Enantioselective analysis of disopyramide and mono-N-dealkyldisopyramide in plasma and urine by high-performance liquid chromatography on an amylose-derived chiral stationary phase.

An enantioselective high-performance liquid chromatography method was developed for the simultaneous determination of disopyramide (DP) and mono-N-dealkyldisopyramide (MND) enantiomers in plasma and urine. The drugs were extracted from plasma samples by liquid-liquid extraction with dichloromethane after protein precipitation with trichloroacetic acid; the urine samples were processed by liquid-liquid extraction with dichloromethane. The enantiomers were resolved on a Chiralpak AD column using hexane-ethanol (91:9, v/v) plus 0.

Enantioselective HPLC analysis of propafenone and of its main metabolites using polysaccharide and protein-based chiral stationary phases.

HPLC on chiral stationary phases has been used for the enantioselective assay of propafenone (PPF), 5-hydroxypropafenone (PPF-50H) and N-despropylpropafenone (PPF-NOR) enantiomers. The results obtained on Chiralpak AD column showed that it is useful for the resolution of PPF and of its main metabolites, although the peaks obtained for PPF-NOR were not symmetrical under the conditions investigated. This column and circular dichroism-based detection system were used to determine the absolute configuration of the eluates.

Enantioselective analysis of metoprolol in plasma using high-performance liquid chromatographic direct and indirect separations: applications in pharmacokinetics.

Direct enantioselective separation on chiral stationary phases and indirect separation based on the formation of diastereomeric derivatives were developed and compared for the HPLC analysis of R(+) and S(-)-metoprolol in human plasma. Plasma samples prepared using solid-phase extraction columns or liquid-liquid extraction were directly analyzed on a Chiralpack AD or on a Chiralcel OD-H columns, respectively. S-(-)-menthyl choroformate was also used to yield diastereomeric derivatives resolved on a RP-8 column.

Simultaneous determination of propafenone and 5-hydroxypropafenone enantiomers in plasma by chromatography on an amylose derived chiral stationary phase.

An enantioselective liquid chromatography method was developed for the simultaneous determination of propafenone (PPF) and 5-hydroxypropafenone (PPF-5OH) enantiomers in plasma. After liquid liquid extraction with dichloromethane, the enantiomers were resolved on a Chiralpak AD column using hexane-ethanol (88:12, v/v) plus 0.1% diethylamine as the mobile phase and monitored at 315 nm.

Time-frequency methods applied to muscle fatigue assessment during dynamic contractions.

This paper discusses the assessment of the electrical manifestations of muscle fatigue during dynamic contractions. In the past, the study of muscle fatigue was restricted to isometric constant force contractions because, in this contraction paradigm, the myoelectric signal may be considered as wide sense stationary over epochs lasting up to two or three seconds, and hence classic spectral estimation techniques may be applied. Recently, the availability of spectral estimation techniques specifically designed for nonstationary signal analysis made it possible to extend the employment of muscle fatigue assessment to cyclic dynamic contractions, thus increasing noticeably its possible clinical applications.

Gait abnormalities in minimally impaired multiple sclerosis patients.

Subclinical evidence of gait abnormalities were identified in a group of seven patients with multiple sclerosis, EDSS scored 0 - 2, without functional limitations. A movement analysis technique was used to identify gait parameters indicative of impaired motor function during walking. Abnormalities related primarily to time-distance parameters (reduced speed of progression, shorter strides, prolonged double support phase) and muscular function (premature recruitment of gastrocnemius and late relaxation of tibialis anterior during stance phase) were identified regardless the severity of the clinical score.

Determination of ametryn herbicide by bioassay and gas chromatography-mass spectrometry in analysis of residues in drinking water.

A simple, rapid and quantitative bioassay method was compared to a gas chromatography/mass spectrometry (GC/MS) procedure for the analysis of ametryn in surface and groundwater. This method was based on the activity of ametryn in inhibiting the growth of the primary root and shoot of germinating letuce, Lactuca sativa L. seed.

Myoelectric activation pattern during gait in total knee replacement: relationship with kinematics, kinetics, and clinical outcome.

