Biomedical subjects

Ana M Afonso

Publications and source records attributed to Ana M Afonso.

7 recordsLinked to original sources

PubMed2006

Optimization of an analytical methodology for the determination of alkyl- and methoxy-phenolic compounds by HS-SPME in biomass smoke.

A sampling and analysis method for the determination of 21 phenolic compounds in smoke samples from biomass combustion has been developed. The smoke is used to make smoked foods, following an artisanal procedure used in some parts of the Canary Islands. The sampling system consists of a Bravo H air sampler, two impingers, each one containing an aqueous solution of sodium hydroxide 0.1 mol L(-1), followed by a silica gel trap. The variables optimized to reach the best sampling conditions were volume of absorbent solution and sampling flow. Under the optimum conditions, 100 mL of absorbent solution of NaOH 0.10 mol L(-1) and 2 L min(-1) for the sampling flow, sampling efficiencies are higher than 80%. Analysis of phenolic compounds was carried out by headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). Five different fiber coatings were employed in this study. By means of a central composite design, extraction time, salt concentration, and pH of the solution were optimized: 65-microm carbowax-divinylbenzene, extraction time 90 min, concentration in NaCl of 35% (m/v), and pH 2 yielded the highest response. Detection limits of phenol and their alkyl derivatives, guaiacol and eugenol, are between 1.13 and 4.60 ng mL(-1). 3-Methoxyphenol, 2,6-dimethoxyphenol, and vanillin have detection limits considerably higher. Good linearity (R2 > or = 0.98) was observed for all calibration curves in the established ranges. The reproducibility of the method (RSD, relative standard deviation) was found to oscillate between 7 and 18% (generally close or lower than 10%).

Biomass↗

PubMed2005

Study of the interactions between phenolic compounds and micellar media using micellar solid-phase microextraction/gas chromatography.

Solid-phase microextraction coupled to gas-chromatography with mass-spectrometry detection has been employed to establish the sensitivity indexes as well as to study the partition coefficients of phenols into ionic and nonionic micelles. The sensitivity indexes values can be used to estimate qualitatively the affinity between phenols and micelles. The studied phenols, some of them with high environmental interest, include chloro-, alkyl-, and methoxy-phenols. The results obtained in this work, using 85 microm polyacrylate fiber and anionic (sodium dodecyl sulphate), cationic (cetyltrimethylammonium bromide), and nonionic (Triton X-100 and polyoxyethylene-10-lauryl ether) surfactants, indicate that SPME is a viable method for estimating the micelle partition coefficients.

Chromatography, Gas↗

PubMed2005

Coupling micelle-mediated extraction using mixtures of surfactants and fluorescence measurements with a fiber-optic for the screening of PAHs in seawater.

The screening of PAHs from seawater samples using cloud-point extraction (CPE) as a step prior to their determination by fluorescence measurements with a fiber-optic is proposed. The CPE is carried out with the nonionic surfactants mixture POLE and Brij 30. The fluorescence measurement parameters were optimized, allowing selection of benzo(a)pyrene (B(a)Py) and benzo(k)fluoranthene (B(k)Ft) as the target analytes for the screening. The reproducibility of the whole screening system, expressed as relative standard deviation, was 9.0% for B(a)Py and 12.1% for B(k)Ft (both for n = 7). The reliability of the method was established at five concentrations for B(a)Py (between 0.5 and 3.3 times the detection limit: 0.31 ng ml(-1)) and at three concentrations for B(k)Ft (between 0.6 and 2.5 times the detection limit: 0.56 ng ml(-1)). The resolution of binary mixtures of these PAHs at different levels of concentration, and a study of the interferences with the rest of the PAHs were also carried out.

Fiber Optic Technology↗

PubMed2005

Polycyclic aromatic hydrocarbons in smoke used to smoke cheese produced by the combustion of rock rose (Cistus monspeliensis) and tree heather (Erica arborea) wood.

