Abstract

Abstract Methodological considerations are presented here for the application of SFC for clinical drug analysis using an open-tubular capillary column with polymethylsiloxane as the stationary phase. Preliminary studies of analysis of phenobarbital in serum showed that the use of liquid-liquid extractions, and recently introduced microfilters did not prevent rapid deterioration of column performance. Through systematic studies with solid-phase, C-18 extraction columns, a retention gap and a non-polar mixture of n-pentane/methylene chloride(25:75) for reconstituting the extracts, the feasibility was established. As a result of the lack of chromatographic interferences as shown by analysis of extract of drug-free serum, the procedure was used to estimate a patient's phenobarbital concentration of about 20 mg/L, comparable to a clinically established determination by fluorescence polarization immunoassay. Precision studies showed comparable mean concentrations for the measurement of quality control samples, ...

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