Search results for "Limit of Detection"
showing 10 items of 146 documents
Determination of carbonyl compounds in particulate matter PM2.5 by in-tube solid-phase microextraction coupled to capillary liquid chromatography/mas…
2013
Abstract In this paper, a new procedure based on in-tube solid phase microextraction (IT-SPME)-capillary liquid chromatography hyphenated to mass spectrometry detection by using microelectrospray ionisation (CapLC–MS), has been reported. The device was proposed to quantify 12 carbonyl compounds (10 aliphatic aldehydes, an unsaturated aldehyde and a ketone) derivatized with 2,4-dinitrophenylhidrazine (DNPH) reagent in aqueous extracts of PM 2.5 . This methodology involves the on-line preconcentration of DNPH-carbonyl compounds derivatives coupled to the CapLC–MS system, efficiently providing appropriate sensitivity for the determination of the target analytes. Detection limits for the analyt…
Multi-residue determination of 47 organic compounds in water, soil, sediment and fish—Turia River as case study
2017
A sensitive and reliable method based on solid-liquid extraction (SLE) using McIlvaine-Na2EDTA buffer (pH = 4.5)-methanol and solid-phase extraction (SPE) clean up prior to ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC–MS/MS) was applied to determine 47 organic contaminants in fish, soil and sediments. The SPE procedure to clean-up the extracts was also used as extraction method to determine these compounds in water. Recoveries ranged from 38 to 104% for all matrices with RSDs 50% for 36 compounds in front of 9, matrix effect < 20% for 31 compounds against 21, and LOQs <25 ng g−1 for 38 compounds against 22) indicates that the proposed method is mor…
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 …
Analysis of perfluoroalkyl substances in waters from Germany and Spain
2012
Water has been identified as one of the main routes of human exposure to perfluoroalkyl substances (PFASs). This work assessed the presence of 21 PFASs along the whole water cycle using a new fast and cost effective analytical method based on an online sample enrichment followed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The method was validated for different types of matrices (ultrapure water, tap water and treated wastewater). The quality parameters for the 21 selected compounds presented good limits of detection (LOD) and quantification (LOQ) ranging, in general, from 0.83-10 ng/L to 2.8-50 ng/L, respectively. The method was applied to assess the occurrence …
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…
Capillary electrophoresis–inductively coupled plasma-mass spectrometry hyphenation for the determination at the nanogram scale of metal affinities an…
2012
Abstract A screening strategy based on hyphenated capillary electrophoresis and inductively coupled plasma mass spectrometry (CE–ICP-MS) was developed to classify phosphorylated ligands according to their europium(III) binding affinity in a hydro-organic medium (sodium formate, pH 3.7, H2O/MeOH 90:10, v/v). Taking advantage of the high sensibility of ICP-MS for detecting phosphorus, this method enabled to assess the affinity of a variety of phosphorylated compounds, including phosphine oxides, thiophosphines, phosphonates, and phosphinates, in less than 1 h and using less than 5 ng of substance. By varying the total europium concentration, complexation constants could be determined accordin…
Biomonitoring of Enniatin B1 and Its Phase I Metabolites in Human Urine: First Large-Scale Study
2020
Enniatins (Enns) are mycotoxins produced by Fusarium spp. which are a fungus widely spread throughout cereals and cereal-based products. Among all the identified enniatins, Enn B1 stands as one of the most prevalent analogues in cereals in Europe. Hence, the aim of this study was to evaluate for the first time the presence of Enn B1 and its phase I metabolites in 300 human urine samples using an ultrahigh-performance liquid chromatography high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) methodology. Enn B1 was detected in 94.3% of samples ranging from 0.007 to 0.429 ng/mL (mean value: 0.065 ng/mL). In accordance with previous in vitro and in vivo analysis, hydroxylated metabolites …
Photochemical sample treatment: a greener approach to chlorobenzene determination in sediments.
2014
Abstract Due to worker׳s exposure, solvent and stationary phases׳ consumption, sample purification is one of the most polluting steps in analytical procedures for determination of organic pollutants in real samples. The use of photochemical sample treatment represents a valid alternative methodology for extracts clean up allowing for a reduction of the used amount of organic solvents. In this paper we report the first application on the photolytic destruction of organic substances to eliminate some of the interferences in the analysis of Chlorobenzenes in sediment samples. The method׳s efficiency and robustness were compared with classic silica column purification process currently used in …
In syringe hybrid monoliths modified with gold nanoparticles for selective extraction of glutathione in biological fluids prior to its determination …
2020
Abstract In this work, a simple device for extraction glutathione (GSH) in biological fluids using a hybrid monolithic material within a polypropylene syringe is developed. For this purpose, glycidyl methacrylate-based monolith was firstly prepared within this housing material, and the polymer was modified with different ligands (ammonia, cysteamine and cystamine). The resulting materials (containing amine or thiol groups, respectively) were then functionalized with gold nanoparticles (AuNPs). The hybrid material that gave the largest AuNPs coverage was selected as solid-phase (SPE) sorbent and several variables affecting the extraction recovery of this compound were investigated. Under opt…
Highly sensitive monoclonal antibody-based immunoassays for the analysis of fluopyram in food samples
2019
Monoclonal antibody-based techniques have become a useful analytical technology in the agro-food sector. Nowadays, residues of the recently registered fungicide fluopyram are increasingly being found in quality control programs. In the present study, novel chemical derivatives of this pesticide were prepared and specific and high-affinity monoclonal antibodies to fluopyram were raised for the first time. Moreover, immunoassays to fluopyram were developed in two alternative enzyme-linked immunosorbent assay formats, using homologous and heterologous assay conjugates, with limits of detection below 0.05 µg L−1. The optimized immunoassays were applied to the analysis of fluopyram in fortified …