Monitoring aminopentamide urinary excretion by means of multiple 'microphase' extraction - a rapid method for the extraction and concentration of small amounts of lipophilic drugs from large volumes of biological fluids without distillation.

It has been demonstrated that low concentrations of basic lipophilic drugs in biological fluids may be extracted and concentrated 10(4)-10(6) times by a series of extraction procedures in which the ratio of the extracting solvent to that of the solution to be extracted is of the order of 1:100 (microphase extraction procedure). Typically, basic drugs (atropine, aminopentamide, hyoscine, chloroquine, pyrimethamine) were extracted and concentrated sufficiently for direct GC analysis from 24-hour urine samples by a procedure involving three simple consecutive extraction steps. Using this procedure, it was demonstrated that after administration of aminopentamide (300 micrograms) to patients in the form of anti-diarrhoeal tablets, measurable quantities of the free, unchanged drug can be demonstrated in 24-hour urine samples. The main advantages of the method are simplicity, rapidity and sensitivity due to the low background interference in the GC separations. The principle involved can be extended to the analysis of acidic drugs with suitable solubility properties.