Effect of volume-oriented versus flow-oriented incentive spirometry on chest wall volumes, inspiratory muscle activity, and thoracoabdominal synchrony in the elderly.

BACKGROUND: Aging causes physiological and functional changes that impair pulmonary function. Incentive spirometry is widely used for lung expansion, but the effects of volume-oriented incentive spirometry (VIS) versus flow-oriented incentive spirometry (FIS) on chest wall volumes, inspiratory muscle activity, and thoracoabdominal synchrony in the elderly are poorly understood. We compared VIS and FIS in elderly subjects and healthy adult subjects. METHODS: Sixteen elderly subjects (9 women, mean ± SD age 70.6 ± 3.9 y, mean ± SD body mass index 23.8 ± 2.5 kg/m(2)) and 16 healthy adults (8 women, mean ± age 25.9 ± 4.3 y, mean ± body mass index 23.6 ± 2.4 kg/m(2)) performed quiet breathing, VIS, and FIS in randomized sequence. Chest wall kinematics (via optoelectronic plethysmography) and inspiratory muscle activity (via surface electromyography) were assessed simultaneously. Synchrony between the superior thorax and abdominal motion was calculated (phase angle). RESULTS: In the elderly subjects both types of incentive spirometry increased chest wall volumes similarly, whereas in the healthy adult subjects VIS increased the chest wall volume more than did FIS. FIS and VIS triggered similar lower thoracoabdominal synchrony in the elderly subjects, whereas in the healthy adults FIS induced lower synchrony than did VIS. FIS required more muscle activity in the elderly subjects to create an increase in chest wall volume. CONCLUSIONS: Incentive spirometry performance is influenced by age, and the differences between elderly and healthy adults response should be considered in clinical practice.

Use of vancomycin silica stationary phase in packed capillary electrochromatography. II. Enantiomer separation of venlafaxine and O-desmethylvenlafaxine in human plasma.

A capillary electrochromatography method, using vancomycin chiral stationary phase packed capillary, was optimized for the simultaneous chiral separation of the antidepressant drug venlafaxine and its main active metabolite O-desmethylvenlafaxine. Simultaneous baseline enantiomeric separation of the two compounds was obtained using a mobile phase composed of 100 mM ammonium acetate buffer pH 6/water/acetonitrile (5:5:90, v/v). The electrokinetic injection for sample introduction provided a limit of quantitation for both the compounds of 0.05 microg/ml racemate concentration suitable for the analysis of venlafaxine and metabolite in biological samples. The acetonitrile mobile phase concentration was found to modulate the analytes elution times, the enantiomeric resolution and the efficiency of the separation. The column was tested for repeatability and linearity showing RSD values (%) in the range of 0.13-0.24, 2.47-3.66 and 1.35-2.50 for migration time, sample/internal standard peak area ratio and enantiomeric resolution, respectively and correlation coefficients higher than 0.9990. The method was applied to the analysis of clinical samples of patients under depression therapy showing a stereoselective metabolism for venlafaxine.

Rosacea: tratamiento con vitamina K topica / Rosacea: vitamin K therapy

La rosácea es una dermopatía que afecta selectivamente la cara, caracterizada por la aparición sucesiva o simultánea de eritema, telangiectasias, pápulas y pústulas, siendo el eritema su sustrato obligado y las dilaciones vasculares una etapa de comienzo. Se realiza un ensayo terapéutico con vitamina K en forma de máscara y en crema para uso diario con una respuesta eficaz en la disminución del eritema(AU)

Rosacea: tratamiento con vitamina K topica / Rosacea: vitamin K therapy

La rosácea es una dermopatía que afecta selectivamente la cara, caracterizada por la aparición sucesiva o simultánea de eritema, telangiectasias, pápulas y pústulas, siendo el eritema su sustrato obligado y las dilaciones vasculares una etapa de comienzo. Se realiza un ensayo terapéutico con vitamina K en forma de máscara y en crema para uso diario con una respuesta eficaz en la disminución del eritema

Use of vancomycin silica stationary phase in packed capillary electrochromatography I. Enantiomer separation of basic compounds.

