Search results for "liquid chromatography"
showing 10 items of 942 documents
Pressurized liquid extraction followed by liquid chromatography–mass spectrometry for determination of zearalenone in cereal flours
2010
Abstract A method for determination of zearalenone in cereal flour has been developed applying pressurized liquid extraction (PLE) using methanol/acetonitrile (50:50 v/v) as the extraction solvent. The extracted samples were analyzed with liquid chromatography coupled to mass spectrometry (LC–MS) with an electro spray ionisation interface (ESI). The method was validated as a quantitative confirmatory method according to the Eu Commission Decision 2002/657/EC. Recoveries of the extraction step data were satisfactory with values higher then 70%. Quantification limits (LOQ) were 5 μg/kg for ESI (+) and 1 μg/kg for ESI (−). Twenty one flour samples produced in different countries were extracted…
Principle and analytical applications of resonance lonization mass spectrometry
1989
Resonance ionization mass spectrometry (RIMS) is a very sensitive analytical technique for the detection of trace elements. This method is based on the excitation and ionization of atoms with resonant laser light followed by mass analysis. It allows element and, in some cases, isotope selective ionization and is applicable to most of the elements of the periodic table. A high selectivity can be achieved by applying three step photoionization of the elements under investigation and an additional mass separation for an unambiguous isotope assignment. An effective facility for resonance ionization mass spectrometry consists of three dye lasers which are pumped by two copper vapor lasers and of…
Synthesis of a technetium-99m labelledL-tyrosine derivative with thefac-99mTc(I)(CO)3-core using a simple kit-procedure
2004
Summary The synthesis of a novel technetium-99m labelled derivative of l-tyrosine as a potential tumour imaging agent for nuclear medicine diagnosis is reported. The synthesis involved the labelling precursor fac-[ 99m Tc(OH2)(CO)3] + which was synthesized using the commercially available Isolink 1 -labelling kit and the tyrosine derivative O-(N,Nbis(carboxymethyl)aminoethyl)-l-tyrosine trifluoroacetate. The labelled compound O( 99m Tc(I)-tricarbonyl-N,N-bis(carboxymethyl)aminoethyl)-l-tyrosine was obtained in a radiochemical yield of 70–80% within 60 min with a radiochemical purity greater than 98% without any HPLC purification step. Purification was achieved merely by solid phase extracti…
Synthesis of novel WAY 100635 derivatives containing a norbornene group and radiofluorination of [18F]AH1.MZ as a serotonin 5-HT1Areceptor antagonist…
2009
5-HT1A receptors are involved in a variety of psychiatric disorders and in vivo molecular imaging of the 5-HT1A status represents an important approach to analyze and treat these disorders. We report herein the synthesis of three new fluoroethylated 5-HT1A ligands (AH1.MZ, AH2.MZ and AH3.MZ) as arylpiperazine derivatives containing a norbornene group. AH1.MZ (Ki= 4.2 nM) and AH2.MZ (Ki=30 nM) showed reasonable in vitro affinities to the 5-HT1A receptor, whereas AH3.MZ appeared to be non-affine toward the 5-HT1A receptor. The receptor profile of AH1.MZ and AH2.MZ showed selectivity within the 5-HT system. 18F-labelling via [18F]FETos to [18F]AH1.MZ was carried out in radiochemical yields of …
MICELLAR CHROMATOGRAPHIC PROCEDURE WITH DIRECT INJECTION FOR THE DETERMINATION OF SULFONAMIDES IN MILK AND HONEY SAMPLES
2001
The capability of liquid chromatography with micellar mobile phases of sodium dodecyl sulfate (SDS), of allowing the direct injection of biological fluids into reversed-phase columns, was applied to the determination of sulfonamides in milk and honey samples. The chromatographic behavior of a group of 15 sulfonamides was studied at pH 3.0 where the drugs showed a greater separation space. Acetonitrile was added to the mobile phase to decrease the retention of the most hydrophobic drugs and increase the efficiencies, which yielded a higher resolution. The samples were diluted with 0.10 M SDS to facilitate the solubilization of the matrix compounds and release the protein-bound drugs. The pro…
