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At least 199 records · Page 11Linked to original sources
PubMed2005

Simultaneous determination of oxymatrine and its active metabolite matrine in dog plasma by liquid chromatography-mass spectrometry and its application to pharmacokinetic studies.

A simple, rapid and reliable method was developed for the quantification of oxymatrine (OMT) and its metabolite matrine (MT) in beagle dog plasma using a liquid-liquid extraction procedure followed by liquid chromatography-electrospray ionization mass spectrometric (LC-ESI-MS) analysis. Extend-C18 column (2.1 mm i.d. x 50 mm, 5 microm) with a C18 guard column (2.1 mm i.d. x 12.5 mm) was used as the analytical column. Linear detection responses were obtained for OMT concentration ranging from 5 to 4000 ng/ml and for MT concentration ranging from 5 to 2000 ng/ml. The precision and accuracy data, based on intra- and inter-day variations over 5 days, were lower than 5%. The limit of quantitation for OMT and MT were 2 and 1 ng/ml, respectively, and their recoveries were greater than 90%. Pharmacokinetic data of OMT and its active metabolite MT obtained with this method following a single oral dose of 300 mg OMT capsules to six beagle dogs was also reported for the first time.

Alkaloids↗
PubMed2005

Determination of lorazepam in plasma from children by high-performance liquid chromatography with UV detection.

A simple, sensitive, selective, and reproducible reversed-phase high-performance liquid chromatographic (HPLC) method with UV detection was developed for the determination of lorazepam (LZP) in human plasma, using oxazepam (OZP) as internal standard. LZP and OZP were extracted from alkalinized (pH 9.5) spiked and clinical plasma samples using a single step liquid-liquid extraction with a mixture of n-hexane-dichloromethane (70:30%; v/v). Chromatographic separation was performed on a reversed-phase Synergi Max RP analytical column (150 mmx4.6 mm i.d.; 4 microm particle size), using an aqueous mobile phase (10 mM KH2PO4 buffer (pH 2.4)-acetonitrile; 65:35%, v/v) delivered at a flow-rate of 2.5 ml/min. Retention times for OZP and LZP were 10.2 and 11.9 min, respectively. Calibration curves were linear from 10 to 300 ng with correlation coefficients (r2) better than 0.99. The limits of detection (LOD) and quantification (LOQ) were 2.5 and 10 ng/ml, respectively, using 0.5 ml samples. The mean relative recoveries at 20 and 300 ng/ml were 84.1+/-5.5% (n=6) and 72.4+/-5.9% (n=7), respectively; for OZP at 200 ng the value was 68.2+/-6.8% (n=14). The intra-assay relative standard deviations (R.S.D.) at 20, 150 and 270 ng/ml of LZP were 7.8%, 9.8% (n=7 in all cases) and 6.6% (n=8), respectively. The inter-assay R.S.D. at the above concentrations were 15.9%, 7.7% and 8.4% (n=7 in all cases), respectively. Intra- and inter-assay accuracy data were within the acceptance interval of +/-20% of the nominal values. There was no interference from other commonly co-administered anticonvulsant, antimicrobial, antipyretic, and antimalarial drugs. The method has been successfully applied to a pharmacokinetic study of LZP in children with severe malaria and convulsions following administration of a single intravenous dose (0.1 mg/kg body weight) of LZP.

Anticonvulsants↗
PubMed2005

Quantitative determination of atractylenolide III in rat plasma by liquid chromatography electrospray ionization mass spectrometry.

Atractylenolide III is a major active component in Atractylodes macrocephala. This paper describes a simple, rapid, specific and sensitive method for the quantification of atractylenolide III in rat plasma using a liquid-liquid extraction procedure followed by liquid chromatography mass spectrometric (LC-MS) analysis. A Kromasil 3.5 microm C(18) column (150 mm x 2.00 mm) was used as the analytical column. Linear detection responses were obtained for atractylenolide III concentration ranging from 5 to 500 ng L(-1). The precision and accuracy data, based on intra-day and inter-day variations over 5 days were within 10.29%. The lower limit of quantitation for atractylenolide III was 5 ng mL(-1), using 0.1 mL plasma for extraction and its recoveries were greater than 85% at the low, medium and high concentrations. The method has been successfully applied to a pharmacokinetic study in rats after an oral administration of atractylenolide III with a dose of 20.0 mg kg(-1). With the lower limits of quantification at 5 ng mL(-1) for atractylenolide III, this method was proved to be sensitive enough for the pharmacokinetics study of atractylenolide III.