Chiral separation of basic compounds was achieved by using 75 or 100 microm ID fused-silica capillaries packed with a vanoomycin-modified diol silica stationary phase. The capillary was firstly packed for about 12 cm with a slurry mixture composed of diolsilica (3:1) then with the vancomycin modified diol-silica (3:1) (23 cm), and finally with diol-silica (3:1) for about 2 cm. Frits were prepared by a heating wire at the two ends of the capillary; the detector window was prepared at 8.5 cm from the end of the capillary where vancomycin was not present. The influence of the mobile phase composition (pH and concentration, organic modifier type and concentration) on the velocity of the electroosmotic flow, chiral resolution and enantioselectivity was studied. Good enantiomeric resolution was achieved for atenolol, oxprenolol, propranolol, and venlafaxine using a mobile phase composition of 100 mM ammonium acetate solution (pH 6)/water/acetonitrile (5:5:90 v/v/v) while for terbutaline a mixture of 5:15:80 v/v/v provided the best separations. The use of methanol instead of acetonitrile caused a general increase of enantiomer resolution of the studied compounds together with a reduction of efficiency and detector response. However, the combination of acetonitrile and methanol in the mobile phase (as, e.g., 10% methanol and 80% acetonitrile) allowed to improve the enantiomer resolution with satisfactory detector response.

Capillary electrochromatography and capillary electrochromatography-electrospray mass spectrometry for the separation of non-steroidal anti-inflammatory drugs.

In this study capillary electrochromatography (CEC) was utilized for the separation of ten non-steroidal anti-inflammatory drugs (NSAIDs). Experiments were carried out in a commercially available CE instrument using a packed capillary with RP-18 silica particles where the stationary phase completely filled the capillary. The mobile phase consisted of a mixture of ammonium formate buffer pH 2.5 and acetonitrile. Selectivity and resolution were studied changing the pH and the concentration of the buffer, the acetonitrile content mobile phase and the capillary temperature. The optimum experimental conditions for CEC separation of the studied drug mixture were found using 50 mM ammonium formate pH 2.5-acetonitrile (40:60) at 25 degrees C. The CEC capillary was coupled to an electrospray mass spectrometer for the characterization of the NSAIDs. A mobile phase composed by the same buffer but with a higher concentration of acetonitrile (90%) was used in order to speed up the separation of analytes.

Lipomatosis de Madelung: revision del tema a proposito de un caso / Madelung lipomatosis: rewiew of the current literature apropos of one case

La lipomatosis de Madelung o Lipomatosis simétrica múltiple, es una enfermedad poco frecuente, caracterizada por la presencia de lipomas no encapsulados, localizados en cuello y mitad superior de tronco. La patogenia estaría relacionada con un defecto a nivel de las catecolaminas que inducen la lipólisis. Esta patología la encontramos frecuentemente asociada al alcoholismo, hepatopatías y tumores malignos. En este artículo presentamos un caso clásico de lipomatosis de Madelung y una revisión del tema(AU)

Lipomatosis de Madelung: revision del tema a proposito de un caso / Madelung lipomatosis: rewiew of the current literature apropos of one case

La lipomatosis de Madelung o Lipomatosis simétrica múltiple, es una enfermedad poco frecuente, caracterizada por la presencia de lipomas no encapsulados, localizados en cuello y mitad superior de tronco. La patogenia estaría relacionada con un defecto a nivel de las catecolaminas que inducen la lipólisis. Esta patología la encontramos frecuentemente asociada al alcoholismo, hepatopatías y tumores malignos. En este artículo presentamos un caso clásico de lipomatosis de Madelung y una revisión del tema

Separation and identification of etodolac and its urinary phase I metabolites using capillary electrochromatography and on-line capillary electrochromatography-electrospray ionisation mass spectrometry coupling.

