Multiresidue method for trace pesticide analysis in honeybee wax comb by GC-QqQ-MS
- Autores
- Gil García, M.D.; Uclés, Samanta; Lozano Fernández, A.B.; Sosa, Alexis Lionel; Rodríguez Fernández-Alba, Amadeo
- Año de publicación
- 2017
- Idioma
- inglés
- Tipo de recurso
- artículo
- Estado
- versión publicada
- Descripción
- The aim of this analytical study is to develop an improved multi-residue methodology of high sensitivity and expanded scope for pesticide residue analysis in honeybee wax combs. The method was validated for 160 pesticide residues (including acaricides, insecticides, fungicides and herbicides) gas chromatography amenable and covering a wide variety of polarity and chemical structure. This method of analysis applied gas chromatography coupled to a triple quadrupole mass spectrometer for the quantitative analysis of pesticide residues. The extraction procedure applied was based QuEChERs method allowing acceptable recoveries for most of the pesticides (98%), within the range 60–120% with an associated precision (RSD) <20%, at concentration levels of MQL of 10 µg kg−1 for all pesticides with the exception of 3,5-dichloroaniline and chlordane (20 µg kg−1). The expanded uncertainty of the results was ±35% on average (coverage factor k=2 for a confidence level of 95%). The chromatographic multi-residue method was applied to determine levels of pesticide residues in 50 honeybee wax comb samples randomly collected from different apiaries in Spain. A total of 32 pesticide residues (14 insecticides/acaricides, 10 insecticides, 6 fungicides and 2 herbicides) were detected in the samples. The highest pesticide concentrations were found for those with insecticide-acaricide activity like acrinathrin, chlorfenvinphos, coumaphos and fluvalinate-tau, some of them are mainly applied in apiculture for controlling the honeybee parasite Varroa destructor. The total load of pesticide residues ranged from 69 to 1000 µg kg−1 for 40% of the analysed samples, 22% contained pesticide residues in the ranges of 1000–2000 µg kg−1, 24% between 2000 and 5000 µg kg−1 and 14% of the samples contained residues between 5000 and 9557 µg kg−1.
EEA Concordia
Fil: Gil García, M.D. Universidad de Almería. Departamento de Química y Física. Campus de Excelencia Internacional en Agroalimentación; España. European Union Reference Laboratory for Pesticide Residues in Fruit and Vegetables; España
Fil: Uclés, Samanta. Universidad de Almería. Departamento de Química y Física. Campus de Excelencia Internacional en Agroalimentación; España. European Union Reference Laboratory for Pesticide Residues in Fruit and Vegetables; España
Fil: Lozano Fernández, A.B. Universidad de Almería. Departamento de Química y Física. Campus de Excelencia Internacional en Agroalimentación; España. European Union Reference Laboratory for Pesticide Residues in Fruit and Vegetables; España
Fil: Sosa, Alexis Lionel. Instituto Nacional de Tecnología Agropecuaria (INTA). Estación Experimental Agropecuaria Concordia; Argentina
Fil: Rodríguez Fernández-Alba, Amadeo. Universidad de Almería. Departamento de Química y Física. Campus de Excelencia Internacional en Agroalimentación; España. European Union Reference Laboratory for Pesticide Residues in Fruit and Vegetables; España - Fuente
- Talanta 163 : 54-64 (January 2017)
- Materia
-
Abeja Melífera
Ceras
Residuos de Plaguicidas
Espectrometría de Masas
Honey Bees
Waxes
Pesticide Residues
Mass Spectrometry - Nivel de accesibilidad
- acceso restringido
- Condiciones de uso
- Repositorio
- Institución
- Instituto Nacional de Tecnología Agropecuaria
- OAI Identificador
- oai:localhost:20.500.12123/2890