Animals↗
PubMed2006

Determination of helicidum and its metabolites in dog plasma by LC/UV/MS/MS and its application to pharmacokinetic studies.

A simple, rapid and reliable method was developed for the identification and quantification of helicidum and its metabolites in beagle dog plasma by liquid chromatography/ultra-violet/electrospray ionization-ion trap mass spectrometry (LC/UV/ESI-ITMS). Two metabolites were identified by MS: formylphenyl-O-beta-d-pyranosyl alloside (I) and hydroxylmethylphenyl-O-beta-d-pyranosyl alloside (II). UV was used for concentration determination with the wavelength of 270 nm. Liquid-liquid extraction was used and the extraction recovery exceeded 90%. Kromacil C(18) column (5 microm, 4.6mm i.d. x 250 mm) was used as the analytical column. Linear detection responses were obtained for helicidum concentration ranging from 1.76 x 10(-4) to 70.4 x 10(-4) micromol/mL (0.050-2.00 microg/mL). The precision and accuracy data, based on intra- and inter-day variations over 3 days, were less than 5%. The limit of determination and quantitation (LOD, LOQ) for helicidum was 0.010 and 0.030 microg/mL, respectively. Pharmacokinetic data of helicidum and the two metabolites were obtained with this method after administration of intravenous injection and a single oral dose of tablets to six beagle dogs, respectively.

Animals↗
PubMed2005

The short-term reliability of grip strength measurement and the effects of posture and grip span.

PURPOSE: Because of the difficulty in verifying the reliability and validity of grip strength there is still no consensus regarding its measurement, particularly short-term reliability. The present study was conducted to investigate the short-term reliability of grip strength measurement and the effects of posture and grip span. METHODS: One hundred healthy subjects (50 men, 50 women; mean age, 38.2 y; range, 22-58 y) were evaluated. Grip strength was measured twice as a single set by using a dynamometer and the mean value for each hand was recorded. First 3 sets of measurements were performed using 2 different approaches: (1) continuous measurement without rest and (2) interval measurement with a 1-minute rest after each set. Next 1 set of measurements was performed with 3 types of grip span: standard grip span (which was measured as one half the distance between the index finger tip and the metacarpophalangeal joint flexion crease at the base of the thumb), +10% of the standard grip span, and -10% of the standard grip span. Finally 1 set of measurements was performed in 3 postures: standing, sitting, and supine. RESULTS: During continuous measurement the grip strength decreased gradually as the number of sets increased. During interval measurement, however, there was no change among sets for both genders and each hand. On the basis of this result subsequent studies were performed using interval measurement. There was no significant difference in maximum grip strength between the standard and +10% of standard grip span measurements; however, the -10% of standard model gave the minimum grip strength in both genders. With regard to posture the minimum grip strength in both genders was obtained when the subject was supine, with no difference between standing and sitting. CONCLUSIONS: Our study showed that interval measurement with a 1-minute rest after each set yielded a constant value; therefore, we advocate this approach for rapid evaluation of grip strength under different conditions. In addition the influence of grip span and posture should be considered to maximize data accuracy.

Adult↗
PubMed2004

A new HPLC/UV method for the determination of clindamycin in dog blood serum.

A new HPLC method for the quantitative determination of clindamycin in dog blood serum at levels down to 80 ng/ml has been developed. Samples were deproteinised with acetonitrile and clindamycin was extracted with dichloromethane. Chromatographic analysis was carried out on a C(18) reversed-phase analytical column in the presence of tetra-n-butylammonium hydrogen sulfate (TBA), as an ion-pairing agent. UV detector wavelength was set at 195 nm. The assay was validated for a concentration range from 80 to 6000 ng/ml serum. Good linearity was observed in the entire concentration range. The limit of quantification (LOQ) was 80 ng/ml and the limit of detection (LOD) was 60 ng/ml. Regression of accuracy data yielded an overall mean recovery value (+/-S.E.M.) of 93.98+/-0.42%, while precision data revealed coefficient of variation (CV (%)) values lower than 4.41%. The method was successfully applied to determine drug concentrations in serum samples from dogs that had been orally administered clindamycin hydrochloride.

Animals↗
PubMed2004

Quantitative determination of albendazole metabolites in sheep spermatozoa and seminal plasma by liquid chromatographic analysis with fluorescence detection.