Capillary high-performance liquid chromatography (capillary HPLC), pressure-assisted capillary electrochromatography (pCEC) and capillary electrochromatography (CEC) were performed in the same capillary packed with 5 microm octadecylsilica (C18) as stationary phase. These three separation modes were compared from the viewpoint of peak efficiency and separation selectivity in order to critically evaluate the advantages which CEC may offer compared to capillary HPLC for the solution of practical biomedical problems. The separation of the non-steroidal anti-inflammatory drug etodolac (ET, 1) and its phase I metabolites, 6-hydroxy etodolac (6-OH-ET, 2), 7-hydroxy etodolac (7-OH-ET, 3) and 8-(1'-hydroxyethyl) etodolac (8-OH-ET, 4) was selected as an example. Baseline separation of all compounds was achieved in different modes and conditions. The effect of pure electrophoretic separation mechanism on the overall separation selectivity observed in CEC has been shown. A high electroosmotic flow (EOF) was observed in C18 packed capillary even at pH 2.5 in various buffers. Furthermore, these separations were coupled on-line with electrospray ionisation mass spectrometry (ESI-MS) and the parent drug and its metabolites were identified in urine. For the coupling of CEC with ESI-MS a laboratory-made electrophoretic device was used in order to overcome some technical disadvantages of commercial instrumentation.

Analysis of hydroquinone and some of its ethers by using capillary electrochromatography.

Capillary electrochromatography (CEC) was used for the analysis of relevant compounds in cosmetic preparation. Hydroquinone (HQ) and some of its ethers (methyl-, dimethyl-, benzyl-, phenyl-, propyl-HQ derivatives) were analyzed by using an octadecylsilica (ODS) stationary phase packed in fused-silica capillary (100 microm I.D.; 30 cm and 21.5 cm total and effective lengths, respectively). 20 mM Ammonium acetate pH 6-acetonitrile (50-70%) were the mobile phases used for the experiments. The acetonitrile (ACN) content strongly influenced the resolution of the studied compounds as well as the efficiency and the retention factor. Baseline resolution for the studied analytes was achieved at both the lowest and the highest percentage of ACN, the last one providing the shortest analysis time. Mobile phase containing 70% of ACN was therefore used for the analysis of an extract of skin-toning cream declared to contain HQ. Good repeatability of both retention times, peak areas and peak areas ratio (Asample/Ainternational standard) was found. The calibration graphs were linear in the concentration range studied (5-90 microg/ml) with correlation coefficients between 0.9975 and 09991. The analysis of the cosmetic preparation revealed the presence of HQ (1.72%, w/w) and of two additional peaks (not identified).

Enantiomeric separation of fluoxetine and norfluoxetine in plasma and serum samples with high detection sensitivity capillary electrophoresis.

A capillary electrophoresis method was optimized for the stereoselective analysis of the antidepressant drug fluoxetine and its main demethylated metabolite norfluoxetine using a cyclodextrin-modified sodium phosphate buffer at pH 2.5. The combination of a neutral and a negatively charged cyclodextrin, dimethylated-beta- and phosphated-gamma-respectively, provided the baseline enantiomeric separation of the two compounds. The very low concentrations of chiral selectors employed together with the use of a high sensitivity detection cell of special design (zeta-shaped) in a diode array UV detector allowed us to reach a limit of detection of 0.005 and 0.01 microg/mL for fluoxetine and norfluoxetine, respectively. Analysis of fluoxetine and norfluoxetine standard mixtures showed a reproducibility of migration times and peak area and linearity in the concentration range of 0.1-2.0 microg/mL. The optimized method was applied to the analysis of clinical serum and plasma samples of patients under depression therapy. In all the analyzed samples the enantiomeric forms of fluoxetine and norfluoxetine were easily identified. The fluoxetine and metabolite enantiomeric ratio confirmed the stereoselectivity of the metabolic process of the fluoxetine drug in accordance with the literature data.

Enantioresolution of pharmaceutical compounds by capillary electrophoresis. Use of cyclodextrins and antibiotics.

Capillary electrophoresis (CE) is a powerful tool for the analysis of chiral compounds of pharmaceutical interest. The separation of enantiomers can be achieved using a chiral environment responsible for the diastereoisomers formation (stable or labile in the indirect or direct separation method, respectively). A wide number of chiral selectors have been employed in CE and among them cyclodextrins or their derivatives and antibiotics are the most used stereoselective agents. The review surveys the chiral separation of drugs using the above mentioned chiral selectors by CE. The main parameters influencing the enantioresolution, e.g., chiral selector type and concentration, buffer type, concentration, pH, organic modifier as well as the capillary temperature are discussed. Finally some selected applications to real samples such as pharmaceutical formulations, serum, urine are also discussed.