Gait usually presents an excellent improvement after total knee replacement. Nevertheless, some abnormalities persist even after a long period of time. The abnormal knee patterns have been attributed to several possible causes, such as implant geometry and surgical technique, posterior cruciate ligament sparing/sacrificing, preoperative "stiff-knee" pattern due to pain and altered biomechanics, weakness of the extensor muscles, preoperative arthritic pattern, proprioceptive deficiency, and multijoint degenerative involvement.

Enantioselective kinetic disposition of albendazole sulfoxide in patients with neurocysticercosis.

The enantioselectivity of the kinetic disposition of albendazole sulfoxide (ASOX) was investigated in 18 patients with neurocysticercosis treated with a multiple dose regimen of albendazole for 8 days (5 mg/kg every 8 h). Serial blood samples were collected on the eighth day of treatment during the last dose interval, with prorogation up to 12 h. Albendazole sulfone (ASON) and enantiomers of ASOX were analyzed in plasma samples by HPLC using a Chiralpak AD column and detection by fluorescence.

EMG assessment of back muscle function during cyclical lifting.

A new approach to estimating the frequency compression of the surface EMG signal during cyclical dynamic exercise is described. The basic properties of the method are first developed using simulated EMG signals. Spectral compression is measured by defining the instantaneous median frequency from time-frequency representations of the signal derived from a transformation of the Cohen class.

Simultaneous determination of albendazole sulfoxide enantiomers and albendazole sulfone in plasma.

A high-performance liquid chromatographic method has been developed for the simultaneous determination of albendazole sulfoxide (ABZSO) enantiomers and albendazole sulfone (ABZSO2) in human plasma. The resolution of ABZSO enantiomers and ABZSO2 was obtained on a Chiralpak AD column using hexane-isopropanol-ethanol (81:14.25:4.

Enantioselective analysis of propafenone in plasma using a polysaccharide-based chiral stationary phase under reversed-phase conditions.

We present a method for the enantioselective analysis of propafenone in human plasma for application in clinical pharmacokinetic studies. Propafenone enantiomers were resolved on a 10-microm Chiralcel OD-R column (250 x 4.6 mm I.

A proposal for standardizing urine collections for bone resorption markers measurement.

Diurnal variations in the excretion of bone resorption markers were assessed in order to identify the type of urine collection which provides the most information on bone resorption rate and its relation to measuring bone dynamics in a postmenopausal population. Sixty women, ages 43-67 and without disease or treatment known to affect bone mineral density, were divided into two groups on the basis of femoral mineral density T-score: <1.5 (Group I), >1.

A statistical method for the measurement of muscle activation intervals from surface myoelectric signal during gait.

The aim of this work is to present an original double-threshold detector of muscle activation, specifically developed for gait analysis. This detector operates on the raw myoelectric signal and, hence, it does not require any envelope detection. Its performances are fixed by the values of three parameters, namely, false-alarm probability (Pfa), detection probability, and time resolution.

Enantioselective analysis of praziquantel in plasma samples.

A direct enantioselective high-performance liquid chromatography method is described for the quantitative determination of praziquantel enantiomers in plasma samples. The method involves two-step extraction of plasma with toluene, evaporation of the solvent and chromatography on a Chiralcel OD-H column using hexane-ethanol (85:15, v/v) as the mobile phase and detection at 220 nm. The assay satisfies all of the criteria required for use in clinical pharmacokinetic studies.

Therapy for neurocysticercosis: pharmacokinetic interaction of albendazole sulfoxide with dexamethasone.

Albendazole is considered the drug of choice for neurocysticercosis. It is frequently used in combination with dexamethasone to prevent the acute inflammatory reaction due to cysticercal death. It has been reported that dexamethasone increases the plasma level of albendazole sulfoxide, the active metabolite of albendazole.

Enantioselective determination of the hydroxylated metabolites of mexiletine in human plasma.

Pre-column derivatization with o-phthaldialdehyde and N-acetyl-l-cysteine was used for liquid-chromatographic diastereomeric resolution of p-hydroxymexiletine (PHM) and hydroxymethylmexiletine (HMM), metabolites of mexiletine formed by aromatic and aliphatic hydroxylation, respectively. The resulting diastereomeric derivatives were resolved on a C18 column and monitored by fluorescence detection. The diastereomeric elution order for both metabolites was determined on the basis of the circular dichroism spectra of each eluted fraction.

