0000000000646295
AUTHOR
P. Campíns Falcó
showing 14 related works from this author
Generalised H-point standard addition method for the isolation of the analyte signal from the sample signal when coelution of unknown compounds occur…
1999
The generalised H-point standard addition method (GHPSAM) is proposed for isolating the analytical signal of an analyte from the signal of an unknown sample. Samples containing two and three coeluting compounds have been analysed. The accuracy of the predictions depends on the shape of the analyte and interferent spectra but not on the degree of chromatographic overlap. This methodology involves the location of linear intervals for the unknown interference spectrum from the spectrum of the sample. Once the linear interval has been found the selection of three wavelengths within the interval will allow the cancellation of the signal of the unknown interferent. The method has been applied to …
Determination of ammonia and primary amine compounds and Kjeldahl nitrogen in water samples with a modified Roth's fluorimetric method.
2005
Abstract A method for the simultaneous determination of primary amino groups and ammonium ion has been proposed. The method is based in solution derivatization with o-Phthaldialdehyde/N-acetyl-cisteine (OPA/NAC) and fluorescence measurement of the formed isoindols. Analytical characteristics and description of the developed procedure have been provided. The calibration graphs for ammonium (up to 1.44 mg L−1 of N) and methylamine as primary amino model compound (up to 0.282 mg L−1 of N), were obtained. Bivariate and multivariate calibration models have been tested. The limits of detection were 0.07 mg L−1 of N and 0.004 mg L−1 of N for ammonium and amine, respectively. The procedure was firs…
Rapid fluorimetric assay for primary amine groups in water samples
2003
Bond Elut C(18) solid-phase extraction cartridges were used for pre-concentration followed by derivatization with o-phthaldialdehyde-N-acetylcysteine (OPA-NAC) of primary amines in water. Optimal conditions were: conditioning the cartridges with borate buffer pH 10.4, retention of the primary amines, addition of the OPA-NAC(3.7 mmol L(-1)) 1:1 molar ratio and borate buffer pH 8, elution of the isoindol with MeOH-borate buffer (9:1) pH 10.2 and fluorescence measurement. The equations of the calibration graphs for methylamine, ethylamine, propylamine, butylamine, pentylamine, and beta-phenylethylamine at lambda(excitation)=330 nm and lambda(emission)=440 nm, in the optimal conditions are pres…
Kinetic-Spectrophotometric Determination of Primary and Secondary Amines by Reaction with 1-2 Naphthoquinone-4-Sulphonate.
1994
Abstract A kinetic-spectrophotometric method for the determination of primary and secondary amines is described. It is based on the coloured reaction of these amines with sodium 1,2 Naphthoquinone 4-sulphonate (NQS) in the presence of a non-ionic surfactant. For each determination the optimum conditions were studied and found to be as follows: pH 10.5. Carbonate-bicarbonate buffer 0.1M, Triton X-100 0.1%, Temperature 45°C, and NQS 6.4 × 10−3 M and interval of time 45–180s at wavelength 490 nm. The parameters used for the quantitative determinations are the reaction rate and the increase in the absorbance of the kinetic curves. This procedure has been applied to the determination of ephedrin…
A chemometric study of the simultaneous determination of calcium and magnesium in natural waters
1999
A method for the simultaneous spectrophotometric determination of calcium and magnesium in mineral waters with an FIA system is tested. The method is based on the reaction between the analytes and arsenazo(III) at pH 8.5. The calculations of the amounts of both analytes in the samples are carried out with the H-point standard addition method (HPSAM) for ternary mixtures, and with a partial least squares (PLS) model after a proper variable selection. The results obtained for the determination of calcium were comparable using both methods. The employment of the HPSAM brings to our attention the influence of the calcium concentration in the sample to the development of the reaction between mag…
Spectrophotometric determination of chlorhexidine with bromocresol green by flow-injection and manual methods
1986
Abstract A spectrophotometric study of the chlorhexidine/bromocresol green/Triton X-100 system is reported; at pH 5.3, both 2:1 and 1:1 bromocresol green/chlorhexidine complexes are formed. In the manual spectrophotometric method, Beer's law is obeyed for chlorhexidine concentrations of 2.9–32.2 μg ml −1 (r.s.d. 0.4–1.3%); the molar absorptivity is 12 500 l mol −1 cm −1 . In the flow-injection method, the calibration graph is linear for the chlorhexidine range 23.0–83.9 μg ml −1 (r.s.d. 0.8%); the injection is ca. 60 h −1 . Benzocaine, acetylsalicylic acid, ascorbic acid and sucrose are tolerated at 10 −2 −10 −3 M levels. Hibitane 5% was analyzed successfully.
Sensitive determination of aliphatic amines in water by high-performance liquid chromatography with chemiluminescence detection.