A new analytical method for the simultaneous quantitative determination of albendazole metabolites in sheep spermatozoa and seminal plasma at levels down to 46.5 ng/mL for albendazole sulphoxide (ABZ-SO), 7.5 ng/mL for albendazole sulphone (ABZ-SO2) and 12 ng/mL for albendazole 2-aminosulphone (ABZ-SO2NH2) has been developed. Analytes were extracted from alkalinized samples with ethyl acetate. Separation was carried out on a C18 column in the presence of tetra-n-butylammonium (TBA) hydrogen sulphate and octanesulphonate sodium (OCT), as ion-pair agents. Fluorometric detection was performed with excitation and emission wavelengths set at 290 and 320 nm, respectively. Accuracy data showed overall recoveries (+/-S.E.M.) of 83.1+/-1.2% for ABZ-SO, 98.8+/-0.6% for ABZ-SO2 and 85.3+/-0.7% for ABZ-SO2NH2, in spermatozoa. Respective values in seminal plasma were 88.0+/-0.9%, 97.7+/-0.5% and 93.2+/-1.7%. Precision data suggested coefficient of variation (CV%) values lower than 5.9% for spermatozoa and 3.8% for seminal plasma. The method was successfully applied for the determination of the three albendazole metabolites in semen samples collected from rams that had been orally administered albendazole.

Albendazole↗
PubMed2005

Application of 2-acetylbutyrolactone to spectrofluorimetry: fluorescence properties of Schiff bases derived from 2-acetylbutyrolactone and spectrofluorimetric determination of primary amine-containing compounds.

2-Acetylbutyrolactone (ABL) has been characterized for use as a fluorogenic reagent for the spectrofluorimetric determination of primary amines. The reagent forms strongly fluorescent Schiff bases upon the reaction with primary amines in acid-catalized aqueous solutions or in dimethylformamide (DMF). Sulfamethoxazole (SMX) and ampicillin sodium (AMP Na) were used as model amines of type ArNH(2) and RNH(2), respectively. The reaction conditions, fluorescence spectral properties and the stability of the derivatives have been investigated. The chemistry and the pathway of the reaction have been discussed. Calibration data, accuracy, precision, limits of detection, limits of quantification and other aspects of analytical merit were presented in the text. The utility of ABL for the analysis of the model drugs in pharmaceutical preparations was demonstrated. The results indicated that the proposed methods are equally accurate and precise as the official or other reported methods.

4-Butyrolactone↗
PubMed2006

Determination of stigmasterol, beta-sitosterol and stigmastanol in oral dosage forms using high performance liquid chromatography with evaporative light scattering detection.

A validated and repeatable high performance liquid chromatography (HPLC) method with online evaporative light scattering (ELSD) was developed for the analysis of two sterols, stigmasterol, beta-sitosterol and a stanol, stigmastanol, found to be common in many herbal formulations and health care supplements. The method is based on the separation of the three marker compounds on a C8 column (Phenomenex Luna, 5 microm, 150 mmx4.6 mm i.d.) using methanol:water (95:5 v/v) as the mobile phase, and a flow rate of 1 ml/min to separate all the marker compounds within 12 min. Cholesterol (50 microg/ml) was used as internal standard and methanol as the extraction solvent. The ELSD response parameters were optimised and the limits of detection (LOD) and quantification (LOQ) were calculated to be 2 and 5 microg/ml, respectively, which is more sensitive than obtained by photo diode array detection (5 and 7 microg/ml). Using ELSD, the percentage relative standard deviation (%R.S.D.) of intra-day and inter-day (3 days) precision for each marker was better than 3%, the accuracy data were within 97-103% and the recovery data were found to be within 95-107% for the five commercially available products examined. This method was used to assay commercially available products formulated as oral dosage forms purported to contain African Potato and associated sterols and stanol and proved to be suitable for the routine analysis and quality control of such products.

Administration, Oral↗
PubMed2005

Incidental effects of emotional valence in single word processing: an fMRI study.

The present study aimed at identifying the neural responses associated with the incidental processing of the emotional valence of single words using event-related functional magnetic resonance imaging (fMRI). Twenty right-handed participants performed a visual lexical decision task, discriminating between nouns and orthographically and phonologically legal nonwords. Positive, neutral and negative word categories were matched for frequency, number and frequency of orthographic neighbors, number of letters and imageability. Response times and accuracy data differed significantly between positive and neutral, and positive and negative words respectively, thus, replicating the findings of a pilot study. Words showed distributed, mainly left hemisphere activations, indicating involvement of a neural network responsible for semantic word knowledge. The neuroimaging data further revealed areas in left orbitofrontal gyrus and bilateral inferior frontal gyrus with greater activation to emotional than to neutral words. These brain regions are known to be involved in processing semantic and emotional information. Furthermore, distinct activations associated with positive words were observed in bilateral middle temporal and superior frontal gyrus, known to support semantic retrieval, and a distributed network, namely anterior and posterior cingulate gyrus, lingual gyrus and hippocampus when comparing positive and negative words. The latter areas were previously associated with explicit and not incidental processing of the emotional meaning of words and emotional memory retrieval. Thus, the results are discussed in relation to models of processing semantic and episodic emotional information.

