Comparative Study of Glyphosate and AMPA Determination in Environmental Samples by Two Green Methods

DOI: 10.4236/oalib.1101553   PDF   HTML   XML   1,313 Downloads   1,975 Views   Citations


Glyphosate, N-phosphonomethyl-glycine (GLY), is a systemic post-emergence herbicide that controls weeds with great efficiency whose low cost is reflected in its wide application. In the environment, the presence of aminomethylphosphonic acid (AMPA), its main degradation product, is indicative of the application of GLY to the land. The aim of this study was to develop two analytical methods for the determination of GLY by HPLC-UV and GLY and AMPA by GC-MS, in water, soil and sediment samples. The proposed HPLC-UV method proved to be an efficient way of determining GLY in environmental samples of water, soil and sediment, eliminating the step of extraction and clean-up. On the other hand, the GC-MS method can be used to determine both GLY and AMPA simultaneously. The limits of detection (LOD) and quantitation (LOQ) for GLY by the HPLC method were 9.93 and 30.1 μg·L﹣1 for water samples, and 0.040 and 0.120 mg·kg﹣1 for soil and sediment samples, respectively. By the GC-MS method, the LOD and LOQ for GLY were 0.67 and 2.02 μg·L﹣1 for water samples, and 0.0027 and 0.0081 mg·kg﹣1 for soil and sediment samples, respectively. For AMPA, these limits were 0.15 and 0.45 μg·L﹣1 for water samples and 0.0006 and 0.0018 mg·kg﹣1 for soil and sediment samples, respectively. The recoveries ranged from 70% to 120% for water, soil and sediment samples.

Share and Cite:

Silva, B. , Benetti, F. and Rezende, M. (2015) Comparative Study of Glyphosate and AMPA Determination in Environmental Samples by Two Green Methods. Open Access Library Journal, 2, 1-11. doi: 10.4236/oalib.1101553.

Conflicts of Interest

The authors declare no conflicts of interest.


[1] Corbera, M., Hidalgo, M., Salvadó, V. and Wieczorek, P.P. (2005) Determination of Glyphosate and
Aminomethylphosphonic Acid in Natural Water Using the Capillary Electrophoresis Combined with
Enrichment Step. Analytica Chimica Acta, 540, 3-7.
[2] Amarante Junior, O.P., Santos, T.C.R., Brito, N.M. and Ribeiro, M.L. (2002) Glifosato: Propriedades,
Toxicidade, Usos e Legislação. Química Nova, 25, 420-428.
[3] Assalin, M.R., De Moraes, S.G., Queiroz, S.C.N., Ferracini, V.L. and Duran. N.J. (2010) Studies on
Degradation of Glyphosate by Several Oxidative Chemical Processes: Ozonation, Photolysis and
Heterogeneous Photocatalysis. Journal of Environmental Science and Health, Part B, 45, 89-94.
[4] Botta, F., Lavison, G., Couturier, G., Alliot, F., Moreau-Guigon, E., Fauchon, N., Guery, B., Chevreuil, M.
and Blanchoud, H. (2009) Transfer of Glyphosate and Its Degradate AMPA to Surface Waters through
Urban Sewerage Systems. Chemosphere, 77, 133-139.
[5] Hsu, C.C. and Whang, C.W. (2009) Microscale Solid Phase Extraction of Glyphosate and
Aminomethylphosphonic Acid in Water and Guava Fruit Extract Using Alumina-Coated Iron Oxide
Nanoparticles Followed by Capillary Electrophoresis and Electrochemiluminescence Detection. Journal of Chromatography A, 1216, 8575-8580.
[6] Souza, T.A., Matta, M.H.R., Montagner, E. and Abreu, A.B.G. (2006) Estudo de recuperação de glifosato e AMPA derivados em solo utilizandose resinas nacionais. Química Nova, 29, 1372-1376.
[7] Khrolenko, M.V. and Wieczorek, P.P. (2005) Determination of Glyphosate and Its Metabolite
Aminomethylphosphonic Acid in Fruit Juices Using Supported-Liquid Membrane Preconcentration Method with High-Performance Liquid Chromatography and UV Detection after Derivatization with p-Toluenesulphonyl Chloride. Journal of Chromatography A, 1093, 111-117.
[8] See, H.H., Hauser, P.C., Ibrahim, W.A.W. and Sanagi, M.M. (2010) Rapid and Direct Determination of
Glyphosate, Glufosinate, and Aminophosphonic Acid by Online Preconcentration CE with Contactless
Conductivity Detection. Electrophoresis, 31, 575-582.
[9] Börjesson, E. and Torstensson, L. (2000) New Methods for Determination of Glyphosate and
(Aminomethyl)phosphonic Acid in Water and Soil. Journal of Chromatography A, 886, 207-216.
[10] Rodríguez, J.O.N.P. (2001) Exotic Species Introductions into South America: An Underestimated Threat? Biodiversity and Conservation, 10, 1983-1996.
[11] Dornelles, C.T.A. (2006) Percepção ambiental: Uma análise na bacia hidrográfica do Rio Monjolinho, São Carlos, SP. Doctorate Thesis, Universidade de São Paulo, São Paulo.
[12] CETESB (2001) Manual de Gerenciamento de áreas Contaminadas. CETESB, São Paulo.
[14] ABNT (1984) NBR 7181—Solo-Análise Granulométrica. Associação Brasileira de Normas Técnicas—ABNT, Rio de Janeiro.
[15] Sparks, D.L., Page, A.L., Helmke, P.A., Loeppert, R.H., Soltanpour, P.N., Tabatabai, M.A., Johnston, C.T. and Sumner, M.E. (1996) Methods of Soil Analysis—Part 3: Chemical Methods. Soil Science Society of America, Madison.
[16] Alberguini, L.B.A., Silva, L.C. and Rezende, M.O.O. (2005) Tratamento de Resíduos Químicos: Guia Prático para a Solução dos Resíduos Químicos em Instituições de Ensino Superior. Rima, São Carlos.
[17] Olivares, I.R.B. and Lopes, F.A. (2012) Essential Steps to Providing Reliable Results Using the Analytical Quality Assurance Cycle. TrAC Trends in Analytical Chemistry, 35, 109-121.
[18] Barros Neto, B., Scarminio, I.S. and Bruns, R.E. (2007) Como Fazer Experimentos: Pesquisa e
Desenvolvimento na Ciência e na Indústria. 3 Edition, Editora da Universidade de Campinas, Campinas.
[20] Cantarella, H., van Raij B. and Quaggio, J.A. (1998) Soil and Plant Analyses for Lime and Fertilizer
Recommendations in Brazil. Communications in Soil Science and Plant Analysis, 29, 1691-1706.
[21] Araújo, R., Goedert, W.J. and Lacerda, M.P.C. (2007) Qualidade de um solo sob diferentes usos e
sob cerrado nativo. Revista Brasileira de Ciência do Solo, 31, 1099-1108.
[23] Brown, M.B. and Forsythe, A.B. (1974) Robust Tests for Equality of Variances. Journal of the American
Statistical Association, 69, 364-367.
[25] Ribani, M., Bottoli, C.B.G., Collins, C.H. and Jardim, I.C.S.F. (2004) Validação em métodos cromatográficos e eletroforéticos. Química Nova, 27, 771-780.

comments powered by Disqus

Copyright © 2020 by authors and Scientific Research Publishing Inc.

Creative Commons License

This work and the related PDF file are licensed under a Creative Commons Attribution 4.0 International License.