Search results for "solid phase"
showing 10 items of 360 documents
Multiresidue analysis of organic pollutants by in-tube solid phase microextraction coupled to ultra-high performance liquid chromatography-electrospr…
2013
In this work, in-tube solid phase microextraction (IT-SPME) coupling with ultra-high-pressure liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) multiresidue analytical method has been proposed for the first time for on-line enrichment of 9 analytes included in Water Frame Directive 2000/60/EC (WFD). The device was equipped with a GC TRB-5 capillary column, used as pre-concentration loop, and two conventional six-port injection valves. Water sample and desorption solvent volumes were tested. The optimum conditions were 4mL of processed sample followed by elution with 40μL of methanol. The analytes were detected with a mass spectrometer after being ionized positively using an elect…
Comparison of various liquid chromatographic methods for the analysis of avermectin residues in citrus fruits.
2001
Abstract Various liquid chromatographic (LC) techniques for analyzing avermectin (Abamectin) were compared after extraction of residues from citrus fruit samples by matrix solid-phase dispersion (MSPD). LC with UV and fluorescence detection were used as also was LC coupled to the mass spectrometer by an electrospray interface. The results obtained by the three methods were compared in terms of sensitivity and selectivity. The combination of MSPD extraction and LC with fluorescence detection have made it possible to quantify 0.5 μg kg −1 of Abamectin in 0.5 g of orange sample, with an overall average recovery of 94%. The procedure provides a simple and sensitive method for monitoring Abamect…
Analysis of meat samples for anabolic steroids residues by liquid chromatography/tandem mass spectrometry.
2007
A rapid, specific and highly sensitive multi-residue method for the determination of anabolic steroid residues in bovine, pork and poultry muscle tissues was developed. The sample preparation involves enzymatic digestion followed by extraction with methanol. The crude extract was cleaned up by solid-phase extraction (SPE) combining C18 and NH2 columns. The detection was carried out by a highly sensitive liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) method using both positive and negative ionization modes. Natural and synthetic steroids covering different polarities could be extracted, concentrated and purified using one single method. Mobile phase com…
Preconcentration and speciation of chromium in waters using solid-phase extraction and atomic absorption spectrometry
2000
Abstract A method for the preconcentration and speciation of chromium was developed. After formation of an anionic compound with ethylenediaminetetraacetic acid (CrY − ), Cr (VI) and Cr (III) are retained on a strong anionic phase (SAX) and controlled elution with 0.5 M NaCl permits their speciation. The retention and elution conditions were optimised, and interferences due to the presence of other ions such as Mg(II), Mn(II), Sn(II), Fe(III), Ba(II), Al(III), Ca(II), chloride, iodine, bromide, fluoride, sulphate, phosphate, bicarbonate and nitrate were studied. The detection limits were 0.4 μg l −1 and 1.1 μg l −1 for Cr(III) and Cr(VI), respectively, and reproducibility was 9%. The result…
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…
Removal and fate of endocrine disruptors chemicals under lab-scalepostreatment stage. Removal assessment using light, oxygen and microalgae
2013
[EN] The aim of this study was to assess the effect of light, oxygen and microalgae on micropollutants removal. The studied micropollutants were 4-(1,1,3,3-tetramethylbutyl)phenol (OP), technical-nonylphenol (t-NP), 4-n-nonylphenol (4-NP), Bisphenol-A (BPA). In order to study the effect of the three variables on the micropollutants removal, a factorial design was developed. The experiments were carried out in four batch reactors which treated the effluent of an anaerobic membrane bioreactor. The gas chromatography mass spectrometry was used for the measurement of the micropollutants. The results showed that light, oxygen and microalgae affected differently to the degradation ratios of each …
Biological effects and photodegradation by TiO(2) of terpenes present in industrial wastewater.
2010
Abstract The aim of this work was to study the biological effects of four monoterpenes, i.e. α-pinene, β-pinene, 3-carene and d -limonene present in the wastewater of a citrus transformation factory. The study was carried out by exposing V79 Chinese hamster cells to single terpene or to the mixture of four terpenes at concentrations corresponding to those in the wastewater evaluated by head space solid phase micro extraction and gas chromatography (HS-SPME-GC) analyses. Treatments with single or combined terpenes similarly affected cell vitality, but only the combined treatments induced the 6-thioguanine resistant mutants. Moreover the photocatalytic degradation of the four terpenes was suc…
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…