Adult↗
PubMed2004

Psychology and neurobiology of simple decisions.

Patterns of neural firing linked to eye movement decisions show that behavioral decisions are predicted by the differential firing rates of cells coding selected and nonselected stimulus alternatives. These results can be interpreted using models developed in mathematical psychology to model behavioral decisions. Current models assume that decisions are made by accumulating noisy stimulus information until sufficient information for a response is obtained. Here, the models, and the techniques used to test them against response-time distribution and accuracy data, are described. Such models provide a quantitative link between the time-course of behavioral decisions and the growth of stimulus information in neural firing data.

Action Potentials↗
PubMed2002

On the impact of different number representations in the number bisection task.

The number bisection task--in which the numerical middle of two other numbers has to be determined (e.g., 6 is the numerical middle of 4 and 8)--has recently been used in neuropsychological case studies in addition to the number comparison task to assess quantitative capabilities in number processing. While factors determining difficulty in normal participants have often been systematically investigated in the number comparison task, this has not yet been done in the number bisection task. Based on a pilot study by van Herten (1999), we extracted four factors that we hypothesized to modulate difficulty in a verification version of the number bisection task in normal participants: Multiplicativity (whether or not the three numbers are part of a multiplication table), range (distance between the smallest and the largest number) for bisectable number triplets as well as distance of the middle number to the numerical middle, and bisection possibility for non-bisectable triplets. In the current study, we obtained large effects for all four factors on RT and accuracy data and some interesting interactions in normal participants. In a regression analysis, we additionally observed inhibitory effects of decade crossing and of ten inclusion (whether or not one of the three numbers was a decade number). We discuss the impact of these results for the use of the number bisection task as an assessment tool in neuropsychology. Finally, we examine the consequences of these results for models of number processing.

Adult↗
PubMed1981

Analysis of the anti-coccidial drug, halofuginone, in chicken tissue and chicken feed using high-performance liquid chromatography.

Methods are described for the analysis of the anti-coccidial drug, halofuginone, in chicken tissue at concentrations as low as 1 ppb (0.001 ppm) and in chicken feed at a concentration of 3 ppm, using high-performance liquid chromatography. The tissue analysis involves: enzymatic release of the halofuginone followed by ethyl acetate extraction under basic conditions, partition into ammonium acetate buffer, concentration using Sep-pakTM C18 cartridge. The feed analysis involves: ethyl acetate extraction under basic conditions, partition into hydrochloric acid, concentration using XAD-2 column chromatography. Both methods use high-performance liquid chromatography with ultraviolet detection for the final analysis. Precision and accuracy data for both methods are given.

Animal Feed↗
PubMed1989

National Pediatric Trauma Registry.

The National Pediatric Trauma Registry (NPTR) is a multi-institutional database designed to compile information concerning all aspects of pediatric trauma care. The registry is designed and operated in a manner that maximizes data accuracy and provides this information to all participating investigators. The growth of the database has allowed the NPTR to provide the first accurate epidemiologic description of pediatric trauma as a national disease, as well as to develop national norms for pediatric trauma care. The registry presently contains 10,177 patients, and is undergoing revisions (phase II) to allow a more focused evaluation of various aspects of the clinical care and rehabilitation of the pediatric trauma patient.

Child↗
PubMed1999

The control of heartwater on large-scale commercial and smallholder farms in Zimbabwe.