Packing meterials with surface barriers, controlled distribution and topography of ligands for sample clean-up and analysis of biologically active so…
1991
Various types of, so-called, restricted access packings have been developed for sample clean-up and analysis of biologically active solutes by means of HPLC. The unique feature of these packings is that they prevent the access of matrix components such as protein whilst selectively retaining the drug components and their metabolites. This results from the fact that the particles of the packings possess a surface barrier for large solutes at the external or internal surface area and exhibit a controlled gradient in the chemical surface composition. They are grouped, according to their particle structures, into internal-surface reversed phases (ISRP), shielded hydrophobic phases (SHP), semi-p…
Multi-residue analysis of 30 currently used pesticides in fine airborne particulate matter (PM 2.5) by microwave-assisted extraction and liquid chrom…
2009
A confirmatory and rapid procedure has been developed for the determination of 30 currently used pesticides (CUP) in fine airborne particulate matter (PM 2.5) at trace level. The proposed method includes extraction of PM 2.5-bound pesticides by microwave-assisted extraction (MAE) followed by a direct injection into LC-MS/MS. The main parameters affecting the MAE extraction (time, temperature and volume of solvent) were optimised using statistical design of experiments (DoE). The matrix effect was also evaluated. Recoveries ranged from 72 to 109% and the limit of quantification (LoQ) was 32.5 pg m(-3) for chlorpyrifos, 13.5 pg m(-3) for fenhexamid, imazalil and prochloraz, and 6.5 pg m(-3) f…
Resolution of mixtures of steroidal hormones with micellar eluents of sodium dodecyl sulphate and acetonitrile or pentanol
2000
An optimization strategy was applied to explore the capability of hybrid micellar eluents of sodium dodecyl sulphate (SDS), using acetonitrile or pentanol as modifiers, to resolve mixtures of eleven steroids showing a wide range of hydrophobicity (clostebol acetate, dehydrotestosterone, dydrogesterone, medroxyprogesterone, medroxyprogesterone acetate, methandienone, methyltestosterone, progesterone, testosterone, testosterone enanthate and testosterone propionate). The accurate prediction of the retention behaviour of the steroids, with relative errors in the 0.8–1.7% and 0.4–2.9% ranges for SDS-acetonitrile and SDS-pentanol eluents, respectively, demonstrated the reliability of the methodo…
Retention-structure relationship studies for some steroidal hormones in micellar liquid chromatography
2000
The retention behavior in a C18 column of fourteen steroidal hormones (clostebol acetate, dehydrotestosterone, dydrogesterone, medroxyprogesterone, medroxyprogesterone acetate, methandienone, methyltestosterone, nandrolone, nandrolone decanoate, progesterone, testosterone, testosterone enanthate, testosterone propionate and, stanozolol) with pure micellar mobile phases prepared from sodium dodecyl sulfate (SDS), and hybrid mobile phases comprising SDS-acetonitrile and SDS-pentanol, was correlated with their octanol-water partition coefficients. Similar correlations were found with retention data obtained by other authors in gas chromatography, conventional reversed-phase liquid chromatograp…
DETERMINATION OF STEROIDAL HORMONES IN URINE SAMPLES BY MICELLAR LIQUID CHROMATOGRAPHY FOLLOWING SOLID-PHASE EXTRACTION
2001
Steroidal hormones were determined in spiked urine samples using micellar mobile phases of sodium dodecyl sulphate (SDS)-pentanol, solid-phase extraction (SPE), and detection in the UV region. In the optimized procedure, a 10 mL aliquot of urine sample is loaded into a C18 cartridge and washed with 2 mL of 50:50 (v/v) methanol-water, followed by 200 μL of 70:30 (v/v) methanol-water. The retained steroids are eluted with 2 mL of methanol and the eluate evaporated to dryness under nitrogen at 50°C. The residue is redissolved with 200 μL of the micellar mobile phase used in the chromatographic separation and injected into the chromatograph. The performance of the procedure was checked for 13 s…