Biomedical subjects

Fernando Mauro Lanças

Publications and source records attributed to Fernando Mauro Lanças.

10 recordsLinked to original sources

PubMed2006

Stir bar sorptive extraction and liquid chromatography with UV detection for determination of antidepressants in plasma samples.

A sensitive and reproducible stir bar sorptive extraction and liquid chromatography (SBSE/LC-UV) method is described for the determination of sertraline, mirtazapine, fluoxetine, citalopram, paroxetine, imipramine, nortriptyline, amitriptyne, and desipramine in plasma samples. Important factors in the optimization of SBSE efficiency are discussed, such as extraction time, pH, ionic strength, influence of plasma proteins, and desorption conditions: solvents, modes (magnetic stir, ultrasonic), time, and number of desorption steps. The SBSE/LC-UV method showed to be linear in a concentration ranging from the limit of quantification (LOQ) to 1000.0 ng mL(-1). The LOQ values ranged from 10.0 ng mL(-1) to 40.0 ng mL(-1). The inter-day precision of the SBSE/LC-UV method presented coefficient of the variation lower than 15%. Based on figures of the merit results, the SBSE/LC-UV methodology showed to be adequate to the antidepressants analyses from therapeutic to toxic therapeutic levels. In order to evaluate the proposed method for clinical use, the SBSE/LC-UV method was applied to the analysis of plasma samples from elderly depressed patients.

Antidepressive Agents↗

PubMed2006

Solid-phase microextraction-liquid chromatography (SPME-LC) determination of fluoxetine and norfluoxetine in plasma using a heated liquid flow through interface.

A simple and sensitive procedure using solid-phase microextraction coupled with high performance liquid chromatography (HPLC) to analyze fluoxetine (FLU) and its metabolite norfluoxetine (nor-FLU) in plasma samples was developed and validated. SPME conditions were optimized employing a factorial design. The sampling step was performed using a PDMS-DVB fiber and desorption was carried out in a novel homemade heated interface. Fluoxetine and norfluoxetine were analyzed by HPLC, using a C18 Phase Sep column (150mmx4.6mm, 3microm) packed "in house", and acetonitrile:acetate buffer 25mmoll(-1) with triethylamine 25mmoll(-1) pH 4.6 (70:30) as the mobile phase. The developed method has shown precision, linearity, specificity, and limit of quantification (LOQ) adequate to assay fluoxetine and norfluoxetine in plasma. Furthermore, the results obtained using the homemade interface has shown an improvement in the desorption process when compared with the results obtained using the off-line mode.

Chromatography, High Pressure Liquid↗

PubMed2006

Exotic flora dependence of an unusual Brazilian propolis: the pinocembrin biomarker by capillary techniques.

Significant amounts of pinocembrin (>10%), a dihydroxy-flavanone, was found in the composition of an unusual brand of a subtropical Brazilian propolis. Incidentally, this sealing material was obtained from hives surrounding a large forestry site based on a single exotic flora, namely poplar (Populus sp.). Examination of the different botanical parts of poplar revealed the buds as the main source of the flavanone. Techniques used for the establishment of the chemical correlation between the propolis brand and the poplar buds were TLC/densitometry, capillary GC-MS in the e.i. mode, and CZE with DAD monitoring. Since color enhancement after Al3+ complexation applies just for more hydroxylated flavonoids, the alternative techniques herein applied were of value for pinocembrin detection and estimation. Analytical data indicated the dominance of the main phenolic pinocembrin biomarker as well as the presence of other related flavonoids in the botanical source and in the propolis derived thereof.

Aluminum↗

PubMed2006

Optimization of solid-phase microextraction procedures for the determination of tricyclic antidepressants and anticonvulsants in plasma samples by liquid chromatography.

