0000000000329684
AUTHOR
M. Llobat-estellés
Comparative evaluation of liquid chromatography versus gas chromatography using a β-cyclodextrin stationary phase for the determination of BTEX in occupational environments
An HPLC method for the determination of benzene, toluene, ethylbenzene and o-xylene, m-xylene and p-xylene in occupational environments was developed and compared with a GC-MS method. Chromatographic analysis using a beta-cyclodextrin stationary phase was performed after active and passive air sampling by adsorption on activated charcoal and pressurized fluid extraction. The analytes were completely separated and quantified using both methods, although GC-MS provided better resolutions and lower detection limits than HPLC. The HPLC method was unsuccessfully applied to the determination of benzene in real samples because its sensitivity was too low. Both methods were applied to the analysis …
Application of pressurized fluid extraction to determine cadmium and zinc in plants
Abstract A procedure for the determination of Cd and Zn in plants is proposed. The metals are extracted by pressurized fluid extraction (PFE). Operational conditions are: pressure 1500 psi, temperature 75 °C, static time 5 min, flush volume 35%, purge time 60 s, cycles 1 and 1,2-diaminocyclohexane- N , N , N ′, N ′-tetraacetic acid (CDTA) 0.01 M at pH 4.5 as extracting solution. Determination of Zn is carried out by flame atomic absorption spectroscopy and depending on the concentration level, Cd content is determined by flame or electrothermal atomic absorption spectroscopy. Certified samples of Virginia tobacco leaves, tea leaves, spinach leaves, poplar leaves, a commercial spinach sample…
Identification and determination of amphetamine and methamphetamine in street drugs
Abstract A procedure to identify and quantify amphetamine and/or methamphetamine in street drugs is proposed. The procedure is based on the application of the ACC method (Apparent content curves method) to emission and absorption data of samples. Discrimination and quantification of amphetamine and methamphetamine in samples is carried out based on their different behavior in acid and basic medium. Potential interfering drugs are tested and the accuracy of the method is verified in prepared and real samples. Results obtained are in agreement with a HPLC procedure used as reference.
Preconcentration and speciation of chromium in waters using solid-phase extraction and atomic absorption spectrometry
Abstract A method for the preconcentration and speciation of chromium was developed. After formation of an anionic compound with ethylenediaminetetraacetic acid (CrY − ), Cr (VI) and Cr (III) are retained on a strong anionic phase (SAX) and controlled elution with 0.5 M NaCl permits their speciation. The retention and elution conditions were optimised, and interferences due to the presence of other ions such as Mg(II), Mn(II), Sn(II), Fe(III), Ba(II), Al(III), Ca(II), chloride, iodine, bromide, fluoride, sulphate, phosphate, bicarbonate and nitrate were studied. The detection limits were 0.4 μg l −1 and 1.1 μg l −1 for Cr(III) and Cr(VI), respectively, and reproducibility was 9%. The result…
Detection of bias errors in ETAASDetermination of copper in beer and wine samples
A method that evidences changes in the shape of the absorbance profiles obtained by graphite furnace atomic absorption spectrometry (ETAAS) is proposed. The method is based upon the apparent content curves model previously described for molecular spectroscopy and it permits the detection of possible sources of bias errors. Moreover, a procedure that allows to detect the existence of constant and/or proportional errors is also described. Both models has been applied to the determination of copper in wine and beer samples with and without pre-treatment of the samples. Results obtained evidence the usefulness of the proposed models.
Application of ACC method to synchronous luminiscence: determination of alpha-tocopherol and alpha-tocopheryl acetate in beverages.
A new method based on the Q parameter, that permits the determination of the C(compound A)/C(compound B) ratio without preparing calibration graphs of the two compounds, is proposed. This method has been applied to signals obtained by synchronous luminiscence. Simultaneous determination of alpha-tocopherol and alpha-tocopheryl acetate in beverages using synchronous fluorescence has been carried out. To isolate the compounds from samples, liquid extraction with n-hexane as the organic phase was employed. The presence of interferences was tested using the apparent content curves (ACC) method and the C(alpha-tocopherol)/C(alpha-tocopheryl acetate) ratio was calculated using the Q parameter. Th…
Samplers for VOCs in air based on cyclodextrin–silica hybrid microporous solid phases
Samplers for VOCs in air based on cyclodextrin-silica hybrid microporous solid phases are proposed. The solid phase preparation is very easy and inexpensive. Proposed samplers compared with other solid phases present the advantages of a wider range of operative conditions for VOCs desorption. Samplers are tested based on results for the determination of benzene, toluene, ethylbenzene and o-xylene, m-xylene and p-xylene (BTEX) in air. Operational parameters are optimized and quantitative recovery is obtained using a solid phase from 2-hydroxypropyl-β-cyclodextrin and acetonitrile as the extraction solvent. The recoveries obtained are 89 ± 4%, 90 ± 6%, 91 ± 2%, 87.0 ± 0.9%, 88 ± 4%, and 88 ± …
Determination of one compound in the presence of a single interference. Linear absorbances method
The paper exposes the theoretical and experimental principles of an analytical procedure for the determination of one compound in the presence of another with an overlapping absorption spectrum, without the need to use any standard solutions of the latter. The proposed method was applied to the determination of binary mixtures of known composition in order to assess its accuracy and precision.
Chromatographic Separation of Cresol Isomers by a β‐Cyclodextrin: Application for the Determination of Volatile Phenols in Alcoholic Beverages
Abstract The chromatographic separation of o‐cresol, m‐cresol, and p‐cresol by using β‐cyclodextrin as a chiral reagent has been studied. Conditions for the chromatographic separation of these isomers by using the cyclodextrin in the mobile phase or bonded in the stationary phase were optimized, and both procedures provided good results for the resolution of the chromatographic peaks. The use of fluorimetric detection (λexc 275 nm λem 300 nm) allows detection and quantification limits of the µg/L for eight studied phenols by using both procedures. The determination of volatile phenols in alcoholic beverages must be carried out using the cyclodextrin in the mobile phase because of the co‐elu…