In this work, the polycyclic aromatic hydrocarbons (PAHs) and their methyl derivatives concentrations have been determined in smoke from the rock rose and tree heather wood combustion. The combustion is done in two types of smokers, kiln and drum, commonly used in the Canary Islands (Spain) to smoke cheese. The low control of the operational conditions justify the great variability of the PAHs concentration in the emissions, with values between 251.8 and 2547 microg/m3N. In general, the lowest concentrations correspond to the tree heather wood combustion in the drum, while the highest concentrations are usually reached in the rock rose wood combustion in the kiln. However, the relative contributions of each PAH to the total concentration are independently similar to the type of smoker and wood used. In the combustion conditions, the equilibrium is not reached during the PAHs distribution process between the gas and aerosol phases. Therefore, while naphthalene and their 1- and 2-methyl derivatives remain in the gas phase, phenanthrene and PAHs with higher molecular weight remain mainly in the aerosol phase. In this phase, the PAHs concentration represents 39.9% of the total PAHs produced by burning rock rose wood and 29.1% of the total PAHs when tree heather wood is used. To establish the carcinogenic potential in both phases, the percentages of some PAHs were calculated. These values are significantly higher in the aerosol phase and, at the same time, higher when rock rose wood is used.

Aerosols↗

PubMed2004

Solid-phase microextraction coupled to gas chromatography/mass spectrometry for determining polycyclic aromatic hydrocarbon-micelle partition coefficients.

Solid-phase microextraction (SPME) coupled to gas chromatography with MS detection has been employed to study the partition coefficients of PAHs to ionic and nonionic micelles. The results obtained in this work for seven PAHs, using 85-microm polyacrylate- and 100-microm poly(dimethylsiloxane)-coated fibers and anionic (sodium dodecyl sulfate), cationic (cetyltrimethylammonium bromide), and nonionic (polyoxyethylene-10-lauryl ether) surfactants, indicate that SPME is a viable method for estimating the partition coefficients of PAHs to micelle. The procedure could also be potentially extended to the measurement of partition coefficients between a wide variety of semi- or nonvolatile compounds and micellar media.

Anions↗

PubMed2004

Solid-phase microextraction coupled with high-performance liquid chromatography for the analysis of heterocyclic aromatic amines.

Solid-phase microextraction (SPME) coupled with high-performance liquid chromatography (HPLC) with UV diode array detection (DAD) for the analysis of heterocyclic aromatic amines (HAs) is described. Four kinds of fiber coatings: Carbowax-templated resin (CW-TPR), Carbowax-divinylbenzene (CW-DVB), poly(dimethylsiloxane)-divinylbenzene (PDMS-DVB) and polyacrylate (PA) were evaluated for extraction of nine most biologically active heterocyclic aromatic amines. Different parameters affecting to the microextraction and determination of HAs were studied, such as absorption and desorption time, desorption mode, composition of the solvent for desorption, pH, ionic strength, and percentage of methanol in the sample. To determine these amines in food samples a new simplified procedure is proposed, consisting of treatment of the sample with methanolic NaOH prior microextraction by CW-TPR fiber coating and HPLC-DAD determination. The advantages of this new method are the reduced amounts of time and organic solvents required.

Amines↗

PubMed2002

Fast microwave-assisted dansylation of N-nitrosamines. Analysis by high-performance liquid chromatography with fluorescence detection.

A fast microwave-assisted dansylation procedure has been developed for the derivatization of N-nitrosamines prior to high-performance liquid chromatography determination. N-Nitrosomorpholine, N-nitrosodimethylamine, N-nitrosodiethylamine, N-nitrosopyrrolidine and N-nitrosopiperidine are first denitrosated by hydrobromic acid-acetic acid to produce secondary amines, which are then quantitatively dansylated in 5 min using radiation power of 378 W and a maximum pressure of 1.4 bar inside the reactor. The reaction mixture is separated on a C18 column with acetonitrile-water (55:45, v/v) as mobile phase with fluorimetric detection at 531 nm (excitation at 339 nm). The detection limits range from 8 to 75 pg for N-nitrosomorpholine and N-nitrosodiethylamine, respectively. The method was applied to study the recoveries of N-nitrosamines in beer and their determination in cigarette smoke.

Chromatography, High Pressure Liquid↗