Determination of atrazine in environmental samples (soil and water) by UHPLC-MS/MS

Atrazine is an extensively used herbicide in Argentina. It solubility in water is 30 mg/L and the average half life in underground waters is of 283 days. It moderate solubility and stability led to the findings of residues in air, soils, surface waters and underground waters. For this reason there is a great demand to determine atrazine and it degradation products at low ppt-ppb levels to satisfy environmental protection needs. This work deals with the optimization of the determination of atrazine in water and soil, by means of a rapid simple preparation procedure followed by determination using a UHPLC-MS/MS system, and its applications to measure real samples from the intensive agricultural Center Region of Argentina. Sample preparation was based on modifications of a SPE procedure described by Min et.al1. Performance aspects, mobile phases, ionization conditions and operation variables for fragmentation/detection in the triple quadrupole mass detector, in multiple reaction monitoring mode (MRM) were evaluated. Separation was done in a rapid resolution UHPLC column (C18, 2.1 mm x 100 mm, 1.7 µm), using a gradient elution of a mobile phase of water and acetonitrile, pH adjusted with 0.1% (v/v) formic acid. LOD and LOQ limits were 1 ng/L and 3 ng/L in water and 20 ng/kg and 50 ng/kg in soil matrixes respectively. Validation of methodology following SANCO/12495/2011 specifications were achieved. Matrix effects evaluation showed significant ion suppression only in soil samples. Validated methodology were applied to study field samples of soil and surface waters: a) 21 samples of agricultural experimental soils from Córdoba Province, obtained at 5, 40 and 90 cm depth previously to atrazine treatment at concentration 48%, loading 2 L/ha), sampling at 7, 15, 30, 60 y 90 days after application. b) 48 samples of surface waters, collected monthly during one year in streams across agricultural zones of Santa Fe Province (Departments of Las Colonias and San Jerónimo): Aº Santa María (31° 41? 01.63?? S/ 61°10? 04.05?? O), Aº Corrallito (31° 47? 13.44?? S /61° 18? 40?? O), Aº Colastiné two sectors: 31° 54? 36.80?? S/61° 08? 49.54?? O y 31° 01?02.15?? S/60° 59´24.97?? O, the last one in the nearby to Río Coronda.

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Bibliographic Details
Main Authors: Repetti M. R., Regaldo L., Murialdo R., Magni, F., Ruiz Moreno D., García S. R., Beldoménico H.
Format: conferenceObject biblioteca
Language:eng
Published: 2013
Subjects:Soil, Water, HPLC MS,
Online Access:http://hdl.handle.net/11086/25419
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spelling dig-unc-ar-11086-254192022-05-31T13:43:56Z Determination of atrazine in environmental samples (soil and water) by UHPLC-MS/MS Repetti M. R. Regaldo L. Murialdo R. Magni, F. Ruiz Moreno D. García S. R. Beldoménico H. Soil Water HPLC MS Atrazine is an extensively used herbicide in Argentina. It solubility in water is 30 mg/L and the average half life in underground waters is of 283 days. It moderate solubility and stability led to the findings of residues in air, soils, surface waters and underground waters. For this reason there is a great demand to determine atrazine and it degradation products at low ppt-ppb levels to satisfy environmental protection needs. This work deals with the optimization of the determination of atrazine in water and soil, by means of a rapid simple preparation procedure followed by determination using a UHPLC-MS/MS system, and its applications to measure real samples from the intensive agricultural Center Region of Argentina. Sample preparation was based on modifications of a SPE procedure described by Min et.al1. Performance aspects, mobile phases, ionization conditions and operation variables for fragmentation/detection in the triple quadrupole mass detector, in multiple reaction monitoring mode (MRM) were evaluated. Separation was done in a rapid resolution UHPLC column (C18, 2.1 mm x 100 mm, 1.7 µm), using a gradient elution of a mobile phase of water and acetonitrile, pH adjusted with 0.1% (v/v) formic acid. LOD and LOQ limits were 1 ng/L and 3 ng/L in water and 20 ng/kg and 50 ng/kg in soil matrixes respectively. Validation of methodology following SANCO/12495/2011 specifications were achieved. Matrix effects evaluation showed significant ion suppression only in soil samples. Validated methodology were applied to study field samples of soil and surface waters: a) 21 samples of agricultural experimental soils from Córdoba Province, obtained at 5, 40 and 90 cm depth previously to atrazine treatment at concentration 48%, loading 2 L/ha), sampling at 7, 15, 30, 60 y 90 days after application. b) 48 samples of surface waters, collected monthly during one year in streams across agricultural zones of Santa Fe Province (Departments of Las Colonias and San Jerónimo): Aº Santa María (31° 41? 