Search results for "Solid phase extraction"
showing 10 items of 297 documents
Occurrence of glyphosate in beer from the Latvian market.
2018
A sensitive LC-MS/MS method for the determination of glyphosate in beer has been developed, validated, and applied to analyse 100 beer samples from 24 different producers and distributors in Latvia. The selected samples represented most beer brands and varieties sold in local supermarkets. Different procedures for sample preparation and chromatographic separation were compared. The final version of the method consisted of solid phase extraction, chromatographic separation on aminopropyl stationary phase, and detection using tandem mass spectrometry. The concentration of glyphosate in beer varied from below the LOD of 0.2 μg kg-1 up to 150 μg kg-1, higher than previously reported. Significan…
Analysis of cannabinoids by liquid chromatography–mass spectrometry in milk, liver and hemp seed to ensure food safety
2017
A method for determining cannabinoids, Δ9-tetrahidrocannabinol (THC), 11-nor-9-carboxy-Δ9-THC (THC-COOH) and 11-hidroxy-Δ9-THC (THC-OH) in milk, liver and hemp seeds based on liquid chromatography tandem mass spectrometry has been optimized and validated. Analytes were extracted with methanol and the extracts cleaned-up by solid-phase extraction using Oasis HLB (60 mg). The developed method was validated according to the Commission Decision 2002/657/EC. The decision limit (CCα) and detection capability (CCβ) ranged from 3.10–10.5 ng g−1 and 3.52–11.5 ng g−1, the recoveries were 76–118% and matrix effect ranged from −17.8% to 19.9% in the three matrices studied. The method was applied to foo…
Suspected-screening assessment of the occurrence of organic compounds in sewage sludge
2021
The profiling of emerging organic pollutants present in sludge and generated during wastewater treatment is much more limited than in water. This is mainly due to the difficulty of sludge analysis because of its high content of organic matter and interfering compounds. In this study, a generic extraction method using a mixture of buffered water (pH 4.1) and solid phase extraction (SPE) clean-up was applied to samples of sludge obtained in different treatment plants. This extraction was followed by determination of the contaminants by ultra-high performance liquid chromatography coupled to high resolution mass spectrometry (UHPLC-HRMS), using suspected screening to detect the most relevant o…
Efficiency of QuEChERS approach for determining 52 pesticide residues in honey and honey bees
2016
A comparison between QuEChERS and other pesticide extraction procedures for honey and honey bee matrices is discussed. Honey bee matrix was extracted by solvent based procedure whereas solid phase extraction was the protocol for the honey matrix. The citrate buffered QuEChERS method was used for both matrices. The methods were evaluated regarding cost (equipment and reagents), time, accuracy, precision, sensitivity and versatility. The results proved that the QuEChERS protocol was the most efficient method for the extraction of the selected pesticides in both matrices. QuEChERS is the most economical and less time-consuming procedure.SPE and solvent-based extraction procedures show equivale…
Multi‐residue extraction to determine organic pollutants in mussel hemolymph
2021
This study assesses the extraction of eleven pharmaceuticals, five pesticides, five perfluoroalkyl substances, and two illicit drugs in hemolymph from (Mytilus Galloprovincialis). Four extraction procedures using Phree™ Phospholipid Removal cartridges were tested using different volumes of methanol (400 and 600 μL) and acetonitrile (300 and 450 μL). The pollutants were determined by high-performance liquid chromatography–tandem mass spectrometry. The use of methanol gave several problems during the extraction procedure, such as longer times and sample loss. Three methods (acetonitrile 300 and 450 μL; and methanol 600 μL) were validated. Recoveries at three concentration levels (5, 50, and 1…
Determination of pesticide residues in fruit and vegetables.
1996
A review concerning the determination of pesticide residues in fruit and vegetables is presented. The basic principles and recent developments in the extraction and quantitation of pesticides are discussed. Consideration is given to solid phase and supercritical extraction techniques, automation and robotic systems, and immunoassay procedures.
Determination of phenolic antioxidants additives in industrial wastewater from polypropylene production using solid phase extraction with high-perfor…
2019
Abstract This paper describes a new method for the effective extraction of the residues of five synthetic phenolic antioxidants (AOs): Ditertbutylphenol (DTF), Irganox 1010, Irganox 1076, Ethanox 330 and Cyanox 1790, from industrial water produced during the polypropylene (PP) deodorization process. In the deordorization process, PP is stored in a column for an average time of four hours and exposed to nitrogen and water vapor to remove inflammable compounds which may generate atypical odors in the PP. The samples of interest were taken in the desorber, followed by cleansing and pre-concentration using modified styrene divinylbenzene polymer cartridges. Liquid chromatography was performed w…
Analysis of insecticides in honey by liquid chromatography–ion trap-mass spectrometry: Comparison of different extraction procedures
2010
The feasibility of different extraction procedures was tested and compared for the determination of 12 organophosphorus and carbamates insecticides in honey samples. In this sense, once the samples were pre-treated - essentially dissolved in hot water by stirring - and before they could be analyzed by liquid chromatography-ion trap-second stage mass spectrometry (LC-MS(2)), four different approaches were studied for the extraction step: QuEChERS, solid-phase extraction (SPE), pressurized liquid extraction (PLE) and solid-phase microextraction (SPME). The main aim of this work was to maximise the sensitivity of pesticides and to minimise the presence of interfering compounds in the extract. …
Determination of urea-derived pesticides in fruits and vegetables by solid-phase preconcentration and capillary electrophoresis
2001
A multiresidue analytical method based on solid-phase extraction (SPE) enrichment combined with capillary electrophoresis (CE), using micellar electrokinetic capillary chromatography (MEKC), was developed to determine ten substituted urea pesticides in orange and tomato samples. Several factors such as pH, composition and concentration of the buffer, concentration of surfactant, addition of organic solvent, and working voltage were optimized to obtain the best compound separation in the shortest time. Separation can be achieved in 7 min using a micellar aqueous pH 9 buffer composed of 4 mM borate and 35 mM sodium dodecyl sulfate. After an SPE procedure, which provided a 10-fold enrichment, …
Highly Efficient Removal of Neonicotinoid Insecticides by Thioether-Based (Multivariate) Metal–Organic Frameworks
2021
Circumventing the impact of agrochemicals on aquatic environments has become a necessity for health and ecological reasons. Herein, we report the use of a family of five eco-friendly water-stable isoreticular metal-organic frameworks (MOFs), prepared from amino acids, as adsorbents for the removal of neonicotinoid insecticides (thiamethoxam, clothianidin, imidacloprid, acetamiprid, and thiacloprid) from water. Among them, the three MOFs containing thioether-based residues show remarkable removal efficiency. In particular, the novel multivariate MOF {SrIICuII6[(S,S)-methox]1.5[(S,S)-Mecysmox]1.50(OH)2(H2O)}·36H2O (5), featuring narrow functional channels decorated with both -CH2SCH3 and -CH2…