Simple TLC-screening of acylglycerol levels in biodiesel as an alternative to GC determination.

Thin layer chromatography (TLC) stained with hot acidic p-anisaldehyde, is an interesting, fast, and low-cost technique to monitor main lipid contaminants such as triacylglycerols, diacylglycerols, and monoacylglycerols in biodiesel. These acylglycerols are detectable by the proposed planar chromatographic method, provided the content of the contaminants exceeds the limits recommended by the international norms applicable to biodiesel quality/specification, namely 0.25% in mass for total combined glycerin. The TLC data are confirmed by gas chromatography of the methyl esters of soy oil.

Polydimethylsiloxane/polypyrrole stir bar sorptive extraction and liquid chromatography (SBSE/LC-UV) analysis of antidepressants in plasma samples.

A new polymeric coating consisting of a dual-phase, polydimethylsiloxane (PDMS) and polypyrrole (PPY) was developed for the stir bar sorptive extraction (SBSE) of antidepressants (mirtazapine, citalopram, paroxetine, duloxetine, fluoxetine and sertraline) from plasma samples, followed by liquid chromatography analysis (SBSE/LC-UV). The extractions were based on both adsorption (PPY) and sorption (PDMS) mechanisms. SBSE variables, such as extraction time, temperature, pH of the matrix, and desorption time were optimized, in order to achieve suitable analytical sensitivity in a short time period. The PDMS/PPY coated stir bar showed high extraction efficiency (sensitivity and selectivity) toward the target analytes. The quantification limits (LOQ) of the SBSE/LC-UV method ranged from 20 ng mL(-1) to 50 ng mL(-1), and the linear range was from LOQ to 500 ng mL(-1), with a determination coefficient higher than 0.99. The inter-day precision of the SBSE/LC-UV method presented a variation coefficient lower than 15%. The efficiency of the SBSE/LC-UV method was proved by analysis of plasma samples from elderly depressed patients.

Influencia da aplicacao previa do ultra-som terapeutico na penetracao transcutanea de diclofenaco sodico em humanos sadios / The influence of the prior application of the therapeutic ultrasound on the transdermal transmission of sodium diclofenac in health humans

A influencia do ultra-som terapeutico na transmissao transcutanea de diclofenaco sodico na forma de gel topico (Voltaren Emulgel) foi investigada em 14 voluntarios sadios (10 mulheres, 4 homens, 26,4 anos de idade, 62kg de peso corporal e 1,7 m de altura, em media). O ultra-som terapeutico (modo continuo, frequencia de 1MHz, 0,5 W/cm2) foi aplicado durante 5 minutos em duas areas de 225cm2 de cada lado do dorso dos voluntarios,utilizando gel comum para acoplamento do transdutor. Em seguida, o gel comum foi removido para aplicacao de 2,5 g do gel de diclofenaco nas mesmas areas. Amostras de sangue foram coletadas imediatamente antes e 60, 120 e 180 minutos apos a aplicacao do gel de diclofenaco, a fim de analisar a massa presente no plasma dos voluntarios por meio decromatografia liquida de alta eficiencia (HPLC)

Determination of amitraz in canine plasma by solid-phase microextraction-gas chromatography with thermionic specific detection.

A simple and rapid analytical method is presented for the determination of amitraz in canine plasma samples using solid-phase microextraction (SPME) and gas chromatography with thermionic specific detection (GC-TSD). The best conditions for the SPME procedure were: direct extraction on a polydimethlysiloxane (PDMS) fiber with 100-microm film thickness; 400 µl of sample plasma matrix modified with 4 ml sodium borate solution (0.01 mol l(-1), pH 6.5); extraction temperature 70 degrees C, with stirring at 2500 rpm for 45 min. The method was linear between 20 and 400 ng ml(-1) with regression coefficients corresponding to 0.998 and coefficient of the variation of the points of the calibration curve lower than 15%. The lowest limit of quantification (LOQ) for amitraz in plasma was 20 ng ml(-1). This LOQ was determined as the lowest concentration on the calibration curve in which the coefficient of variation was lower than 15%. The proposed method was applied to determine amitraz concentrations in canine plasma to look for toxicity after treatment with amitraz in a dipping bath.

Coating of solid-phase microextraction fibers with chemically bonded silica particles: selective extraction of polycyclic aromatic hydrocarbons from drinking water samples.

