On-line solid-phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry for the determination of avermectins and milbemycin in soils

Autor(es)

Ferreira, Fabricio de Oliveira ; Rodrigues-Silva, Caio ; Rath, Susanne

• Tipo de documento: Artigo Científico
• Fonte: Journal of Chromatography A; v. 1471, p. 118-125, NOV 4 2016.
• Citações Web of Science: 8

Resumo

Avermectins and milbemycin are widely used as veterinary drugs and as agricultural pesticides, and their residues have been detected in soil. This study reports a simple and high-throughput method for determining ivermectin (IVER), abamectin (ABA), doramectin (DORA), eprinomectin (EPRI), and moxidectin (MOXI) residues in soils, employing an on-line solid-phase extraction technique coupled with ultra-high performance liquid chromatography and tandem mass spectrometry (SPE-UHPLC-MS/MS). The method was validated and applied for the determination of ABA in soils from an orange plantation treated with this pesticide. The sample preparation procedure consisted of extraction of,the compounds from soil using methanol (with recoveries of 73-85%), and subsequent on-line SPE cleanup and concentration using a C8 sorbent coupled to the UHPLC-MS/MS system. The optimal conditions were: water:methanol (40:60, v/v) sample solvent; water:methanol (96:4, v/v) loading solvent; 2 x 250 mu L sample volume; and elution of the analytes retained on the SPE column in back flush with 5 mmol L-1 ammonium acetate:acetonitrile (10:90, v/v) chromatographic mobile phase. The method produced linear results in the ranges 0.1-10 ng g(-1) (IVER, ABA, DORA, and MOXI) and 0.5-10 ng g(-1) (EPRI), with linearity greater than 0.99. The precision of the method was better than 19% and accuracy was in the range 74-89%. The limits of quantitation were 0.2 ng g(-1) for EPRI and 0.1 ng g(-1) for the other compounds. The SPE column could be reused in more than 2000 analyses without loss of efficiency. The ABA concentration in the soil varied between 1.7 and 18 ng g(-1), and no dissipation was observed during five consecutive days after application of the pesticide to the orange plantation. (C) 2016 Elsevier B.V. All rights reserved. (AU)

• Processo FAPESP: 13/09543-7 - Resíduos de medicamentos veterinários no ambiente
• Beneficiário: Susanne Rath
• Modalidade de apoio: Auxílio à Pesquisa - Temático
• Processo FAPESP: 14/16622-3 - Identificação dos intermediários formados durante a degradação de fármacos veterinários por processos oxidativos avançados
• Beneficiário: Caio Alexandre Augusto Rodrigues da Silva
• Modalidade de apoio: Bolsas no Brasil - Pós-Doutorado
• Processo FAPESP: 13/25670-9 - Antiparasitários em solos brasileiros: estudo de sorção, dessorção e degradação
• Beneficiário: Fabricio de Oliveira Ferreira
• Modalidade de apoio: Bolsas no Brasil - Doutorado