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O Soares

Publications and source records attributed to O Soares.

4 recordsLinked to original sources

Simultaneous determination of pyrimethamine and sulphadoxine in human plasma by high-performance liquid chromatography after automated liquid-solid extraction.

A high-performance liquid chromatographic method with ultraviolet detection is described for the simultaneous measurement of pyrimethamine and sulphadoxine in human plasma. After an automated liquid-solid extraction on a C8 cartridge, the compounds are separated on a C18 column by isocratic elution; the mobile phase is methanol-acetonitrile-water (10:25:65, v/v/v) with triethylamine (1%) and adjusted to pH 5.6 with phosphoric acid. The eluent is monitored with an ultraviolet detector at 240 nm. The limit of quantification was 10 ng/ml for pyrimethamine and 22 microg/ml for sulphadoxine. No chromatographic interferences can be detected from endogenous compounds, other anti-malarial drugs or major drugs used for the treatment of children. Sulphadimethoxine is used as an internal standard. The method is accurate and precision is good with relative standard deviations lower than 6%. The chromatographic procedure takes 11 min. The method is comparatively rapid, simple, sensitive and can be used for therapeutic drug monitoring, clinical and pharmacokinetic studies.

Automation↗

New solid-phase extraction for an improved high-performance liquid chromatographic procedure for the quantitation of halofantrine and monodesbutylhalofantrine in blood or plasma.

A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method, with fluorimetric detection, for the simultaneous measurement of halofantrine and desbutylhalofantrine in human plasma or whole blood is described. Sample preparation involved protein precipitation, followed by an efficient solid-phase extraction on a C8 cartridge. Analytes were isolated from 1 ml of the biological fluids and recovered by a 2% acetic acid in ethyl acetate solution. Chromatographic separation was carried out on a LiChrospher 60 RP select B, C8 bonded phase (5 microns particle size, 25 cm x 4 mm I.D.) using a mobile phase of water-acetonitrile (35:65, v/v) containing triethylamine (1%) and adjusted to pH 4 with orthophosphoric acid. The total run time was 14 min. Relative standard deviations of the intra-and inter-assay precisions were less than 5.9%. Assumption of linearity was investigated by studying the y-residuals and by ANOVA (analysis of variance). Because of the wide range of calibration (0.1 to 2.0 microgram/ml) variances were non-homogeneous (Hartley's test) and the weighted regression line was computed in order to allow pharmacokinetic studies. Accuracy was tested using a t-statistic. Limits of decision, detection and quantification were realized from an analysis of the blanks. Application of the method to clinical specimens was demonstrated.

Antimalarials↗

Simultaneous determination of chloroquine and quinine in human biological fluids by high-performance liquid chromatography.

A high-performance liquid chromatographic method with fluorescence detection is described for the simultaneous measurement of quinine, chloroquine and mono- and bidesethylchloroquine in human plasma, erythrocytes and urine. After a liquid-solid extraction on a Bond Elut C8 cartridge, the compounds are separated on an Inertsil silica column by gradient elution; the mobile phase is a mixture of acetonitrile and methanol-25% ammonia solution (92.7:7.5, v/v). The eluent was monitored with a fluorescence detector (excitation wavelength 325 nm and emission wavelength 375 nm). The limit of detection was ca. 5 ng/ml for chloroquine and ca. 23 ng/ml for quinine. No chromatographic interferences could be detected from endogenous compounds or other antimalarial drugs. The method is accurate with inter- and intra-assay coefficients of variation lower than 7%. Hydroxychloroquine is used as an internal standard because of its structural similarity to chloroquine. The procedure requires 30 min and can be used for therapeutic drug monitoring.

Chloroquine↗