Atrazine and 2, 4-D Determination in Corn Samples Using Microwave Assisted Extraction and On-line Solid-phase Extraction Coupled to Liquid Chromatography
Abstract: In this study, on-line sample pretreatment (clean-up and analyte preconcentration) using sequential injection analysis was coupled to high performance liquid chromatography with UV detection (HPLC/UV) for the determination of 2,4-D (2,4-dichlorophenoxyacetic acid) and atrazine in corn samples. Prior to their analysis, microwave-assisted extraction approach for 2,4-D and atrazine in corn samples was carried out using MeOH: H2O (30:70 v/v) solvent at 50°C for 20 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 ACN: 10 mM CH3COOH/CH3COONa buffer at pH 4 (20:80, v/v) was employed as mobile phase at 2 mL min-1 flow rate for chromatographic 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 concentration level of 0.07 and 0.30 mg kg-1. The extraction recoveries of 2,4-D and atrazine in corn samples were from 82.6 to 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, and thus minimizing risks of sample contamination and analyte losses.
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Sociedad Química de México A.C.
2018
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oai:scielo:S1870-249X20180002002822019-03-26Atrazine and 2, 4-D Determination in Corn Samples Using Microwave Assisted Extraction and On-line Solid-phase Extraction Coupled to Liquid ChromatographySantos-Hernández,Ana SusanaHinojosa-Reyes,LauraSáenz-Tavera,Isabel del CarmenHernández-Ramírez,AracelyGuzmán-Mar,Jorge Luis herbicide corn microwave assisted extraction on-line SPE-HPLC/UV Abstract: In this study, on-line sample pretreatment (clean-up and analyte preconcentration) using sequential injection analysis was coupled to high performance liquid chromatography with UV detection (HPLC/UV) for the determination of 2,4-D (2,4-dichlorophenoxyacetic acid) and atrazine in corn samples. Prior to their analysis, microwave-assisted extraction approach for 2,4-D and atrazine in corn samples was carried out using MeOH: H2O (30:70 v/v) solvent at 50°C for 20 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 ACN: 10 mM CH3COOH/CH3COONa buffer at pH 4 (20:80, v/v) was employed as mobile phase at 2 mL min-1 flow rate for chromatographic 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 concentration level of 0.07 and 0.30 mg kg-1. The extraction recoveries of 2,4-D and atrazine in corn samples were from 82.6 to 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, and thus minimizing risks of sample contamination and analyte losses.info:eu-repo/semantics/openAccessSociedad Química de México A.C.Journal of the Mexican Chemical Society v.62 n.2 20182018-06-01info:eu-repo/semantics/articletext/htmlhttp://www.scielo.org.mx/scielo.php?script=sci_arttext&pid=S1870-249X2018000200282en10.29356/jmcs.v62i2.475 |
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Santos-Hernández,Ana Susana Hinojosa-Reyes,Laura Sáenz-Tavera,Isabel del Carmen Hernández-Ramírez,Aracely Guzmán-Mar,Jorge Luis |
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Santos-Hernández,Ana Susana Hinojosa-Reyes,Laura Sáenz-Tavera,Isabel del Carmen Hernández-Ramírez,Aracely Guzmán-Mar,Jorge Luis Atrazine and 2, 4-D Determination in Corn Samples Using Microwave Assisted Extraction and On-line Solid-phase Extraction Coupled to Liquid Chromatography |
author_facet |
Santos-Hernández,Ana Susana Hinojosa-Reyes,Laura Sáenz-Tavera,Isabel del Carmen Hernández-Ramírez,Aracely Guzmán-Mar,Jorge Luis |
author_sort |
Santos-Hernández,Ana Susana |
title |
Atrazine and 2, 4-D Determination in Corn Samples Using Microwave Assisted Extraction and On-line Solid-phase Extraction Coupled to Liquid Chromatography |
title_short |
Atrazine and 2, 4-D Determination in Corn Samples Using Microwave Assisted Extraction and On-line Solid-phase Extraction Coupled to Liquid Chromatography |
title_full |
Atrazine and 2, 4-D Determination in Corn Samples Using Microwave Assisted Extraction and On-line Solid-phase Extraction Coupled to Liquid Chromatography |
title_fullStr |
Atrazine and 2, 4-D Determination in Corn Samples Using Microwave Assisted Extraction and On-line Solid-phase Extraction Coupled to Liquid Chromatography |
title_full_unstemmed |
Atrazine and 2, 4-D Determination in Corn Samples Using Microwave Assisted Extraction and On-line Solid-phase Extraction Coupled to Liquid Chromatography |
title_sort |
atrazine and 2, 4-d determination in corn samples using microwave assisted extraction and on-line solid-phase extraction coupled to liquid chromatography |
description |
Abstract: In this study, on-line sample pretreatment (clean-up and analyte preconcentration) using sequential injection analysis was coupled to high performance liquid chromatography with UV detection (HPLC/UV) for the determination of 2,4-D (2,4-dichlorophenoxyacetic acid) and atrazine in corn samples. Prior to their analysis, microwave-assisted extraction approach for 2,4-D and atrazine in corn samples was carried out using MeOH: H2O (30:70 v/v) solvent at 50°C for 20 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 ACN: 10 mM CH3COOH/CH3COONa buffer at pH 4 (20:80, v/v) was employed as mobile phase at 2 mL min-1 flow rate for chromatographic 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 concentration level of 0.07 and 0.30 mg kg-1. The extraction recoveries of 2,4-D and atrazine in corn samples were from 82.6 to 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, and thus minimizing risks of sample contamination and analyte losses. |
publisher |
Sociedad Química de México A.C. |
publishDate |
2018 |
url |
http://www.scielo.org.mx/scielo.php?script=sci_arttext&pid=S1870-249X2018000200282 |
work_keys_str_mv |
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