Search results for "RESIDUES"
showing 10 items of 147 documents
The application of phospholipid removal columns and ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry for quantificati…
2016
In this study a robust and sensitive method based on a proposed sample purification procedure, using zirconia-coated Phree™ columns and analysis by ultra-high performance liquid chromatography with triple quadrupole tandem mass spectrometry are presented for the assessment of multi-class antibiotics in farmed fish species. The sample preparation procedure benefited from combined precipitation of proteins and selective removal of phospholipids by Phree™ columns, resulting in a high sensitivity of the method (LOQ 0.3-9mgkg(-1)). The in-house validation results (precision, repeatability, decision limit CCα, detection capability CCβ, etc.) indicate that the elaborated method is fully suitable f…
Determination of pharmaceutical residues in wastewater using high performance liquid chromatography coupled to quadrupole-Orbitrap mass spectrometry
2016
Abstract A multi-class method for the determination of 24 emerging pharmaceutical residues has been developed and validated. The method is based on solid-phase extraction of wastewater samples using Strata-X cartridges followed by high performance liquid chromatography coupled to hybrid quadrupole − Orbitrap high resolution mass spectrometry (HPLC-Q-Orbitrap-HRMS). A single-laboratory validation procedure showed satisfactory analytical performance. The analysis of 21 samples collected at the wastewater treatment plant in Riga revealed the occurrence of 20 compounds of different therapeutic classes. The highest concentration was found for the central nervous system stimulator caffeine − up t…
Effects of cropping systems and irrigation on the bio-agronomic and quality response of industrial tomato (Lycopersicon esculentum mill.).
2012
This paper shows the results obtained in 2009 of a study carried out by the Dipartimento di Agronomia Ambientale e Territoriale (D.A.A.T.) aimed at identifying and evaluating various low input cropping systems for industrial tomato varieties, a traditional farming crop in Sicily. The tests were carried out on the Sparacia experimental farm (Cammarata AG, 37°37’N, 13°42’E). The farm is located in a sub-arid area with average rainfall levels of approx. 500 mm and average min/max temperatures of 9 and 21°C. The soils, typical of soil types in the area, are Eutric Vertisols. A split-split plot design with three repetitions was adopted and the following variables were studied: 1) management of c…
Impact of maize mucilage on atrazine mineralization andatzC abundance
2005
Soil was amended with maize mucilage, a major rhizodeposit, to study its role on the number of culturable soil micro-organisms, the structure of the bacterial community, atrazine mineralization and atzC abundance. The maximal percentage of atrazine mineralization was lower for mucilage-amended than for water-amended soil. Total culturable soil bacteria and 16S rDNA copy number, measured by RT-PCR, presented similar values and were not significantly (P < 0.05) different among treatments. Mucilage applied at a rate of 70 mu g C g(-1) dry soil day(-1) over two weeks did not modify the abundance of the total soil microflora. Global structure of soil bacterial communities revealed by RISA analys…
Site-heterologous haptens and competitive monoclonal antibody-based immunoassays for pyrimethanil residue analysis in foodstuffs
2015
Pyrimethanil is a widely used post-harvest fungicide whose residues are commonly found in fruits and vegetables. We herein report the synthesis of two new functionalized derivatives of pyrimethanil carrying an equivalent spacer arm at different positions of the molecule. The influence of the linker tethering site on the affinity of monoclonal antibodies was shown. Moreover, the development of competitive immunoassays in different formats and with high sensitivity to the target analyte - IC50 values below 0.3μg/L - is described. Optimized assays were characterized by the determination of the limit of quantification, trueness, and precision using water-diluted QuEChERS extracts of fruits and …
Determination of carbamate residues in fruits and vegetables by matrix solid-phase dispersion and liquid chromatography-mass spectrometry.
2000
Abstract Thirteen carbamates were analysed in orange, grape, onion and tomatoes by matrix solid-phase dispersion (MSPD) followed by liquid chromatography–mass spectrometry (LC–MS). Electrospray (ES) and atmospheric pressure chemical ionisation (APCI) were compared and both gave similar results in terms of sensitivity and structural information because at 20 V fragmentor voltages the fragmentation is minimal. The efficiency of different solid-phases (C18, C8, cyano, amine and phenyl) for the MSPD was compared. Mean recoveries using C8 varied from 64 to 106% with relative standard deviations of 5–15% in the concentration range of 0.01–10 mg kg−1. Matrix constituents did not interfere signific…
Analysis of organophosphorus pesticides in honeybee by liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry.
2001
Pesticides applied in extended agricultural fields may be controlled by means of bioindicators, such as honeybees, in which are the pesticides bioaccumulate. Liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) experiments with positive (PI) and negative (NI) ion modes were optimized for the analysis of 22 organophosphorus pesticides in honeybee samples. The extraction required 3 g of sample, which was extracted with acetone. The extract was purified with coagulating solution and reextracted with Cl(2)CH(2). Pesticides studied could be detected by both ionization modes except for parathion, parathion-methyl, and bromophos, which did not give signals …
Miniaturized matrix solid phase dispersion procedure and solid phase microextraction for the analysis of organochlorinated pesticides and polybromina…
2009
Abstract This work has developed a miniaturized method based on matrix solid phase dispersion (MSPD) using C18 as dispersant and acetonitrile–water as eluting solvent for the analysis of legislated organochlorinated pesticides (OCPs) and polybrominated diphenylethers (PBDEs) in biota samples by GC with electron capture (GC-ECD). The method has compared Florisil®-acidic Silica and C18 as dispersant for samples as well as different solvents. Recovery studies showed that the combination of C18–Florisil® was better when using low amount of samples (0.1 g) and with low volumes of acetonitrile–water (2.6 mL). The use of SPME for extracting the analytes from the solvent mixture before the injectio…
Solid-Phase Microextraction Liquid Chromatography/Tandem Mass Spectrometry To Determine Postharvest Fungicides in Fruits
2003
A method to determine five postharvest fungicides (dichloran, flutriafol, o-phenylphenol, prochloraz, tolclofos methyl) in fruits (cherries, lemons, oranges, peaches) has been developed using solid-phase microextraction (SPME) coupled to liquid chromatography (LC) with photodiode array (DAD), mass spectrometry (MS), or tandem mass spectrometry (MS/MS) with ion trap detection. Extraction involved sample homogenization with an acetone/water solution (5:1), filtration, and acetone evaporation prior to fiber extraction. The pesticides were isolated with a fused-silica fiber coated with 50-microm Carbowax/template resin. The effects of pH, ion strength, sample volume, and extraction time were in…
Determination of amitraz and its transformation products in pears by ethyl acetate extraction and liquid chromatography-tandem mass spectrometry.
2008
A method has been developed for identification and quantification of the acaricide amitraz and its transformation products, 2,4-dimethylaniline (DMA), 2,4-dimethylformamidine (DMF) and N-2,4-dimethylphenyl-N-methylformamidine (DMPF) in pears. The analytes were extracted using ethyl acetate and anhydrous sodium sulphate. Analysis was performed by liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS) in the positive ion mode using a triple quadrupole (QqQ) instrument. Two precursor-product ion transitions were monitored for each compound in the selected reaction monitoring (SRM) mode. The method was validated with pears taken from the orchard before the amitraz treatment …