title: A single-step pesticide extraction and clean-up multi-residue analytical method by selective pressurized liquid extraction followed by on-line solid phase extraction and ultra-high-performance liquid chromatography-tandem mass spectrometry for complex matrices.
abstract: Pesticides, a group of compounds linked to human activity, may, when in toxic levels, have a profound effect on water quality, and hence result in adverse consequences to aquatic life and ultimately to human health. Analytical challenges arise when successfully trying to determine these levels in environmental complex matrices. Therefore, fast, simple, sensitive and selective analytical methodologies for multi-residue determination of pesticides (atrazine, azoxystrobin, bentazon, λ-cyhalothrin, penoxsulam and terbuthylazine) in sediment, macrophytes (algae and aquatic plants) and aquatic animals were developed and validated. The established methods were matrix-dependent and were based on Selective Pressurized Liquid Extraction (SPLE) followed by on-line Solid Phase Extraction and Ultra Performance Liquid Chromatography-tandem Mass Spectrometry (on-line SPE-UPLC-ESI-MS/MS). This cutting-edge research methodology uses a small amount of sample, is time saving and reduces the use of organic solvents in compliance with Green Chemistry principles. The analytical features were adequate for all compounds in all studied matrices. The established methodology was applied on real marine samples and no pesticide concentrations above their respective method quantification limits were measured in sediments or aquatic plants. However, terbuthylazine was found in the macroalgae Ulva spp. (108ngg(-1)dw) and all the prospected pesticides were measured above their respective method quantification limits in the bivalve Scrobicularia plana (atrazine: 48ngg(-1)dw, azoxystrobin: 64ngg(-1)dw, bentazon: 33ngg(-1)dw, λ-cyhalothrin: 2531ngg(-1)dw, penoxsulam: 50ngg(-1)dw, and terbuthylazine: 44ngg(-1)dw).
authors.affiliation: CFE-Centre for Functional Ecology, Department of Life Sciences, University of Coimbra, Calçada Martim de Freitas, 3000-456 Coimbra, Portugal. Electronic address: etrodrig@zoo.uc.pt.
authors.forename: Elsa Teresa
authors.initials: ET
authors.lastname: Rodrigues
authors.affiliation: CFE-Centre for Functional Ecology, Department of Life Sciences, University of Coimbra, Calçada Martim de Freitas, 3000-456 Coimbra, Portugal. Electronic address: mpardal@zoo.uc.pt.
authors.forename: Miguel Ângelo
authors.initials: MÂ
authors.lastname: Pardal
authors.affiliation: QANAP-Grupo Química Analítica Aplicada, Instituto Universitario de Medio Ambiente (IUMA), Centro de Investigaciones Científicas Avanzadas (CICA), Departamento de Química Analítica, Facultade de Ciencias, Universidade da Coruña, Campus de A Coruña, E-15071 A Coruña, Spain. Electronic address: n.salgueiro@udc.es.
authors.forename: Noelia
authors.initials: N
authors.lastname: Salgueiro-González
authors.affiliation: QANAP-Grupo Química Analítica Aplicada, Instituto Universitario de Medio Ambiente (IUMA), Centro de Investigaciones Científicas Avanzadas (CICA), Departamento de Química Analítica, Facultade de Ciencias, Universidade da Coruña, Campus de A Coruña, E-15071 A Coruña, Spain. Electronic address: smuniat@udc.es.
authors.forename: Soledad
authors.initials: S
authors.lastname: Muniategui-Lorenzo
authors.affiliation: IAREN-Water Institute of the Northern Region, Rua Dr. Eduardo Torres 229, 4450-113 Matosinhos, Portugal. Electronic address: mfalpendurada@iaren.pt.
authors.forename: Maria Fátima
authors.initials: MF
authors.lastname: Alpendurada
mesh_terms: D000818:Animals; D059001:Aquatic Organisms / Q000737:chemistry; D049872:Bivalvia / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid; D019015:Geologic Sediments / Q000737:chemistry; D055772:Green Chemistry Technology; D010573:Pesticide Residues / Q000302:isolation & purification*; D010944:Plants / Q000737:chemistry; D011312:Pressure; D052616:Solid Phase Extraction / Q000379:methods*; D012997:Solvents / Q000737:chemistry; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013997:Time Factors; D044445:Ulva / Q000737:chemistry
chemical_list: D010573:Pesticide Residues; D012997:Solvents
keywords: Environmental samples; Green chemistry; Marine complex matrices; On-line SPE-UPLC-ESI–MS/MS; Pesticides; Selective pressurized liquid extraction