Koper, “Nitrogen cycle electrocatalysis,” Chem. Rev., vol. 109, no. 6, pp. 2209–2244, 2009.
doi: 10.1021/cr8003696

[18] L. Merino, “Development and validation of a method for determination of residual nitrite/nitrate in foodstuffs and water after zinc reduction,” Food Anal. Methods, vol. 2, no. 3, pp. 212–220, 2009.
doi: 10.1007/s12161-008-9052-1

[19] D. C. Woollard and H. E. Indyk, “Colorimetric determination of nitrate and nitrite in milk and milk powders–Use of vanadium (III) reduction,” Int. Dairy J., vol. 35, no. 1, pp. 88–94, 2014.
doi: 10.1016/j.idairyj.2013.08.011

[20] M. R. McIlvin and M. A. Altabet, “Chemical conversion of nitrate and nitrite to nitrous oxide for nitrogen and oxygen isotopic analysis in freshwater and seawater,” Anal. Chem., vol. 77, no. 17, pp. 5589–5595, 2005.
doi: 10.1021/ac050528s

[21] V. V Nikonorov and T. A. Belyanskaya, “Comparative study of various methods of the heterogeneous reduction of nitrate ions,” J. Anal. Chem., vol. 55, no. 2, pp. 116–120, 2000.
doi: 10.1007/BF02757734

[22] A. G. González and M. Á. Herrador, “A practical guide to analytical method validation, including measurement uncertainty and accuracy profiles,” TrAC Trends Anal. Chem., vol. 26, no. 3, pp. 227–238, 2007.
doi: 10.1016/j.trac.2007.01.009

[23] J. Miller and J. C. Miller, Statistics and chemometrics for analytical chemistry. Pearson education, 2018.
Available: googlescolar

[24] Departemen Kesehatan Republik Indonesia, “Bahan Tambahan Makanan,” Permenkes No.1168/Menkes/Per/X/1999, 1999.
Available: googlescolar

DOI: https://doi.org/10.20961/jkpk.v6i3.54583

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