Clinical Chemistry · 1979 · 13 citations · 0 references
PharmacyPharmaceutical AnalysisPharmacologyAnalytical ChemistryAnalytical ToxicologyChromatographic AnalysisAnalytical ChromatographyBioanalytical Method ValidationChromatographic Analysis Of PharmaceuticalsChromatographyGas ChromatographyMetabolite ExtractionChromatographic Residue DeterminationConcentrationInstrument Response FunctionsInternal Standard AnalysisInternal Standard EvaluationPrecision
In this procedure for disopyramide in serum, the drug is extracted into n-heptane/isobutanol (96/4 by vol), then back-extracted into 1 mol/L H2SO4. The acidic solution is made basic with sodium hydroxide, extracted with diethyl ether, and the extract evaporated. The residue is redissolved in ethanol and analyzed by gas-chromatography, with use of a nitrogen-selective detector. p-Chlorodisopyramide is used as internal standard. Concentration and instrument response for serum extracts are linearly related from 1 to 5 mg/L, the slope being 0.61, the y-intercept -0.10, the standard error of estimate 0.01, and the correlation coefficient 0.99. Within-run precision was 6 and 4% for 3 and 5 mg/L concentrations, respectively, with a between-run precision of 7% at the 3 mg/L concentration. Diazepam interferes, but procainamide, chlordiazepoxide, quinidine, lidocaine, propranolol, sulfanilamide, and many other basic drugs do not.