In this study, solid-phase microextraction fibers coated with modified silica particles (5 pm dp) bonded to methyl (C1), hexyl (C6), octyl (C8), and polymeric octadecyl (C18) groups are prepared and evaluated. Selective extraction of polycyclic aromatic hydrocarbons (PAHs) from river water is used to demonstrate the selective behavior of the fibers as a function of the alkyl chains bonded to the silica phase. Scanning electron micrography suggests that the coating structure consists in a monolayer of particles bonded to the surface of the fiber. The behavior of the fibers upon the extraction of PAHs from water samples is compared with the use of standard polydimethylsiloxane fibers that are commercially available.

Determination of lamotrigine simultaneously with carbamazepine, carbamazepine epoxide, phenytoin, phenobarbital, and primidone in human plasma by SPME-GC-TSD.

A simple and rapid analytical method is presented for the determination of lamotrigine simultaneously with primidone, carbamazepine, carbamazepine epoxide, phenobarbital, and phenytoin in human plasma using solid-phase microextraction (SPME) and gas chromatography with thermionic specific detection. The best conditions for the SPME procedure is established as following: direct extraction on a 65-microm Carbowax-divinylbenzene fiber; 1.0 mL of a sample plasma matrix modified with 15% NaCl and 3 mL of a potassium phosphate buffer (pH 7.0); extraction temperature at 30 degrees C; and stirring at a rate of 2500 rpm for 15 min. The method shows good linearity between 0.05 and 40.0 microg/mL with regression coefficients ranging between 0.9965 and 0.9995 and a coefficient of variation of the points of the calibration curve lower than 10%. The lowest limit of quantitation for the plasma-investigated drugs varies from 0.05 to 0.20 microg/mL, according to the drug. The proposed method is sensitive enough to work into subtherapeutic and therapeutic concentrations, being that it is applied in pharmacokinetic studies and patient routine therapeutic drug monitoring.

Separation of underivatised triterpene acids by capillary supercritical fluid chromatography.

Capillary supercritical fluid chromatography with flame ionisation detection was used for the separation of some underivatised triterpene acids such as betulinic, oleanolic, polpunonic and ursolic acids. Supercritical fluid chromatography showed advantages over capillary gas chromatography since derivatisation was not required and separation was obtained in less than 15 min with high efficiency and good resolving power.

Comparison between solid-phase extraction methods for the chromatographic determination of organophosphorus pesticides in water.

A solid-phase microextraction (SPME) procedure has been developed to extract eight organophosphorus pesticides (OPs) in water and the method was compared with a conventional solid phase extraction (SPE) technique. The extracted OPs were analyzed by gas chromatography using thermionic specific detection. Both extraction methods presented linear calibration at least over the concentration range investigated (100 to 1000 ng x mL(-1) for SPE and 1 to 100 ng x mL(-1) for SPME). SPME method presented higher sensitivity than SPE. The quantitation limits were between 0.1 to 1.0 ng x mL(-1) for SPME depending upon the analyte, and 100 ng x mL(-1) for SPE. The precision, as measured by the standard deviations (RSD), were in the range 3.6% to 5.8% for SPME and 2.4% to 9.2% for SPE. Along with the feature of being a solvent - free sampling technique, SPME offers additional benefits due to its high sensitivity, simplicity, and small size sample required (typically: SPE - 500 mL, SPME - 5 mL).

An alternative supercritical fluid extraction system for aqueous matrices and its application in pesticides residue analysis.

Supercritical fluid extraction (SFE) is a rapid and convenient method for the isolation of organic compounds from environmental samples. This paper describes a supercritical carbon dioxide (CO2) extraction system that uses a newly designed extraction cell to recover organic compounds from an aqueous matrix. Analysis of the extracts by gas chromatography-electron capture detector (GC-ECD) indicated that the herbicide trifluralin (2,6-dinitro-N,N-dipropyl-4-trifluoromethylaniline) could be quantitatively extracted by using the SFE system proposed with small amounts of sample. The percentage of recovery obtained with the SFE system described was twice as high as the result obtained using a conventional solid-phase extraction technique. Extraction by SFE was completed in a short period of time using a simple and low-cost home-made system that did not require the use of organic solvents.

Analytical methods for the determination of alachlor, metolachlor, simazine and atrazine mobility in soils.

A method for the determination of the mobility of the herbicides, alachlor, metolachlor, simazine and atrazine in soil is described. The method is based on the use of soil thin-layer chromatography (TLC) and does not require the use of radiolabelled compounds. Soil on the TLC plate after development was separated into various bands, the material in each band was extracted with solvents and analyzed by gas chromatography.