A method consisting of dispersive liquid-liquid microextraction (DLLME) followed by injection-port derivatization and gas chromatography-mass spectrometry (GC-MS) for the analysis of free lipophilic compounds in fruit juices is described. The method allows the analysis of several classes of lipophilic compounds, such as fatty acids, fatty alcohols, phytosterols and triterpenes. The chromatographic separation of the compounds was achieved in a chromatographic run of 25.5min. The best conditions for the dispersive liquid-liquid microextraction were 100μL of CHCl in 1mL of acetone. For the injection-port derivatization, the best conditions were at 280°C, 1min purge-off, and a 1:1 sample:derivatization reagent ratio (v/v) using N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA):pyridine (1:1) as reagent. Quality parameters were assessed for the target compounds, giving a limits of detection (LODs) ranging from 1.1 to 5.7ng/mL and limits of quantification (LOQs) from 3.4 to 18.7ng/mL for linoleic and stearic acid, respectively. Repeatability (%RSD, n=5) was below 11.51% in all cases. In addition, the method linearity presented an r ≥0.990 for all ranges applied. Finally, the method was used to test the lipophilic fraction of various samples of commercial fruit juice.
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http://dx.doi.org/10.1016/j.chroma.2017.03.027 | DOI Listing |
Cell
December 2024
Schaller Research Groups, Department of Infectious Diseases, Virology, Heidelberg University, Heidelberg, Germany; BioQuant, Heidelberg University, Heidelberg, Germany. Electronic address:
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.
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