As part of a series of studies associated with the development of improved vaccines for heartwater (a tick-borne disease of ruminant livestock caused by Cowdria ruminantium), field surveys were carried out to assess losses associated with the disease and the costs associated with controlling it in the two main agro-ecological zones of Zimbabwe (lowveld and highveld) where heartwater is believed to be endemic and epidemic, respectively. In each zone, a cross-sectional study was performed in the main farming systems (smallholder (SH) and large-scale commercial (LSC) beef and dairy), followed by longitudinal studies in the same sectors to improve data accuracy for some parameters. Suspected heartwater-specific mortality in cattle was similar in all LSC sectors (p = 0.72) accounting for a median 1% mortality risk. Heartwater-specific mortality in SH areas was not assessed due to poor diagnostic ability of the farmers. Few LSC farms and SH households kept sheep; suspected heartwater-specific mortality in LSC sheep was 0.8% in the lowveld and 2.4% in the highveld. Goats were a major enterprise in SH areas but not on LSC farms. Suspected heartwater mortality in LSC goats was 0.8% at one site in the highveld and 17.5% on a farm in the lowveld. Application of acaricides was the major control method for heartwater and other tick-borne diseases on both SH and LSC farms. On LSC farms, plunge dipping was used most frequently and the number of acaricide applications ranged widely between 3 and 52 per year. The total cost of acaricides per head per annum was higher in highveld dairies than in highveld and lowveld beef enterprises (p = 0.03). In SH areas, cattle plunge dipping was conducted by the government with an average frequency of 8 +/- 2 (sd) immersions per annum in both the lowveld and highveld. The type of tick control on sheep and goats in all production systems was highly variable (ranging from none to hand removal or intensive acaricide treatment). Suspected heartwater cases on LSC farms were treated with tetracyclines; treatment was not reported in SH areas. Reported treatment costs were high (median Z$ 120) and highly variable (range Z$-833). Vaccination against heartwater with the live, blood-based vaccine was reported on only one LSC farm. LSC farms applying acaricide 30 or more times per year reported higher morbidity (p < 0.0001) and mortality (p < 0.0001) than farms applying acaricides less than 30 times a year. This finding supports the use of reduced tick control in the management of heartwater in Zimbabwe.

Agriculture↗
PubMed1988

Sensitive quantification of pseudoephedrine in human plasma and urine by high-performance liquid chromatography.

An assay for the selective quantification of pseudoephedrine in human plasma and urine was developed using high-performance liquid chromatography with UV detection at 205 nm. Analyte and internal standard were extracted from alkaline plasma or urine into a mixture of n-hexane and diethyl ether, and the organic phase was back-extracted into dilute acid. The chromatographic system comprises microparticulate cyanopropyl-silica as stationary phase and a ternary solvent mixture with ion-pair reagents as mobile phase. Using 0.25 ml plasma, the lower limit of quantification was 25 ng/ml with excellent linearity up to 1000 ng/ml. In urine, the calibration ranged from 2.5 to 100 micrograms/ml. The selectivity of the method was demonstrated for several pharmaceuticals with similar structures. The validated method was applied to a pharmacokinetic study with a single oral dose of 100 mg of pseudoephedrine in two galenic formulations. Precision and accuracy data of the assay and calculated pharmacokinetic parameters are presented.

Adolescent↗
PubMed1996

Trace analysis of albendazole and its sulphoxide and sulphone metabolites in milk by liquid chromatography.

Analytical methodology for determination of albendazole and its sulphoxide and sulphone metabolites in milk at levels down to 2-5 ng/ml has been developed. Extraction was carried out with ethyl acetate under alkaline conditions, and extracts were analyzed on a silica-based C18 column in the presence of positively-charged pairing ions. Accuracy data showed overall recoveries ranged from 78.4% to 100%, whereas precision data, based on within and between-day variation, suggested overall precision values better than 4.9%. The method was successfully applied to determine residues in milk of a dairy cow orally given albendazole.

Albendazole↗
PubMed1999

Determination of the geometrical diarylpropenamine isomers in feces by high-performance liquid chromatography.

Diarylpropenamine derivatives are a class of compounds which have been evaluated as potential drug candidates. Here a specific and reproducible HPLC method for the determination of cis- and trans-isomers of the unsubstituted derivative, 3-(4'-bromo-[1,1'-biphenyl]-4-yl)-3-(4-X-phenyl-N,N-dimethyl-2-propen -1-amine (I, where X=H) in feces is described. The analyte I and internal standard, nitro derivative (II, where X=NO2), were isolated from the basified biological matrix using a liquid-liquid extraction with ethyl acetate followed by a solid-phase procedure performed on a silica cartridge. The organic phase was evaporated to dryness, the residue was reconstituted in mobile phase and injected into the HPLC system. The analytes were eluted with ethyl acetate-hexane-triethylamine (59:40:1) in HPLC column (silica) and detected by UV spectrophotometry at 272 nm. Linearity, precision and accuracy data for feces standards after extraction were acceptable. The method has been applied to analyses of feces samples from rats dosed with I, in which it could be anticipated that fecal excretion is quantitatively the major route for I elimination.

Amines↗