Stereoselective analysis of acid herbicides in natural waters by capillary electrophoresis.

A capillary electrophoretic method for the stereoselective analysis of aryloxypropionic and aryloxyphenoxypropionic acidic herbicides in ground water and river water was performed. Vancomycin and gamma-cyclodextrin were added to the background electrolyte (BGE) as chiral selectors. Water sample preconcentration was accomplished by solid-phase extraction on styrene-divinylbenzene packed cartridges (2 L of ground water and 1 L of river water). The analytical method allowed for the resolution of mecoprop, fenoprop, fluazifop and haloxyfop racemic mixtures in natural water samples spiked with enantiomer concentration levels in the range 0.1-0.13 ppb for ground water and 0.4-0.54 ppb for river water.

Simultaneous stereoselective analysis by capillary electrophoresis of tramadol enantiomers and their main phase I metabolites in urine.

Capillary zone electrophoresis was successfully applied to the enantiomeric resolution of racemic tramadol and its six phase I metabolites using carboxymethylated beta-cyclodextrin (CMB) added to the background electrolyte (BGE). Baseline resolution of tramadol and its metabolites was obtained in less than 30 min using a 50 mM phosphate buffer (pH 2.5) containing 5 mM of CMB. Chiral determinations of tramadol and its main three metabolites, O-demethyltramadol (M1), N-demethyltramadol (M2) and O-demethyl-N-demethyltramadol (M5), were performed in urine after a simple double liquid-liquid extraction of 200 microliters of biological material. In the tested concentration range (0.5-20 micrograms/ml, except for M2: 0.5-10 micrograms/ml) coefficients of correlation superior than 0.994 were obtained. Within-day variation determined on three different concentrations for each enantiomers showed accuracies ranging from 95.4% to 103.2%. The relative standard deviation (RSD) of these assays was determined to be less than 10.0%. Day-to-day variation presented accuracies ranging from 96.3% to 106.5% with a RSD less than 9.0%. After oral administration of 100 mg of tramadol hydrochloride to an healthy volunteer, the urinary excretion was monitored during 30 h. About 15% of the dose was excreted as unchanged tramadol. The enantiomeric ratios of all the excreted analytes, T, M1, M2 and M5, were found to be very different to 1.0, showing that a stereoselective metabolism of tramadol clearly occurred.

A new electrode chamber for stable performance in capillary electrophoresis.

Prerequisite to running automated sequences of analyses in capillary electrophoresis is a stable performance of the system. The products of the electrode reaction with the running background electrolyte (BGE) may play an important role, since even the neutral products may be driven into the capillary by electroosmosis and may severely deteriorate the stability of the baseline. Here, a simple, inexpensive, and fast procedure is described for improving the stability of the performance of capillary electrophoresis using a modified vial serving as the electrode chamber for the running BGE. The modification is based on creating two separate rooms in the vial, one for the electrode and a second one for the capillary. These two rooms are connected by a cotton plug. When both rooms are filled with the running BGE, the electrolytic connection between the electrode and the capillary is ensured; however, the convective transport of the electrode reaction products into the capillary is practically eliminated.

Investigation of the in vitro biotransformation of R-(+)-thalidomide by HPLC, nano-HPLC, CEC and HPLC--APCI-MS.

High-performance liquid chromatography (HPLC), nano-HPLC, capillary electrochromatography (CEC) and on-line HPLC-atmospheric pressure chemical ionization mass spectrometry (APCI-MS) techniques were used for the identification and detailed characterization of two new metabolites of the former sedative drug thalidomide (TD). The advantages of nano-HPLC and CEC are higher peak efficiency and a drastic decrease in the analysis time, which, together with lower sample dilution during the analyses, allowed to obtain a detection sensitivity that was comparable to HPLC with common-sized columns. Both, nano-HPLC and CEC could be realized in the commercially available capillary electrophoresis system HP3D. On-line HPLC-APCI-MS coupling is a very useful technique for the rapid identification of metabolites without any need for reference compounds.

Use of cyclodextrins in capillary electrophoresis: resolution of tramadol enantiomers.