2004
A sensitive method has been developed for liquid chromatographic determination of short aliphatic amines in water samples. Analytes are preconcentrated and dansylated on solid sorbents (C18 solid-phase extraction cartridges). The dansyl derivatives are chromatographed and post-column mixed with peroxyoxalate (TCPO) and H2O2 in order to perform chemiluminescence detection. Optimal results have been obtained using a sample volume of 5 ml. The method has been applied to the quantification or screening of several aliphatic amines: methylamine, ethylamine, butylamine, diethylamine, pentylamine and hexylamine. The screening procedure has been developed including also polyamines (putrescine, cadav…
Evaluation of C18 adsorbent cartridges for sampling and derivatization of primary amines in air
2004
Abstract The sampling efficiency of C18 solid-phase extraction cartridges was investigated for methylamine, ethylamine, propylamine, butylamine and pentylamine, in air. Determination of these analytes was based on derivatization with o-phthaldialdehyde–N-acetylcysteine (OPA–NAC) on the solid support and fluorescence detection at λexcitation=330 nm and λemission=440 nm of the eluted derivatives. The calibration model derived from aqueous standards was statistically comparable with the calibration model for air standards. Aqueous amines can be used as standards. The method was useful for calculating short-term exposure limits (STEL). A sampling time of 15 min at 30 ml min−1 was employed. Good…
Analysis of primary aliphatic short-chain monoamines by LC in water samples
2003
Abstract Several derivatization procedures with o-phthaldialdehyde-N-acetylcysteine (OPA-NAC) were compared for a rapid analysis of primary aliphatic short-chain monoamines in water samples by HPLC using a LiChorospher analytical separation column (100RP18 125 mm ×4 mm i.d., 5 μm). Both the solution and the solid-support assisted off-line derivatization on C18 SPE cartridges were inadequate options because of beginning degradation processes of the instable isoindol derivatives during their transfer to the analytical column. This problem was precluded with the on-column or solid-support assisted on-line derivatization. In the last mentioned procedure, the derivatization took place in a Hype…
Creatinine determination in urine samples by batchwise kinetic procedure and flow injection analysis using the Jaffé reaction: chemometric study
2001
The classical Jaffé reaction for the determination of creatinine in urine samples is tested. A comparative study of the main analytical characteristics focussed to minimize the bias error and improve the precision, for the batchwise and flow injection (FI) methods is realized. Also, the effect of the albumin concentration in the determination of creatinine has been studied. Different analytical signals were studied. Absorbance increments at different times permit to estimate the creatinine concentration free from bias error in urine by the batchwise method using the calibration graph obtained with creatinine standards and no measurement of the blank solution is needed. The lineal interval w…
Amphetamine and methamphetamine determination in urine by reversed-phase high-performance liquid chromatography with sodium 1,2-napthoquinone 4-sulfo…
1995
A rapid method is described for the identification and determination of amphetamine and methamphetamine in human urine samples by liquid chromatography with UV-Vis detection. The samples were transferred onto a C18 solid-phase extraction column and chromatographed on a Hypersil ODS RP C18, 5 microns (250 x 4 mm I.D.) with an acetonitrile-water elution gradient containing propylamine. Under these conditions, the amines are eluted with a short retention time. The procedure has been applied to the determination of amphetamine and methamphetamine in the range 0.3-4.0 micrograms/ml in spiked urine samples. The detection limits at 280 nm were 4 and 2 ng/ml for amphetamine and methamphetamine, res…
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 …
Determination of triamterene in urine by HPLC using fluorescence detection and column-switching
1994
A liquid chromatographic method incorporating column-switching and fluorimetric detection for the determination of triamterene in untreated urine, is described. The urine samples (5 μL) were directly introduced onto an Hypersil ODS-C18, 30 μm (20 mm×2.1 mm I.D.) pre-column. Polar urinary compounds were removed by flushing the pre-column with water for 1 min, and the analyte was then switched onto an HP-LiChrospher RP C18,5 μm (125 mm×4mm ID) analytical column using an acetonitrile/phosphate buffer gradient elution. Fluorescence detection was performed at 230 nm excitation and 430 nm emission wavelengths. The recovery of drug was 102±2% in the 0.10–20.0 μg/mL concentration range, the limit o…
Determination of methamphetamine in urine samples with sodium 1,2-naphthoquinone-4-sulphonate
1994
Optimal conditions have been studied for the determination of methamphetamine in urine samples by an extractive-spectrophotometric method with sodium 1,2-naphthoquinone-4-sulphonate (NQS) as reagent. These conditions are: NaHCO3 pH 10, NQS 6.3 × 10−3 mol/l and heating for 5 min at 45°C. The accuracy and precision of the method were tested. The detection limits were 0.2 mg/l in the standard and 0.9 mg/l when 5 ml of urine sample were taken. The standard deviation of blank urine was evaluated from 12 different samples. The relative errors found in the determination of methamphetamine in urine were lower than 10% if the methamphetamine-amphetamine ratio was higher than 4.