Enantioselective analysis of albendazole sulfoxide in plasma using the chiral stationary phase.

We present a method for the enantioselective analysis of albendazole sulfoxide (ABZSO) in plasma for application in clinical pharmacokinetic studies. ABZSO enantiomers were separated on a 5-micron Chiralcel OB-H column (4.6 x 150 mm) using hexane:ethanol (93:7, v/v) as the mobile phase and fluorescence detection.

High-performance liquid chromatographic determination of mexiletine enantiomers in plasma using direct and indirect enantioselective separations.

Two methods were developed for the determination of mexiletine enantiomers in plasma samples suitable for studies on the stereoselective disposition of this drug. Both methods used fluorescence detection to improve sensitivity and selectivity. The direct enantioselective separation was based on the chiral resolution of mexiletine-2-naphthamide derivatives on a Chiralcel OJ column.

Simultaneous HPLC analysis of tricyclic antidepressants and metabolites in plasma samples.

A sensitive, selective and rapid reverse-phase high-performance liquid chromatographic method was developed for the simultaneous analysis of imipramine, desipramine, amitriptyline and nortriptyline in human plasma. The procedure consisted of extracting the drugs and the internal standard (clomipramine) from 1 ml plasma with hexane:isoamyl alcohol (99:1, v/v) in alkaline medium. A newly marketed column, LiChrospher 60 RP-select B (dp 5 microns) of Merck was employed.

Improved late potential analysis in frequency domain.

This work presents a technique to improve the identification of late potentials (LP) in patients affected by greater arrhythmogenic right ventricular disease (GARVD). Several authors have documented the correlation between GARVD and LP by means of time domain analysis. Moreover, the high incidence of bundle branch block in patients affected by GARVD suggests LP analysis in the frequency domain be performed.

Factors influencing plasma concentrations of carbamazepine and carbamazepine-10,11-epoxide in epileptic children and adults.

Plasma carbamazepine (CBZ) and carbamazepine-10,11-epoxide (CBZ-E) concentrations were measured in 160 epileptic patients in order to determine the effect of factors such as age, daily dosing schedule, formulation, and combination with other antiepileptic drugs on these concentrations in relation to the daily dose. The results showed that the CBZ plasma level/dose ratio was affected by all factors studied, whereas the CBZ-E plasma level/dose ratio was affected only by formulation and age. The ratio of CBZ-E to CBZ plasma levels (CBZ-E/CBZ) was affected by daily dosing schedule, age, and combination with other antiepileptic drugs.

Determination of albendazole metabolites in plasma by HPLC.

Albendazole is an antihelminthic agent belonging to the benzimidazole class and has been used successfully in the treatment of neurocysticercosis. We report here a method for the determination of the two major albendazole metabolites in plasma, albendazole sulfone and albendazole sulfoxide. The method consists of drug extraction from 500 microL of plasma previously acidified with chloroform-isopropanol (9:1, v/v) and extract purification with n-hexane immediately before chromatographic analysis.

Measurement of carbamazepine and its main biotransformation products in plasma by HPLC.

We present a method that permits the simultaneous analysis of carbamazepine (CBZ) and its major biotransformation products, carbamazepine-10,11-epoxide (CBZ-E) and carbamazepine-10,11-dihydroxide (CBZ-diOH), in plasma samples. The method consists of plasma extraction in alkaline medium with NaCl added using chloroform-ethyl acetate (1:1, v/v) and later purification with n-hexane. The samples were submitted to reversed-phase chromatography (RP-18) using acetonitrile-water (3:7, v/v) as the mobile phase and detection at 220 nm.

A new derivatization procedure for the analysis of hippuric acid and m-methyl-hippuric acid by gas chromatography.

The industrial solvents, toluene and xylene, have physicochemical properties that can be hazardous to the workers exposed. Since hippuric acid and m-methyl-hippuric acid represent the products of toluene and xylene biotransformation in urine, they are used as biological markers in studies on occupational exposure to these solvents. Several methods have been used to determine hippuric acid and m-methyl-hippuric acid--either based on gas chromatography or on high-performance liquid chromatography.