Capillary zone electrophoresis was successfully applied to the enantiomeric resolution of racemic tramadol. Both uncoated and polyacrylamide-coated capillaries were tested for method optimization using either negatively charged or native cyclodextrins (CD) added to the background electrolyte (BGE). The resolution was strongly influenced by the CD type and concentration as well as by the pH and the concentration of the BGE. Among the CDs tested, carboxymethylated-beta-cyclodextrin allowed the baseline separation of tramadol enantiomers. After the method was optimized, it was validated in a coated capillary for enantiomeric analysis of tramadol enantiomers in pharmaceutical formulation, including specificity and elution order, linearity, accuracy and precision, determination of limit of detection (LOD) and quantification (LOQ), enantiomeric purity linearity, freedom from interference, and stability of sample solutions. Precision at the target concentration was less than 2%, with an accuracy higher than 99%. Furthermore, the method was able to detect 0.3% and to quantify 1% of the minor enantiomer in the presence of the major one at the target value.

Quantitative analysis of synthetic dyes in lipstick by micellar electrokinetic capillary chromatography.

The separation of synthetic dyes, used as color additives in cosmetics, by micellar electrokinetic capillary chromatography (MEKC) is described in this study. The separation of seven dyes, namely eosine, erythrosine, cyanosine, rhodamine B, orange II, chromotrope FB and tartrazine has been achieved in about 3 min in an untreated fused silica capillary containing as background electrolyte a 25 mM tetraborate/phosphate buffer, pH 8.0, and 30 mM sodium dodecyl sulfate. The electrophoretic method exhibits precision and relatively high sensitivity. A detection limit (LOD, signal/noise = 3) in the range of 5-7.5 X 10(-7) M of standard compounds was recorded. Intra-day repeatability of all the studied dye determinations (8 runs) gave the following results (limit values), % standard deviation: 0.24-1.54% for migration time, 0.99-1.24% for corrected peak areas, 0.99-1.24% for corrected peak area ratio (analyte/internal standard) and 1.56-2.74% for peak areas. The optimized method was successfully applied to the analysis of a lipstick sample where eosine and cyanosine were present.

Use of a Hepta-tyr glycopeptide antibiotic as chiral selector in capillary electrophoresis.

A new glycopeptide antibiotic, MDL 63,246 (Hepta-tyr), of the teicoplanin family, has been evaluated in capillary electrophoresis for the resolution of chiral compounds of pharmaceutical and environmental interest. Electrophoretic separations were carried out in a polyacrylamide-coated capillary using the partial filling-counter current mode with aqueous-organic buffers in the pH range 4-6. Experimental parameters affecting resolution, such as antibiotic concentration, buffer pH, organic modifier type and capillary temperature, were studied. The Hepta-tyr antibiotic exhibited a high enantiorecognition capability towards the studied compounds at very low concentrations (1-2 mg/mL). The optimum experimental conditions were achieved by using a buffer at pH 5 containing acetonitrile at 25 degrees C.

Chiral analysis by capillary electrophoresis using antibiotics as chiral selector.

The separation of chiral compounds by capillary electrophoresis (CE) is a very interesting field of research in different areas such as pharmaceutical, environmental, agricultural analysis etc. The separation of two enantiomers can be achieved in CE using a chiral environment interacting with the two analytes on forming diastereoisomers with different stability constants and thus different mobilities. A wide number of chiral selectors have been employed in CE and among them glycopeptide antibiotics exhibited excellent enantioselective properties towards a wide number of racemic compounds. Vancomycin, ristocetin A, rifamycins, teicoplanin, kanamycin, streptomycin, fradiomycin, and two vancomycin analogues, added to the background electrolyte (BGE), are the antibiotics studied by CE running the separation in untreated and/or coated fused-silica capillary. Due to adsorption and absorption phenomena, some drawbacks can be expected when using bare fused-silica capillary, e.g., changes of electroosmotic flow (EOF), broaden peaks, reduced efficiency and low sensitivity. Coated capillary and counter current mode can be the solution to overcome the above mentioned problems. This review surveys the separation of enantiomers by CE when macrocyclic antibiotics are used as chiral selector. The enantioselectivity can be easily controlled modifying several parameters such as antibiotic type and concentration, pH, ionic strength and concentration of the background electrolyte, organic modifier etc. The paper also presents a list of the latest chiral separations achieved by CE where antibiotics were used as chiral selector.