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Multiresidue method for trace pesticide analysis in honeybee wax comb by GC-QqQ-MSGil García, M.D.Uclés, SamantaLozano Fernández, A.B.Sosa, Alexis LionelRodríguez Fernández-Alba, AmadeoAbeja MelíferaCerasResiduos de PlaguicidasEspectrometría de MasasHoney BeesWaxesPesticide ResiduesMass SpectrometryThe aim of this analytical study is to develop an improved multi-residue methodology of high sensitivity and expanded scope for pesticide residue analysis in honeybee wax combs. The method was validated for 160 pesticide residues (including acaricides, insecticides, fungicides and herbicides) gas chromatography amenable and covering a wide variety of polarity and chemical structure. This method of analysis applied gas chromatography coupled to a triple quadrupole mass spectrometer for the quantitative analysis of pesticide residues. The extraction procedure applied was based QuEChERs method allowing acceptable recoveries for most of the pesticides (98%), within the range 60–120% with an associated precision (RSD) <20%, at concentration levels of MQL of 10 µg kg−1 for all pesticides with the exception of 3,5-dichloroaniline and chlordane (20 µg kg−1). The expanded uncertainty of the results was ±35% on average (coverage factor k=2 for a confidence level of 95%). The chromatographic multi-residue method was applied to determine levels of pesticide residues in 50 honeybee wax comb samples randomly collected from different apiaries in Spain. A total of 32 pesticide residues (14 insecticides/acaricides, 10 insecticides, 6 fungicides and 2 herbicides) were detected in the samples. The highest pesticide concentrations were found for those with insecticide-acaricide activity like acrinathrin, chlorfenvinphos, coumaphos and fluvalinate-tau, some of them are mainly applied in apiculture for controlling the honeybee parasite Varroa destructor. The total load of pesticide residues ranged from 69 to 1000 µg kg−1 for 40% of the analysed samples, 22% contained pesticide residues in the ranges of 1000–2000 µg kg−1, 24% between 2000 and 5000 µg kg−1 and 14% of the samples contained residues between 5000 and 9557 µg kg−1.EEA ConcordiaFil: Gil García, M.D. Universidad de Almería. Departamento de Química y Física. Campus de Excelencia Internacional en Agroalimentación; España. European Union Reference Laboratory for Pesticide Residues in Fruit and Vegetables; EspañaFil: Uclés, Samanta. Universidad de Almería. Departamento de Química y Física. Campus de Excelencia Internacional en Agroalimentación; España. European Union Reference Laboratory for Pesticide Residues in Fruit and Vegetables; EspañaFil: Lozano Fernández, A.B. Universidad de Almería. Departamento de Química y Física. Campus de Excelencia Internacional en Agroalimentación; España. European Union Reference Laboratory for Pesticide Residues in Fruit and Vegetables; EspañaFil: Sosa, Alexis Lionel. Instituto Nacional de Tecnología Agropecuaria (INTA). Estación Experimental Agropecuaria Concordia; ArgentinaFil: Rodríguez Fernández-Alba, Amadeo. Universidad de Almería. Departamento de Química y Física. Campus de Excelencia Internacional en Agroalimentación; España. European Union Reference Laboratory for Pesticide Residues in Fruit and Vegetables; España2018-07-26T15:56:16Z2018-07-26T15:56:16Z2017-01-15info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfhttps://www.sciencedirect.com/science/article/pii/S0039914016308384?via%3Dihubhttp://hdl.handle.net/20.500.12123/28900039-9140https://doi.org/10.1016/j.talanta.2016.10.083Talanta 163 : 54-64 (January 2017)reponame:INTA Digital (INTA)instname:Instituto Nacional de Tecnología Agropecuariaenginfo:eu-repo/semantics/restrictedAccess2025-09-04T09:47:22Zoai:localhost:20.500.12123/2890instacron:INTAInstitucionalhttp://repositorio.inta.gob.ar/Organismo científico-tecnológicoNo correspondehttp://repositorio.inta.gob.ar/oai/requesttripaldi.nicolas@inta.gob.arArgentinaNo correspondeNo correspondeNo correspondeopendoar:l2025-09-04 09:47:23.181INTA Digital (INTA) - Instituto Nacional de Tecnología Agropecuariafalse |
dc.title.none.fl_str_mv |
Multiresidue method for trace pesticide analysis in honeybee wax comb by GC-QqQ-MS |
