Dispersive liquid-liquid microextraction (DLLME) combined with gas chromatography and mass spectrometry (GC-MS) was applied to the determination of five organophosphorous pesticides (OPPs) in water samples. The analytes included in this study were prophos, diazinon, chlorpyrifos methyl, fenchlorphos, and chlorpyrifos. The use of nonhalogenated solvents (cyclohexane, heptane, and octane) as extraction solvents was investigated using acetone, acetonitrile, or methanol, as dispersion solvents. The combination of less polar dispersion solvents (1-propanol and 2-propanol) and nonhalogenated extraction solvents was also studied in dispersive liquid-liquid microextraction for the first time. Several experimental conditions were tested (nature and volume of extraction solvents, nature and volume of dispersion solvents, salting-out effect) and the corresponding enrichment factors and recoveries were evaluated. The best microextraction condition was obtained using 50 μL of cyclohexane and 0.3 mL of 1-propanol. The detection and quantification limits were in the low ppt range, with values between 3.3-8.0 ng/L and 11.0-26.6 ng/L, respectively. Relative standard deviations were between 6.6 and 13.1% for a fortification level of 500 ng/L. At the same fortification level, the relative recoveries (RR) of Alvito's dam water, Judeu's river water, and well water samples were in the range of 50.3-97.1%.
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http://dx.doi.org/10.1002/jssc.201200241 | DOI Listing |
J Environ Health Sci Eng
June 2025
Department of Environmental Health Engineering, School of Health, Isfahan University of Medical Sciences, Isfahan, Iran.
In the present study, two most commonly used Perfluoroalkyl substances (PFASs), namely perfluorooctanoic acid (PFOA) and perfluorooctanesulfonate (PFOS), were determined in 45 tap water samples from the city of Isfahan (Iran) by dispersive liquid-liquid extraction (DLLME) and liquid chromatography-mass spectrophotometry (LC-MS) analysis. Risk assessment was also performed to determine the risk to human health. The mean concentration of PFOA was 38.
View Article and Find Full Text PDFTalanta
December 2024
Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, Regional Campus of International Excellence "Campus Mare Nostrum", E-30100, Murcia, Spain.
A reliable and sensitive analytical platform is proposed for the assessment of pig exposure to mycotoxins through the consumption of commercial feed. A total of 48 naturally contaminated feed and 55 urine samples collected from eight Spanish farms were analyzed using a fast and simple methodology based on solid-liquid extraction (SLE) or liquid-liquid extraction (LLE) and dispersive liquid-liquid microextraction (DLLME). High-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) was used for the targeted analysis of 27 mycotoxins from different families in both matrices achieving limits of quantification in a range of 0.
View Article and Find Full Text PDFMar Pollut Bull
December 2024
Universidade Federal de Pernambuco, Departamento de Química Fundamental, Av. Jornalista Aníbal Fernandes, s/n, Cidade Universitária, 50740-560 Recife, PE, Brazil. Electronic address:
In August 2019, Brazil experienced its largest large oil spill, which impacted extensive areas and significantly affected the northeastern region, particularly Pernambuco. Polycyclic aromatic hydrocarbons (PAHs), major oil components, are critical for assessing fish contamination risks. This study presents two sample pretreatment methods for fish samples - ultrasound-enhanced air-assisted liquid-liquid microextraction (UE-AA-LLME) for low molar mass PAHs, and matrix solid-phase dispersion for high molar mass PAHs - followed by a Gas-Chromatography coupled to Mass Spectrometry (GC-MS) detection.
View Article and Find Full Text PDFChemosphere
December 2024
Department of Environmental Chemistry, Institute of Environmental Assessment and Water Research, 08034 Barcelona, Spain. Electronic address:
The assessment of persistence of organic pollutants in seawater is limited by the lack of user-friendly, quick protocols for assessing one of their main sinks, degradation by marine bacteria. Here we present an experimental workflow to identify organic pollutants degradation, taking organophosphate esters flame retardants and plasticizers (OPEs-FR-PL), as a model family of synthetic chemicals released into the marine environment that are particularly widespread due to their persistence and semi-volatile nature. The proposed novel workflow combines culture-dependent techniques, solvent demulsification-dispersive liquid-liquid microextraction, with quantitative liquid chromatography coupled with mass spectrometry analyses in order to identify marine bacterial isolates with the potential to degrade OPEs-FR-PL in the marine environment.
View Article and Find Full Text PDFJ Chromatogr A
December 2024
Food and Drug Safety Research Center, Tabriz University of Medical Sciences, Tabriz, Iran; Research Center of New Material and Green Chemistry, Khazar University, 41 Mehseti Street, Baku AZ1096, Azerbaijan; Pharmaceutical Analysis Research Center, Tabriz University of Medical Sciences, Tabriz, Iran.
This paper introduces an innovative technique for extracting pesticides from herbal infusions using a core-shell magnetic adsorbent (i.e., Cu-BTC@FeO) where achieving a notable enrichment factor for the target pesticides by coupling with a dispersive liquid-liquid microextraction method.
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