Simple, sensitive, and reproducible off-line solid-phase microextraction and liquid chromatography (SPME/LC) methods are described for the determination of seven anticonvulsants and tricyclic antidepressants in human plasma. Factorial design and simplex methodology were applied in the optimization of the SPME procedure for tricyclic antidepressants analyses. Important factors in the SPME efficiency are discussed, such as the fiber coatings (both lab-made and commercial), extraction time, pH, ionic strength, influence of plasma proteins, and desorption conditions. The development of the lab-made fiber coatings, namely, octadecylsilane, aminosilane, and polyurethane, are further described and applied to anticonvulsants analyses. The investigated plasmatic range for the evaluated anticonvulsants, using CW-TPR fiber, were the following: phenylethylmalonamide (3.00-40.0 microg mL(-1)), phenobarbital (5.00-40.0 microg mL(-1)), primidone (3.00-40.0 microg mL(-1)), carbamazepine and carbamazepine-epoxide (2.00-24.0 microg mL(-1)), phenytoin (2.00-40.0 microg mL(-1)), and lamotrigine (0.50-12.0 microg mL(-1)). The antidepressants' linear plasmatic concentration ranged from 75.0 to 500 ng mL(-1) for imipramine, amitriptyline, and desipramine, and from 50.0 to 500 ng mL(-1) for nortriptyline, being in all cases, the limit of quantification represented by the lowest value. The precision (interassays) for all investigated drugs in plasma sample spiked with different concentrations of each analyte and submitted to the described procedures were lower than 15%. The off-line SPME/LC methodologies developed allow anticonvulsants and antidepressants analyses from therapeutic to toxic levels for therapeutic drug monitoring.

Amitriptyline↗

PubMed2006

Optimization of the SPME parameters and its online coupling with HPLC for the analysis of tricyclic antidepressants in plasma samples.

Solid-phase microextraction (SPME)-liquid chromatography (LC) is used to analyze tricyclic antidepressant drugs desipramine, imipramine, nortriptyline, amitriptyline, and clomipramine (internal standard) in plasma samples. Extraction conditions are optimized using a 2(3) factorial design plus a central point to evaluate the influence of the time, temperature, and matrix pH. A Polydimethylsiloxane-divinylbenzene (60-mum film thickness) fiber is selected after the assessment of different types of coating. The chromatographic separation is realized using a C(18) column (150 x 4.6 mm, 5-microm particles), ammonium acetate buffer (0.05 mol/L, pH 5.50)-acetonitrile (55:45 v/v) with 0.1% of triethylamine as mobile phase and UV-vis detection at 214 nm. Among the factorial design conditions evaluated, the best results are obtained at a pH 11.0, temperature of 30 degrees C, and extraction time of 45 min. The proposed method, using a lab-made SPME-LC interface, allowed the determination of tricyclic antidepressants in in plasma at therapeutic concentration levels.

Antidepressive Agents, Tricyclic↗

PubMed2005

Preparation of packed capillary columns using supercritical carbon dioxide on cyclone-type slurry reservoir.

Fused silica packed capillary columns has been prepared using a new type of reservoir designed and engineered in house. We named it "cyclone" in analogy to an industrial equipment having similar shape. The performance of these columns was evaluated using solvating gas chromatography (SGC), a particular case of the transition phase chromatography (TPC); experiments showed that high efficient columns with a reduced plate height of ca. 2.0 were obtained even using 10 microns ODS particles. The advantageous features, obtained by using the cyclone device, make the newly developed columns suitable for separations of very complex samples and trace analysis. All steps involved in the preparation of the columns are addressed and discussed.

Carbon Dioxide↗

PubMed2005

Diclofenac phonophoresis in human volunteers.