title |
Multiresidue method for trace pesticide analysis in honeybee wax comb by GC-QqQ-MS |
spellingShingle |
Multiresidue method for trace pesticide analysis in honeybee wax comb by GC-QqQ-MS Gil García, M.D. Abeja Melífera Ceras Residuos de Plaguicidas Espectrometría de Masas Honey Bees Waxes Pesticide Residues Mass Spectrometry |
title_short |
Multiresidue method for trace pesticide analysis in honeybee wax comb by GC-QqQ-MS |
title_full |
Multiresidue method for trace pesticide analysis in honeybee wax comb by GC-QqQ-MS |
title_fullStr |
Multiresidue method for trace pesticide analysis in honeybee wax comb by GC-QqQ-MS |
title_full_unstemmed |
Multiresidue method for trace pesticide analysis in honeybee wax comb by GC-QqQ-MS |
title_sort |
Multiresidue method for trace pesticide analysis in honeybee wax comb by GC-QqQ-MS |
dc.creator.none.fl_str_mv |
Gil García, M.D. Uclés, Samanta Lozano Fernández, A.B. Sosa, Alexis Lionel Rodríguez Fernández-Alba, Amadeo |
author |
Gil García, M.D. |
author_facet |
Gil García, M.D. Uclés, Samanta Lozano Fernández, A.B. Sosa, Alexis Lionel Rodríguez Fernández-Alba, Amadeo |
author_role |
author |
author2 |
Uclés, Samanta Lozano Fernández, A.B. Sosa, Alexis Lionel Rodríguez Fernández-Alba, Amadeo |
author2_role |
author author author author |
dc.subject.none.fl_str_mv |
Abeja Melífera Ceras Residuos de Plaguicidas Espectrometría de Masas Honey Bees Waxes Pesticide Residues Mass Spectrometry |
topic |
Abeja Melífera Ceras Residuos de Plaguicidas Espectrometría de Masas Honey Bees Waxes Pesticide Residues Mass Spectrometry |
dc.description.none.fl_txt_mv |
The aim of this analytical study is to develop an improved multi-residue methodology of high sensitivity and expanded scope for pesticide residue analysis in honeybee wax combs. The method was validated for 160 pesticide residues (including acaricides, insecticides, fungicides and herbicides) gas chromatography amenable and covering a wide variety of polarity and chemical structure. This method of analysis applied gas chromatography coupled to a triple quadrupole mass spectrometer for the quantitative analysis of pesticide residues. The extraction procedure applied was based QuEChERs method allowing acceptable recoveries for most of the pesticides (98%), within the range 60–120% with an associated precision (RSD) <20%, at concentration levels of MQL of 10 µg kg−1 for all pesticides with the exception of 3,5-dichloroaniline and chlordane (20 µg kg−1). The expanded uncertainty of the results was ±35% on average (coverage factor k=2 for a confidence level of 95%). The chromatographic multi-residue method was applied to determine levels of pesticide residues in 50 honeybee wax comb samples randomly collected from different apiaries in Spain. A total of 32 pesticide residues (14 insecticides/acaricides, 10 insecticides, 6 fungicides and 2 herbicides) were detected in the samples. The highest pesticide concentrations were found for those with insecticide-acaricide activity like acrinathrin, chlorfenvinphos, coumaphos and fluvalinate-tau, some of them are mainly applied in apiculture for controlling the honeybee parasite Varroa destructor. The total load of pesticide residues ranged from 69 to 1000 µg kg−1 for 40% of the analysed samples, 22% contained pesticide residues in the ranges of 1000–2000 µg kg−1, 24% between 2000 and 5000 µg kg−1 and 14% of the samples contained residues between 5000 and 9557 µg kg−1. EEA Concordia Fil: Gil García, M.D. Universidad de Almería. Departamento de Química y Física. Campus de Excelencia Internacional en Agroalimentación; España. European Union Reference Laboratory for Pesticide Residues in Fruit and Vegetables; España Fil: Uclés, Samanta. Universidad de Almería. Departamento de Química y Física. Campus de Excelencia Internacional en Agroalimentación; España. European Union Reference Laboratory for Pesticide Residues in Fruit and Vegetables; España