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An assay using high-performance liquid chromatography has been developed for the determination of bromazepam in plasma. After a single-step extraction from basified samples with dichloromethane, using decarboxyloflazepate as an internal standard, samples were analysed using a reversed-phase Nova Pak 5-microns column with a mobile phase of methanol - phosphate buffer (60 + 40) adjusted to pH 7.6. The drugs were detected at 239 nm and the limit of detection was found to be 3 micrograms l-1 for bromazepam. The method is simple, rapid and sensitive and permits bromazepam levels in clinical and pharmacokinetic studies to be monitored.  相似文献   

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A simple and sensitive method for determination of benzodiazepines in plasma has been developed using high-performance liquid chromatography in a reverse-phase mode. The method is illustrated by application to plasma samples containing diazepam and N-desmethyldiazepam at concentrations which would be encountered during therapy, with limits of detection of 10 ng/ml and 2 ng/ml for diazepam and N-desmethyldiazepam, respectively.  相似文献   

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A simple high-performance liquid chromatographic (HPLC) method was developed and validated for rapid quantification of linezolid in human plasma. Protein precipitation using a mixture of 5% trichloroacetic acid and methanol (3:1, v/v) provided a straightforward method of sample preparation and the internal standard eperezolid was employed. A concentration range from 0.20 to 40.0 mg/L was utilized to construct calibration curves, and analysis of low- (0.40 mg/L), medium- (7.50 mg/L) and high-quality (25.0 mg/L) control samples revealed excellent reproducibility (相似文献   

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Ambroxol has been determined in biological fluids using a rapid and sensitive high-performance liquid chromatographic method. The samples prepared from plasma by liquid-liquid extraction were analysed on reversed-phase silica gel by competing-ion chromatography with ultraviolet detection. The method was applied to the determination of ambroxol levels in twelve healthy volunteers after oral administration of 90 mg of ambroxol in tablets of Mucosolvan and Ambrosan.  相似文献   

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A new method is described for the determination of submicromolar concentrations of 5-bromodeoxyuridine in human plasma. Sample pretreatment involves cold methanol deproteinization, freezing-thawing and lyophilization. The sample is then analysed by reversed-phase high-performance liquid chromatography. This method is very reproducible and has a detection limit of 0.1 microgram/ml (0.32.10(-6) M). Comparison with other procedures indicates that the method is advantageous as regards sensitivity and specificity and can be readily applied in clinical pharmacological investigations.  相似文献   

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A selective high-performance liquid chromatographic (HPLC) method with ultraviolet-visible (UV-VIS) detection was developed to measure therapeutic concentrations of spectinomycin in turkey plasma. Treatment of plasma samples with 3% trifluoroacetic acid in acetonitrile facilitated spectinomycin extraction and protein precipitation. After centrifugation, the stable derivatization reagent, 2,4-dinitrophenyl-hydrazine, was added to an aliquot of the supernatant, and the mixture was incubated for 30 min at 70 degrees C. Excess reagent was quenched with acetone and additional heating. The resulting derivative, a proposed spectinomycin-hydrazone, was separated from other compounds by reversed-phase HPLC during a short gradient run. The absorbance of the effluent was monitored spectrophotometrically with the UV-VIS detector set at 205 nm. The detector response was linear through the range of interest, 2-100 micrograms/ml.  相似文献   

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A high-performance liquid chromatographic (HPLC) method with ultraviolet detection for the determination of a novel 4-aza-steroidal inhibitor of 5 alpha-reductase in human plasma has been developed. The assay is based on a single solid-phase extraction and an efficient HPLC separation on two analytical columns in series. The assay has been fully validated and used to support Phase II and III clinical pharmacokinetic studies. The lowest limit of quantification was found to be at 1 ng/ml and allowed pharmacokinetic evaluation of the drug at doses down to 5 mg.  相似文献   

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A high-performance liquid chromatographic assay for determination of cefonicid concentrations in human plasma and urine samples has been developed using cefazolin as an internal standard. For the analysis of plasma samples two calibration curves were utilized covering the cefonicid concentration ranges of 0.05-1.0 microgram/ml and 1.0-50.0 micrograms/ml, respectively. Coefficients of variation of 7.4% or less were obtained for cefonicid concentrations of 0.05-50.0 micrograms/ml. Mean bias was +6.0% at 0.05 micrograms/ml cefonicid and between -2.1% and +1.6% for 1.0-50.0 micrograms/ml cefonicid. Plasma samples containing 30 ng/ml cefonicid could be well distinguished from blank plasma samples. Urine samples were analysed by using a calibration curve for cefonicid concentrations between 1.0 and 50.0 micrograms/ml. ranged from 8.6% at a cefonicid concentration of 1.0 microgram/ml to 0.5% at 50.0 micrograms/ml with a mean bias between -3.0% and +0.3%.  相似文献   

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A selective and sensitive high-performance liquid chromatographic method for determination of intact glibenclamide in human plasma or urine has been developed. With glibornuride as internal standard, acid-buffered plasma or urine was extracted with benzene. The organic layer was evaporated and the residue was dissolved in equilibrated mobile phase (acetonitrile-phosphate buffer 0.01 M pH 3.5, 50:50). An aliquot of 20 microliters was chromatographed on a Spherisorb ODS reversed-phase column, and quantitation was achieved by monitoring the ultraviolet absorbance at 225 nm. The response was linear (0-1000 ng/ml) and the detection limit was 5-10 ng/ml in plasma or urine. The within-assay variation was less than or equal to 10%. No interferences from metabolites or endogenous constituents could be noted. The utility of the method was demonstrated by analysing glibenclamide in samples from diabetic subjects on therapeutic doses of the drug.  相似文献   

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