Search results for "preparation"
showing 10 items of 939 documents
COMPARATIVE STUDY OF C18- AND STYRENE-DIVINYLBENZENE-BASED SORBENTS FOR THE ENRICHMENT OF PHENOLS FROM WATER
2001
The potential of solid-phase extraction with C18- and styrene divinylbenzene-based sorbents for the preconcentration of phenols from water samples has been evaluated for a variety of phenols of different polarities: phenol, o-, m- and p-cresol, 2-chlorophenol, and 4-chloro-3-methylphenol. The extraction efficiencies have been calculated for different volumes of samples containing the analytes at different concentration levels. The UV limits of detection were of 1–5 ng/mL, for the method using Bond Elut C18 cartridges and sample volumes of 25 mL, and 0.05–0.1 ng/mL (except for 4-chloro-3-methylphenol) for the method using the polymeric sorbent Bond Elut PPL and 1000 mL of the samples. Possib…
Use of micellar mobile phases for the chromatographic determination of clorazepate, diazepam, and diltiazem in pharmaceuticals
2001
An ODS-2 column, a micellar mobile phase of high elution strength containing 0.1M sodium dodecyl sulfate and 3% (v/v) butanol, and ultraviolet detection at 230 nm are used for the determination of either of two benzodiazepines (clorazepate and diazepam) and a benzothiazepine (diltiazem) in pharmaceuticals. The procedure is shown to be competitive against conventional chromatography with methanol-water mobile phases, especially for diltiazem. The composition of the micellar mobile phase is selected using a predictive strategy based on an accurate retention model and assisted by computer simulation. Calibration graphs are linear at least in the 2.5 to 20 microg/mL, 4 to 20 microg/mL, and 5 to…
Improved detection limit for ammonium/ammonia achieved by Berthelot's reaction by use of solid-phase extraction coupled to diffuse reflectance spectr…
2005
Abstract The proposed procedure is based on the extraction of the indothylmol blue into C 18 solid-phase extraction (SPE) membranes and direct quantification on the membrane surface by diffuse reflectance spectroscopy. The analytical performance of the proposed method has been evaluated for standard solutions of ammonium using reflectance values, R , as well as the Kubelka–Munk function, F ( R ). The results have been compared with those obtained by the conventional method, which uses UV–vis absorption spectroscopy with a sensor-based method. The described methodology provided satisfactory linearity and reproducibility within the ammonium concentration intervals 25–250 μg L −1 and 25–500 μg…
Preconcentration and dansylation of aliphatic amines using C18 solid-phase packings
2002
Abstract Precolumn preconcentration and derivatization on solid sorbents (Bond Elut C18 solid-phase extraction cartridges) of low-molecular-mass aliphatic amines in water samples have been performed using dansyl chloride (Dns-Cl) as derivatization reagent. Conditions for analyte preconcentration and derivatization such as volume sample, reagent concentration, time, pH and temperature reaction were optimised. On the basis of these studies a rapid and sensitive method for screening of aliphatic amines in waters is presented. Up to volumes of 5 ml, samples are drawn through the sorbent, the analytes retained are dansylated at basic pH, at 100 °C for 10 min or 85 °C for 15 min. The derivatized …
Univariate near infrared methods for determination of pesticides in agrochemicals
2006
Abstract It has been developed a general strategy for the determination of pesticides in agrochemicals by Fourier transform near infrared (FT-NIR) spectroscopy. The methodology is based on previous extraction of the active principles through sonication with acetonitrile and direct determination by transmission measurements, using glass vials as measurement cells and univariate calibration at selected wavenumbers as a function of the pesticide to be analyzed. Chlorsulfuron, metamitron, iprodione, pirimicarb, procymidone and tricyclazole were used as test molecules and data obtained by FT-NIR for 20 samples containing one of these active principles compare well with those found by reference l…
Determination of cyromazine in pesticide commercial formulations by vibrational spectrometric procedures
2004
Two vibrational spectrometry-based methodologies were developed for Cyromazine determination in solid pesticide formulations: a Fourier transform infrared (FTIR) procedure, based on the extraction of Cyromazine by CH3OH and direct determination in the extracts by peak height measurement at 1622 cm−1 corrected using a baseline defined at 1900 cm−1, and a FT-Raman determination, made directly on the powdered solid products using standard chromatographic glass vials as sample cells and measuring the Raman intensity between 633 and 623 cm−1 for a baseline established between 663 and 601 cm−1. The sensitivity obtained was 0.01631 absorbance g−1 mg for FTIR determination and 2.23 area values g−1 …
Fourier transform infrared determination of imidacloprid in pesticide formulations
2004
A simple method has been developed for Fourier Transform Infrared (FTIR) determination of Imidacloprid in pesticide formulations. Samples were diluted with CHCl3 and the FTIR spectra of samples and standards were obtained at a nominal resolution of 4 cm-1 from 4000 to 900 cm-1 accumulating 25 scans. Imidacloprid determination was based on the measure of either peak area from 1577 to 1567 cm-1 or peak height at 1572 cm-1, both corrected using a horizontal baseline defined at 1900 cm-1. The limits of detection achieved, of the order of 9 µg g-1, were appropriate for the determination of Imidacloprid in commercially available formulations. FTIR results were statistically comparable to those fo…
Optimization of LC–MS/MS using triple quadrupole mass analyzer for the simultaneous analysis of carbosulfan and its main metabolites in oranges
2006
This paper describes an analytical method involving a simple solvent extraction for the simultaneous liquid chromatography coupled to quadrupole tandem mass spectrometry (LC-MS/MS) determination of carbosulfan, its most toxic metabolite--carbofuran--, and its other main metabolites--3-hydroxycarbofuran, 3-ketocarbofuran, 3-hydroxy-7-phenolcarbofuran, 3-keto-7-phenolcarbofuran, 7-phenolcarbofuran and dibutylamine--in oranges. Chromatography was performed on a Zorbax Bonus-RP (150 mm x 2.1 mm, 5 microm). The mobile phase was a ternary gradient water-methanol-acetonitrile with 1.0 mM ammonium acetate at flow rate of 0.2 ml min(-1). The LC separation and MS/MS optimization were studied to selec…
Quantification of Imidacloprid in Honeybees: Development of a Chemiluminescent ELISA
2010
A Chemiluminescente Enzyme-Linked Immuno-Sorbent Assay (CL-ELISA) for determination and quantification of the fungicide imidacloprid in honeybees was developed in an indirect competitive format. The assay was optimized by determining: the optimal coating conjugate concentration and anti-imidacloprid antiserum dilution, the effect of the incubation time on the competitive step, the tolerance to organic solvents. The IC50 and the limit of detection (LOD) values were 14.8 ng mL-1 and 0.11 ng mL -1, respectively, similar to those of colorimetric ELISA with a calibration range of 0.1 – 2600 ng mL-1. Cross reactivity of some related compounds such as three imidacloprid metabolites, 6-chloro nicot…
Environmental and food applications of LC-tandem mass spectrometry in pesticide-residue analysis: An overview
2003
An overview is given on pesticide-residue determination in environmental and food samples by liquid chromatography/mass spectrometry/mass spectrometry (LC/MS/MS). Pesticides comprise a large number of substances that belong to many completely different chemical groups, the only common characteristic is that they are effective against pests. They still constitute a challenge in MS because there is no collective pathway for fragmentation. A brief introduction to the theory of tandem MS permits a discussion of which parameters influence the ionization efficiency when the ions are subjected to different actions. Emphasis is placed on the different tandem MS instruments: triple and ion-trap quad…