01.63?? S/ 61°10? 04.05?? O), Aº Corrallito (31° 47? 13.44?? S /61° 18? 40?? O), Aº Colastiné two sectors: 31° 54? 36.80?? S/61° 08? 49.54?? O y 31° 01?02.15?? S/60° 59´24.97?? O, the last one in the nearby to Río Coronda. publishedVersion Fil: Repetti M. R. Universidad Nacional del Litoral. Facultad de Ingeniería Química; Argentina. Fil: Regaldo L. Universidad Nacional del Litoral. Facultad de Humanidades y Ciencias. Departamento de Ciencias Naturales; Argentina. Fil: Murialdo R. Universidad Nacional de Córdoba. Facultad de Ciencias Exactas, Físicas y Naturales; Argentina. Fil: Magni, F. Universidad Nacional del Litoral. Facultad de Ingeniería Química; Argentina. Fil: Ruiz Moreno D. Universidad Nacional del Litoral. Facultad de Ingeniería Química; Argentina. Fil: García S. R. Universidad Nacional del Litoral. Facultad de Ingeniería Química; Argentina. Fil: Beldoménico H. Universidad Nacional del Litoral. Facultad de Ingeniería Química; Argentina. Química Analítica 2022-05-30T14:17:38Z 2022-05-30T14:17:38Z 2013 conferenceObject http://hdl.handle.net/11086/25419 eng Attribution-NonCommercial-ShareAlike 4.0 International http://creativecommons.org/licenses/by-nc-sa/4.0/ Impreso
institution UNC AR
collection DSpace
country Argentina
countrycode AR
component Bibliográfico
access En linea
databasecode dig-unc-ar
tag biblioteca
region America del Sur
libraryname Biblioteca 'Ing. Agrónomo Moisés Farber' de la Facultad de Ciencias Agropecuarias
language eng
topic Soil
Water
HPLC MS
Soil
Water
HPLC MS
spellingShingle Soil
Water
HPLC MS
Soil
Water
HPLC MS
Repetti M. R.
Regaldo L.
Murialdo R.
Magni, F.
Ruiz Moreno D.
García S. R.
Beldoménico H.
Determination of atrazine in environmental samples (soil and water) by UHPLC-MS/MS
description Atrazine is an extensively used herbicide in Argentina. It solubility in water is 30 mg/L and the average half life in underground waters is of 283 days. It moderate solubility and stability led to the findings of residues in air, soils, surface waters and underground waters. For this reason there is a great demand to determine atrazine and it degradation products at low ppt-ppb levels to satisfy environmental protection needs. This work deals with the optimization of the determination of atrazine in water and soil, by means of a rapid simple preparation procedure followed by determination using a UHPLC-MS/MS system, and its applications to measure real samples from the intensive agricultural Center Region of Argentina. Sample preparation was based on modifications of a SPE procedure described by Min et.al1. Performance aspects, mobile phases, ionization conditions and operation variables for fragmentation/detection in the triple quadrupole mass detector, in multiple reaction monitoring mode (MRM) were evaluated. Separation was done in a rapid resolution UHPLC column (C18, 2.1 mm x 100 mm, 1.7 µm), using a gradient elution of a mobile phase of water and acetonitrile, pH adjusted with 0.1% (v/v) formic acid. LOD and LOQ limits were 1 ng/L and 3 ng/L in water and 20 ng/kg and 50 ng/kg in soil matrixes respectively. Validation of methodology following SANCO/12495/2011 specifications were achieved. Matrix effects evaluation showed significant ion suppression only in soil samples. Validated methodology were applied to study field samples of soil and surface waters: a) 21 samples of agricultural experimental soils from Córdoba Province, obtained at 5, 40 and 90 cm depth previously to atrazine treatment at concentration 48%, loading 2 L/ha), sampling at 7, 15, 30, 60 y 90 days after application. b) 48 samples of surface waters, collected monthly during one year in streams across agricultural zones of Santa Fe Province (Departments of Las Colonias and San Jerónimo): Aº Santa María (31° 41? 01.63?? S/ 61°10? 04.05?? O), Aº Corrallito (31° 47? 13.44?? S /61° 18? 40?? O), Aº Colastiné two sectors: 31° 54? 36.80?? S/61° 08? 49.54?? O y 31° 01?02.15?? S/60° 59´24.97?? O, the last one in the nearby to Río Coronda.
format conferenceObject
topic_facet Soil
Water
HPLC MS
author Repetti M. R.
Regaldo L.
Murialdo R.
Magni, F.
Ruiz Moreno D.
García S. R.
Beldoménico H.
author_facet Repetti M. R.
Regaldo L.
Murialdo R.
Magni, F.
Ruiz Moreno D.
García S. R.
Beldoménico H.
author_sort Repetti M. R.
title Determination of atrazine in environmental samples (soil and water) by UHPLC-MS/MS
title_short Determination of atrazine in environmental samples (soil and water) by UHPLC-MS/MS
title_full Determination of atrazine in environmental samples (soil and water) by UHPLC-MS/MS
title_fullStr Determination of atrazine in environmental samples (soil and water) by UHPLC-MS/MS
title_full_unstemmed Determination of atrazine in environmental samples (soil and water) by UHPLC-MS/MS
title_sort determination of atrazine in environmental samples (soil and water) by uhplc-ms/ms
publishDate 2013
url http://hdl.handle.net/11086/25419
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