Search results for "Solid phase extraction"
showing 10 items of 297 documents
Biomonitoring of glyphosate and AMPA in the urine of Spanish lactating mothers
2021
The objectives of this study were to evaluate the urinary levels of Glyphosate (Gly) and its metabolite aminomethylphosphonic acid (AMPA) in Spanish breastfeeding mothers (n = 97), to identify the main predictors of exposure and to perform a risk assessment. Urine samples were analyzed using a method based on solid phase extraction and liquid chromatography tandem mass spectrometry (LC-MS/MS) determination. The developed method showed limits of quantification of 0.1 μg/L for both analytes. The detection frequencies (DFs) were 54% for Gly and 60% for AMPA, with geometric means (GMs) of 0.12 μg/L and 0.14 μg/L, respectively. In the statistical analysis, no relationship was found between the u…
Measurement of pollution levels of N-nitroso compounds of health concern in water using ultra-performance liquid chromatography–tandem mass spectrome…
2017
International audience; This paper reports the development of a highly sensitive analytical method combining solid-phase extraction (SPE) with ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC–MS/MS), for the monitoring of ultra-trace levels of N-nitrosamines in water samples. Under optimized analytical conditions, chromatographic separation was performed in 3 min, in isocratic mode, using an Acquity UHPLC C18 column and a mobile phase consisting of acetonitrile, water, and formic acid (60:40:0.1, v/v/v) at a flow rate of 0.4 mL min−1. Electrospray ionization tandem interface was employed prior to mass spectrometric detection. Good linearity (R2 ≥ 0.9…
Development and optimization of gas chromatography coupled to high resolution mass spectrometry based method for the sensitive determination of Dechl…
2017
An analytical method has been developed for the trace determination of 10 dechlorane-related compounds (DRCs) in food products by gas chromatography - high resolution mass spectrometry (GC-HRMS). The highest sensitivity of this instrumental analysis method was achieved by selection of the GC column type, optimization of the heated zones within the instrument, and adjusting the electron impact energy. The efficiency of solid phase extraction as clean-up procedure was also optimized. Two different types of cartridges - neutral silica gel and Florisil®, as well as seven organic solvents or their mixtures - n-hexane, cyclohexane, acetone, toluene, n-hexane/ethyl acetate, n-hexane/acetone, and n…
Photo-induced fluorescence of magnesium derivatives of tetracycline antibiotics in wastewater samples
2009
Abstract An analytical strategy, for the determination of tetracyclines (TCs), based on a HPLC system coupled with a photo-reactor followed by post-column derivatization was developed. Higher fluorescence emission after coupling the resulting photo-fragments with magnesium ions was observed for the determination of minocycline (MC), epitetracycline (ETC), tetracycline (TC) and doxycycline (DC). The manifold included a HPLC system with a photo-reactor (PTFE tubing helically coiled around a low-pressure mercury lamp), a mixing T-piece and a fluorescence detector. The derivatization reagent was delivered at 0.5 mL min −1 by a pump. After HPLC separation using a gradient system with a mobile ph…
Analysis of Trace Pharmaceuticals and Related Compounds in Municipal Wastewaters by Preconcentration, Chromatography, Derivatization, and Separation …
2014
A significant portion of pharmaceuticals and other organic chemicals consumed by people and animals are released into municipal wastewater treatment plants. Most of them are degraded during the wastewater treatment processes, but some of them degrade only partially and may be widely transported and dispersed into the aquatic environment. This is why efficient and fast analytical methods are needed for detection of organic compounds in wastewaters at trace levels. Because wastewaters often consist of complex matrices and high-molecular mass materials, e.g., lignocellulosic biomass, which may bring challenges to the sample preparation procedures, efficient pre-concentration methods such as so…
Design, characterization and comparison of materials based on β and γ cyclodextrin covalently connected to microporous silica for environmental analy…
2018
Abstract Determination of organic pollutants in environmental samples presents great difficulties due to the lack of sensitivity and selectivity in many of the existing analytical methods. In this work, the efficiency of materials based on silica structures containing bounded γ-cyclodextrin has been evaluated to determinate phenolic compounds and polycyclic aromatic hydrocarbons in air and water samples, respectively, in comparison with materials made of β-cyclodextrin. According to the results obtained for the material characterization, the new γ-cyclodextrin solid phase does not apparently present any porosity when used in air samples, but it has been shown to work efficiently for the pre…
A preliminary study on the distribution of morphine and its glucuronides in the subcompartments of blood.
1998
[Abstract ] The distribution of morphine, morphine-3-glucuronide (M3G), and morphine-6-glucuronide (M6G) in whole blood, plasma, and packed erythrocytes was studied. Parameters investigated were the hematocrit values (10, 42, 44, and 71%) and the water content of the samples. The blood-to-plasma ratio of morphine concentrations was unaffected by variations in hematocrit and water content, whereas the corresponding ratios for M3G and M6G were strongly influenced. Ratios were 0.53 to 0.65 and 0.52 to 0.62 in specimens with average hematocrit values (42 and 44%, respectively), and the ratios were 0.81 or 0.89 (hematocrit 10%) and 0.27 or 0.28 (hemalocrit 71%) in blood samples with different he…
Sensitive determination of polycyclic aromatic hydrocarbons in water samples using monolithic capillary solid-phase extraction and on-line thermal de…
2011
A methacrylate-based monolithic capillary column has been evaluated for the preconcentration of polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. For this purpose, the monolyte was in situ synthesized in a 6cm×0.32mm id fused-silica capillary. The microextraction unit was fitted to a micro-HPLC pump to pass 10mL of sample. The isolated pollutants were eluted by means of 10μL of methanol, the organic phase being directly collected in a specific interface that can be fitted to the injection port of the gas chromatograph without modification. The interface allows the on-line thermal desorption of the PAHs, avoiding the dilution and providing enough sensitivity to reach …
Analysis of 18 perfluorinated compounds in river waters: Comparison of high performance liquid chromatography–tandem mass spectrometry, ultra-high-pe…
2012
In this work, the performance of ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) and capillary liquid chromatography-mass spectrometry (CLC-MS) has been studied for the analysis of eighteen perfluorinated compounds in water samples. UHPLC-MS/MS and CLC-MS analysis were carried out using a Zorbax C-18 column (50 mm × 2.1 mm, 1.8 μm) and a Zorbax SB-C18 column (150 mm × 0.5 mm, 3.5 μm), respectively, in gradient elution mode with a mobile phase of ammonium formate and methanol. Both techniques were compared with conventional LC-MS/MS in terms of speed, sensitivity, selectivity and resolution. Water samples were extracted by solid phase extraction (SPE). Mea…
Distribution and fate of perfluoroalkyl substances in Mediterranean Spanish sewage treatment plants.
2014
The concentrations of 21 perfluoroalkyl substances (PFASs: C4-C14, C16, C18 carboxylates, C4, C6-C8 and C10 sulfonates and C8 sulfonamide) were determined in influent, effluent and sludge from 16 different sewage treatment plants (STPs) located in the Ebro (6), Guadalquivir (5), Jucar (2) and Llobregat (3) Rivers, in two consecutive years (2010 and 2011). The analytes were extracted by solid phase extraction (SPE) and determined by Liquid Chromatography triple Quadrupole Mass Spectrometer (LC-QqQ-MS). All samples, except two sludges from Guadalquivir River STPs, were contaminated with at least one PFAS. Perfluorobutanoate (PFBA), perfluoropentanoate (PFPeA) and perfluorooctane sulfonate (L-…