A quantitative study of sodium diclofenac (Voltaren Emulgel, Novartis) phonophoresis was undertaken in humans. Fourteen healthy human volunteers were submitted to ultrasound irradiation on two 225-cm2 areas on the dorsum (group A), followed by the application of the medication gel, and the plasma diclofenac mass was measured at 1, 2 and 3 h later by high performance liquid chromatography. The same procedure was repeated one month later with the same volunteers but with the ultrasound equipment switched off for the control group (group B). The plasma diclofenac mass was significantly higher in group A than in group B at 1 h (0.0987 microg/mL as opposed to 0.0389 microg/mL; p=0.01) and 2 h (0.0724 microg/mL as opposed to 0.0529 microg/mL; p=0.01), but not at 3 h (0.0864 microg/mL as opposed to 0.0683 microg/mL; p=0.16). The authors conclude that previously applied therapeutic ultrasound irradiation enhances the percutaneous penetration of the topical diclofenac gel, although the mechanism remains unclear.

Administration, Topical↗

PubMed2005

Analysis of complex samples by solvating gas chromatography (supercritical fluid to gas transition).

The various forms of chromatography are primarily determined by differences in the physical state of the mobile phases. The main chromatographic categories include gas chromatography (GC), liquid chromatography, and supercritical fluid chromatography. Adjusting a temperature and pressure will change the mobile phase from liquid to supercritical fluid to gas, with concomitant changes in their physical properties. In this paper, the technique transition-phase chromatography (TPC) is described. In TPC, different mobile phase conditions exist inside the column. This phase transformation within the column results in huge differences in density, solvating power, viscosity, diffusivity, and, as a consequence, in the chromatographic properties of the mobile phase. TPC experiments using capillary columns packed in our laboratory have shown that when the mobile phase is transformed from supercritical fluid to gas, high column efficiencies can be achieved. The transition from supercritical fluid to gas (also called solvating GC), a particular case of the TPC, is evaluated for the separation of complex real samples (environmental, food, and fuels).

Journal Article↗

PubMed2004

Validation of non-aqueous capillary electrophoresis for simultaneous determination of four tricyclic antidepressants in pharmaceutical formulations and plasma samples.

We present the validation of a method using non-aqueous capillary electrophoresis (NACE) for quantitative analysis of four tricyclic antidepressants (TADs) in pharmaceutical formulations and plasma. The method presented high resolution allowing the separation of the TADs in 4.3 min at optimized conditions: 50 mM ammonium acetate, 1 M acetic acid in acetonitrile, capillary with 48 cm in length, 40 cm to the detector, and voltage of 30 kV. Acceptable precision (relative standard deviation R.S.D.14.1% from plasma samples) and linearity were achieved using the internal standard (IS) method. The limits of quantification determined for plasma, after liquid-liquid extraction (LLE), were between 30 and 50 ng ml-1. These values are beyond the plasmatic therapeutic concentration. Our results were found comparable or better than those described in the literature for high performance liquid chromatography (HPLC)-based methods.

Antidepressive Agents, Tricyclic↗

PubMed2003

Multiplexed DNA sizing by capillary electrophoresis using entangled polymer solutions and diode array detection.

We developed a method for the analysis of multiplexed double-stranded DNA (dsDNA) samples complexed to various intercalating dyes using entangled polymer solution. A commercial single-column capillary electrophoresis (CE) instrument with diode array detection was used for multiplexed detection of DNA samples by addition of intercalating fluorescent molecules. A Phi X174HinfI and a pGEM DNA ladder (1 mg/mL) were used for the electrophoretic separation of dsDNA fragments ranging in size from 24 to 726 and 36 to 2645 bp, respectively. The results suggested that simultaneous electrophoretic separation of different DNA ladders multiplexed with different dyes could be performed in the same capillary yielding fast DNA sizing separations. CE analysis, which is often overpowered by slab gel in sample throughput, could now overcome this disadvantage by allowing multiplexed sample analysis in a fraction of the time needed for slab gel analysis. The separation efficiency of stained DNA molecules with both dyes were dramatically improved with buffers containing a large cation such as tetrapentylammonium ion (Npe(4) (+)) as the only cation in the buffer.

Bacteriophage phi X 174↗