Atrazine and 2, 4-D determination in corn samples using microwave assisted extraction and on-line solid-phase extraction coupled to liquid chromatography.


  • Ana Susana Santos-Hernández Universidad Autónoma de Nuevo León (UANL) Facultad de Ciencias Químicas
  • Laura Hinojosa-Reyes Universidad Autónoma de Nuevo León (UANL) Facultad de Ciencias Químicas
  • Isabel del Carmen Sáenz-Tavera Universidad Autónoma de Nuevo León (UANL) Facultad de Ciencias Químicas
  • Aracely Hernández-Ramírez Universidad Autónoma de Nuevo León (UANL) Facultad de Ciencias Químicas
  • Jorge Luis Guzmán-Mar Universidad Autónoma de Nuevo León (UANL) Facultad de Ciencias Químicas



herbicide, corn, microwave assisted extraction, on line SPE-HPLC/UV.


On-line sample pretreatment (clean-up and analyte preconcentration) was coupled to sequential injection chromatography for the determination of 2, 4-D (2,4-dichlorophenoxyacetic acid) and atrazine in corn samples. Prior to their analysis, microwave-assisted approach was evaluated and optimized for the extraction of 2,4-D and atrazine in corn samples. Extraction was carried out using MeOH:water (30:70 v/v) solvent at 50°C for 15 min. The on-line SPE-HPLC/UV approach combined reversed solid-phase extraction using strata X sorbent with MeOH:H2O (80:20 v/v) at 1 mL min-1 as eluent for the enrichment of the analytes. C18 monolithic column with acetonitrile:10 mM acetate buffer pH 4 (20:80, v/v) was employed as mobile phase at 2 mL min-1 flow rate for separation of the compounds before UV detection. Enrichment factors up to 13.4 were achieved with a 10 mL sample volume. The developed procedure showed linear response ranges from 0.07–0.70 mg kg−1 for 2,4-D and atrazine with correlation coefficients >0.993. The LODs were 0.03 and 0.02 mg kg-1 for 2,4-D and atrazine, respectively with RSD ranged from 4.0 to 7.2 % at 0.07 and 0.30 mg kg-1. The recoveries of 2,4-D and atrazine in corn samples were from 82.6 and 98.2%. The proposed method showed good recoveries and reasonable precision for herbicide analysis in corn samples avoiding the time-consuming batch sample pretreatment step, thus minimizing risks of sample contamination and analyte losses.


Download data is not yet available.


Gaba, S., et al. Scientific reports. 2016, 6, 30112

Islam, F., et al. Environment international. 2017,

Zhang, L., et al. Talanta. 2014, 122, 43-50

Barchanska, H.; Rusek, M.; Szatkowska, A. Environmental monitoring and assessment. 2012, 184, 321-34

Kock-Schulmeyer, M., et al. The Science of the total environment. 2013, 458-460, 466-76

Handford, C. E.; Elliott, C. T.; Campbell, K. Integrated environmental assessment and management. 2015, 11, 525-36

Cunha, S. C.; Fernandes, J. O. Journal of chromatography. A. 2011, 1218, 7748-57

Barchanska, H., et al. Environmental science and pollution research international. 2017, 24, 644-658

Hou, X., et al. Food Chem. 2013, 138, 1198-205

Behbahani, M., et al. Environmental monitoring and assessment. 2014, 186, 2609-18

Shamsipur, M., et al. Journal of separation science. 2012, 35, 2718-24

Zhao, Q., et al. Journal of chromatography. A. 2015, 1376, 26-34

Guo, F., et al. Talanta. 2014, 119, 396-400

Batista, A. D., et al. Talanta. 2015, 133, 142-9

Chavez-Moreno, C. A., et al. Analytical and bioanalytical chemistry. 2012, 403, 2705-14

Singer, H., et al. Environmental pollution. 2010, 158, 3054-64

Garcia-Ac, A., et al. Journal of chromatography. A. 2009, 1216, 8518-27

Wu, L., et al. Food Chem. 2014, 162, 253-60

Wang, H., et al. Journal of chromatography. A. 2012, 1233, 36-43

Shah, J., et al. Environmental monitoring and assessment. 2011, 178, 111-9

Wang, H.; Ding, J.; Ren, N. TrAC Trends in Analytical Chemistry. 2016, 75, 197-208

Medina, L. M.; Mackenzie, J.; Bermúdez, A. S. 1990. 1990, 19, 8

Kearns, J. P., et al. Water research. 2014, 62, 20-8

Biesaga, M.; Jankowska, A.; Pyrzy?ska, K. Microchimica Acta. 2005, 150, 317-322

Safari, M., et al. Microchimica Acta. 2015, 183, 203-210

Nollet, L. M.; Toldrá, F. Handbook of seafood and seafood products analysis. CRC Press, 2009.

Veggi, P. C.; Martinez, J.; Meireles, M. A. A., in: Microwave-assisted extraction for bioactive compounds, Springer, 2012, 15-52.

Xiong, G., et al. Talanta. 1999, 48, 333-339

Montgomery, D. C. Diseño y análisis de experimentos. Limusa Wiley, 2008.