Fil: Lozano Fernández, A.B. Universidad de Almería. Departamento de Química y Física. Campus de Excelencia Internacional en Agroalimentación; España. European Union Reference Laboratory for Pesticide Residues in Fruit and Vegetables; España Fil: Sosa, Alexis Lionel. Instituto Nacional de Tecnología Agropecuaria (INTA). Estación Experimental Agropecuaria Concordia; Argentina Fil: Rodríguez Fernández-Alba, Amadeo. Universidad de Almería. Departamento de Química y Física. Campus de Excelencia Internacional en Agroalimentación; España. European Union Reference Laboratory for Pesticide Residues in Fruit and Vegetables; España |
description |
The aim of this analytical study is to develop an improved multi-residue methodology of high sensitivity and expanded scope for pesticide residue analysis in honeybee wax combs. The method was validated for 160 pesticide residues (including acaricides, insecticides, fungicides and herbicides) gas chromatography amenable and covering a wide variety of polarity and chemical structure. This method of analysis applied gas chromatography coupled to a triple quadrupole mass spectrometer for the quantitative analysis of pesticide residues. The extraction procedure applied was based QuEChERs method allowing acceptable recoveries for most of the pesticides (98%), within the range 60–120% with an associated precision (RSD) <20%, at concentration levels of MQL of 10 µg kg−1 for all pesticides with the exception of 3,5-dichloroaniline and chlordane (20 µg kg−1). The expanded uncertainty of the results was ±35% on average (coverage factor k=2 for a confidence level of 95%). The chromatographic multi-residue method was applied to determine levels of pesticide residues in 50 honeybee wax comb samples randomly collected from different apiaries in Spain. A total of 32 pesticide residues (14 insecticides/acaricides, 10 insecticides, 6 fungicides and 2 herbicides) were detected in the samples. The highest pesticide concentrations were found for those with insecticide-acaricide activity like acrinathrin, chlorfenvinphos, coumaphos and fluvalinate-tau, some of them are mainly applied in apiculture for controlling the honeybee parasite Varroa destructor. The total load of pesticide residues ranged from 69 to 1000 µg kg−1 for 40% of the analysed samples, 22% contained pesticide residues in the ranges of 1000–2000 µg kg−1, 24% between 2000 and 5000 µg kg−1 and 14% of the samples contained residues between 5000 and 9557 µg kg−1. |
publishDate |
2017 |
dc.date.none.fl_str_mv |
2017-01-15 2018-07-26T15:56:16Z 2018-07-26T15:56:16Z |
dc.type.none.fl_str_mv |
info:eu-repo/semantics/article info:eu-repo/semantics/publishedVersion http://purl.org/coar/resource_type/c_6501 info:ar-repo/semantics/articulo |
format |
article |
status_str |
publishedVersion |
dc.identifier.none.fl_str_mv |
https://www.sciencedirect.com/science/article/pii/S0039914016308384?via%3Dihub http://hdl.handle.net/20.500.12123/2890 0039-9140 https://doi.org/10.1016/j.talanta.2016.10.083 |
url |
https://www.sciencedirect.com/science/article/pii/S0039914016308384?via%3Dihub http://hdl.handle.net/20.500.12123/2890 https://doi.org/10.1016/j.talanta.2016.10.083 |
identifier_str_mv |
0039-9140 |
dc.language.none.fl_str_mv |
eng |
language |
eng |
dc.rights.none.fl_str_mv |
info:eu-repo/semantics/restrictedAccess |
eu_rights_str_mv |
restrictedAccess |
dc.format.none.fl_str_mv |
application/pdf |
dc.source.none.fl_str_mv |
Talanta 163 : 54-64 (January 2017) reponame:INTA Digital (INTA) instname:Instituto Nacional de Tecnología Agropecuaria |
reponame_str |
INTA Digital (INTA) |
collection |
INTA Digital (INTA) |
instname_str |
Instituto Nacional de Tecnología Agropecuaria |
repository.name.fl_str_mv |
INTA Digital (INTA) - Instituto Nacional de Tecnología Agropecuaria |
repository.mail.fl_str_mv |
tripaldi.nicolas@inta.gob.ar |
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12.623145 |