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Determination of pesticides in sewage sludge from an agro-food industry using QuEChERS extraction followed by analysis with liquid chromatography-tandem mass spectrometry.
Anal Bioanal Chem. 2017 Oct; 409(26):6181-6193.AB

Abstract

An analytical method was developed and validated for the determination of ten pesticides in sewage sludge coming from an agro-food industry. The method was based on the application of Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction for solid sewage sludge and SPE extraction for sludge aqueous phase, followed by liquid chromatography (LC) coupled to hybrid quadrupole/linear ion trap mass spectrometry (QqLIT-MS). The QuEChERS method was reported 14 years ago and nowadays is mainly applied to the analysis of pesticides in food. More recent applications have been reported in other matrices as sewage sludge, but the complexity of the matrix makes necessary the optimization of the cleanup step to improve the efficiency of the analysis. With this aim, several dispersive solid-phase extraction cleanup sorbents were tested, choosing C18 + PSA as a d-SPE sorbent. The proposed method was satisfactorily validated for most compounds investigated, showing recoveries higher than 80% in most cases, with the only exception of prochloraz (71%) at low concentration level. Limits of quantification were lower than 40 ng l-1 in the aqueous phase and below 40 ng g-1 in the solid phase for the majority of the analytes. The method was applied to solid sludge and the sludge aqueous phase coming from an agro-food industry which processes fruits and vegetables. Graphical abstract Application of LC/MS/MS advanced analytical techniques for determination of pesticides contained in sewage sludge.

Authors+Show Affiliations

Plataforma Solar de Almería-CIEMAT, Carretera de Senés Km4, 04200, Tabernas, Almería, Spain. CIESOL, Joint Centre of the University of Almería-CIEMAT, Carretera de Sacramento s/n, 04120, La Cañada de San Urbano, Almería, Spain.CIESOL, Joint Centre of the University of Almería-CIEMAT, Carretera de Sacramento s/n, 04120, La Cañada de San Urbano, Almería, Spain.CIESOL, Joint Centre of the University of Almería-CIEMAT, Carretera de Sacramento s/n, 04120, La Cañada de San Urbano, Almería, Spain.Plataforma Solar de Almería-CIEMAT, Carretera de Senés Km4, 04200, Tabernas, Almería, Spain. CIESOL, Joint Centre of the University of Almería-CIEMAT, Carretera de Sacramento s/n, 04120, La Cañada de San Urbano, Almería, Spain.Plataforma Solar de Almería-CIEMAT, Carretera de Senés Km4, 04200, Tabernas, Almería, Spain. CIESOL, Joint Centre of the University of Almería-CIEMAT, Carretera de Sacramento s/n, 04120, La Cañada de San Urbano, Almería, Spain.CIESOL, Joint Centre of the University of Almería-CIEMAT, Carretera de Sacramento s/n, 04120, La Cañada de San Urbano, Almería, Spain. aaguera@ual.es.

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

28840278

Citation

Ponce-Robles, Laura, et al. "Determination of Pesticides in Sewage Sludge From an Agro-food Industry Using QuEChERS Extraction Followed By Analysis With Liquid Chromatography-tandem Mass Spectrometry." Analytical and Bioanalytical Chemistry, vol. 409, no. 26, 2017, pp. 6181-6193.
Ponce-Robles L, Rivas G, Esteban B, et al. Determination of pesticides in sewage sludge from an agro-food industry using QuEChERS extraction followed by analysis with liquid chromatography-tandem mass spectrometry. Anal Bioanal Chem. 2017;409(26):6181-6193.
Ponce-Robles, L., Rivas, G., Esteban, B., Oller, I., Malato, S., & Agüera, A. (2017). Determination of pesticides in sewage sludge from an agro-food industry using QuEChERS extraction followed by analysis with liquid chromatography-tandem mass spectrometry. Analytical and Bioanalytical Chemistry, 409(26), 6181-6193. https://doi.org/10.1007/s00216-017-0558-5
Ponce-Robles L, et al. Determination of Pesticides in Sewage Sludge From an Agro-food Industry Using QuEChERS Extraction Followed By Analysis With Liquid Chromatography-tandem Mass Spectrometry. Anal Bioanal Chem. 2017;409(26):6181-6193. PubMed PMID: 28840278.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of pesticides in sewage sludge from an agro-food industry using QuEChERS extraction followed by analysis with liquid chromatography-tandem mass spectrometry. AU - Ponce-Robles,Laura, AU - Rivas,Gracia, AU - Esteban,Belen, AU - Oller,Isabel, AU - Malato,Sixto, AU - Agüera,Ana, Y1 - 2017/08/24/ PY - 2017/06/13/received PY - 2017/07/31/accepted PY - 2017/07/13/revised PY - 2017/8/26/pubmed PY - 2018/5/1/medline PY - 2017/8/26/entrez KW - Agro-food industry KW - Industrial wastewater KW - LC-MS KW - Pesticides KW - QuEChERS KW - Sludge SP - 6181 EP - 6193 JF - Analytical and bioanalytical chemistry JO - Anal Bioanal Chem VL - 409 IS - 26 N2 - An analytical method was developed and validated for the determination of ten pesticides in sewage sludge coming from an agro-food industry. The method was based on the application of Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction for solid sewage sludge and SPE extraction for sludge aqueous phase, followed by liquid chromatography (LC) coupled to hybrid quadrupole/linear ion trap mass spectrometry (QqLIT-MS). The QuEChERS method was reported 14 years ago and nowadays is mainly applied to the analysis of pesticides in food. More recent applications have been reported in other matrices as sewage sludge, but the complexity of the matrix makes necessary the optimization of the cleanup step to improve the efficiency of the analysis. With this aim, several dispersive solid-phase extraction cleanup sorbents were tested, choosing C18 + PSA as a d-SPE sorbent. The proposed method was satisfactorily validated for most compounds investigated, showing recoveries higher than 80% in most cases, with the only exception of prochloraz (71%) at low concentration level. Limits of quantification were lower than 40 ng l-1 in the aqueous phase and below 40 ng g-1 in the solid phase for the majority of the analytes. The method was applied to solid sludge and the sludge aqueous phase coming from an agro-food industry which processes fruits and vegetables. Graphical abstract Application of LC/MS/MS advanced analytical techniques for determination of pesticides contained in sewage sludge. SN - 1618-2650 UR - https://www.unboundmedicine.com/medline/citation/28840278/Determination_of_pesticides_in_sewage_sludge_from_an_agro_food_industry_using_QuEChERS_extraction_followed_by_analysis_with_liquid_chromatography_tandem_mass_spectrometry_ L2 - https://dx.doi.org/10.1007/s00216-017-0558-5 DB - PRIME DP - Unbound Medicine ER -