Search results for "Derivatization"
showing 10 items of 215 documents
Spectrophotometric determination of phenol and resorcinol by reaction with p-aminophenol
1993
Abstract Based on the reaction with p-aminophenol, a series of procedures have been developed for the spectrophotometric determination of phenol and resorcinol. Three basic approaches have been studied: (i) a batch procedure, using the dissolved oxygen as oxidant, (ii) a stopped-flow procedure by use of KIO4 as oxidant and (iii) a flow injection (FI) procedure developed in the presence of KIO4. Phenol can be accurately determined at 626 nm, in the stopped-flow mode, after a reaction time of 45 min in 0.005M NaOH, 0.004M KIO4 and 500 μg/ml of PAP. The development of a manifold, which incorporates a sample parking, is a convenient approach which makes it possible to measure, in the stopped-fl…
Rapid microwave assisted hydrolysis of formetanate
1993
Abstract A fast microwave-assisted hydrolysis procedure has been developed for the derivatization of formetanate previously to the flow-injection spectrophotometric determination of m -aminophenol by reaction with p -aminophenol. Formetanate is quantitatively hydrolyzed with 0.1 M NaOH in 150 s using a closed polyetrafluoroethylene reactor with 115 ml internal volume and a radiation power of 390 W. The above procedure has been applied, as a previous step, for the flow-injection spectrophotometric determination of formetanate in spiked water samples and accurate and precise results have been found. The method permits to obtain a limit of detection of 0.025 mg 1 −1 of formetanate. The relativ…
Determination of catecholamines as aminochromes by micellar liquid chromatography with thermal lens spectrophotometric detection
1994
The determination of catecholamines (CAs) using micellar liquid chromatography with thermal lens spectrophotometric detection has been studied. CAs are oxidized with hexacyanoferrate(III) to aminochromes which are separated with a mobile phase of 0.05 M sodium dodecyl sulphate, 7% propanol and 0.03 M citrate buffer, pH 4.8, on a partially endcapped C18 column. The aminochrome-micelles and aminochrome-stationary phase association constants are evaluated. Using the 488 nm line of an Ar+ laser with 250 mW pump power the limits of detection are about 4 ng mL−1. The technique is applied to the determination of unconjugated CAs in urine using isoproterenol as internal standard.
Improving detection limits for organotin compounds in several matrix water samples by derivatization-headspace-solid-phase microextraction and GC-MS.
2010
Triethyltin, tributyltin, diphenyltin and triphenyltin were selected as model compounds. The method is based on in situ ethylation and simultaneous headspace-solid-phase microextraction (HS-SPME) and gas chromatographic-mass spectrometry analysis (GC-MS). The extraction procedure was optimized studying some variables such as reaction time, salinity, sample volume and headspace volume. SPME-GC-MS and SPME-GC-FID techniques were compared; quality assurance parameters such as sensitivity, selectivity and precision were established. The proposed procedure showed limits of detection between 0.025 and 1 ng/L. The linearity was in the 0.025-5000 ng/L range. The precision expressed as relative stan…
Derivatization of tertiary amphetamines with 9-fluorenylmethyl chloroformate for liquid chromatography: determination of N-methylephedrine.
2000
The fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) was evaluated for the derivatization of tertiary amphetamines prior to liquid chromatographic analysis. Conditions for the derivatization were investigated, including the reaction time, the derivatization reagent concentration and the pH, using N-methylephedrine as a model compound. On the basis of these studies, a method for the quantification of N-methylephedrine is presented. The method involves derivatization with FMOC at ambient temperature and separation of the derivatives formed on a LiChrospher C18, 5 μm, 125 × 4 mm id column using acetonitrile–water gradient elution. The proposed procedure shows good linearity, accuracy…
Flow injection-spectrophotometric determination of cresol compounds in water by reaction withp-aminophenol
1993
A spectrophotometric method has been developed for the simultaneous determination ofo-cresol andm-cresol in water by reaction withp-aminophenol (PAP). Three different methodologies have been assayed; (i) batch analysis, after reaction in an alkaline medium in the presence of dissolved molecular oxygen as oxidizing agent, (ii) a stopped-flow procedure, carried out in the presence of KIO4 and (iii) a flow injection method based on the same approach. The batch procedure requires 22 min for the full development of colour witho-cresol and 12 min form-cresol. In the stopped-flow mode, using KIO4 and a reaction time of 12 min, better sensitivity can be obtained for both compounds and limits of det…
Liquid chromatographic determination of trimethylamine in water.
2004
A method for the selective determination of trimethylamine (TMA) in aqueous matrices by liquid chromatography is reported. The proposed procedure is based on the derivatization of the analyte with 9-fluorenylmethyl chloroformate (FMOC) in a precolumn (Hypersil C18, 30 microm, 20 mm x 2.1 mm i.d.) connected on-line to the analytical column (LiChrosphere 100 RP18, 5 microm, 125 mm x 4 mm i.d.). Gradient elution was performed with a mixture of acetonitrile-water-0.05 M borate buffer (pH 9.0). The method has been applied to the direct determination of TMA in water within the 0.25-10.0 microg/ml concentration interval, and can also be adapted to the determination of TMA over the range 0.05-1.0 m…
Extraction and analysis of ochratoxin A in bread using pressurised liquid extraction and liquid chromatography.
2005
A pressurised liquid extraction (PLE) method for the analysis of ochratoxin A (OTA) in bread samples is given. Parameters such as solvent, temperature, pressure and time were investigated thoroughly. The optimized PLE conditions were: methanol as extraction solvent, 80 degrees C, 2000 psi and a 5-min cycle. OTA was determined by liquid chromatography coupled with fluorescence detection and confirmed by methyl ester derivatization. Under these conditions OTA recovery is 92.3% with a RSD of 5%. Limits of detection and quantification were 0.02 and 0.06 microg/kg, respectively. The proposed method was applied to 20 bread samples, finding two positive samples with OTA levels below the maximum pe…
Quality control of pharmaceuticals containing clenbuterol by thermal lens spectrometry.
1996
An ultrasensitive absorptiometric procedure for the determination of clenbuterol in pharmaceutical preparations was developed. Clenbuterol was diazotized with nitrite and coupled with 1-(naphthyl)ethylenediamine, and the absorbance of the azo dye formed was measured by both spectrophotometry and ultrasensitive thermal lens spectrometry (TLS). The TLS limit of detection was 1.5 ppb, 14-fold lower than with a Hewlett-Packard diode array spectrophotometer. Thus, the TLS procedure can be advantageously applied to quality control of clenbuterol at the individual dose level and in small samples. Repeatability as relative standard deviation was 1.5% (50 ppb, n = 6).
Sensitive determination of methylenedioxylated amphetamines by liquid chromatography.
2001
Different strategies for the liquid chromatographic determination of methylenedioxylated amphetamines were evaluated: separation and detection of underivatized analytes by (i) UV or (ii) fluorescence, (iii) derivatization with 3,5-dinitrobenzoyl chloride followed by separation and UV detection of the derivatives formed and (iv) derivatization with 9-fluorenylmethyl chloroformate (FMOC) and subsequent separation and fluorimetric detection of the derivatives. The compounds tested were 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyethylamphetamine (MDE). On the basis of these studies, a new procedure for the chromatographic determination of…