title: Liquid-chromatographic determination of 4-aminopyridine in serum, saliva, and urine.
abstract: We have developed "high-performance" liquid-chromatographic methods for determining 4-aminopyridine, an acetylcholine-releasing drug, in serum, saliva, and urine. As little as 1 microgram/L can be detected by extracting the alkalinized sample plus the internal standard (3,4-diaminopyridine) into dichloromethane, mixing the organic phase with 1-pentanol, evaporating the dichloromethane, and injecting the residue onto a reversed-phase column, where it is eluted with acetonitrile/methanol/aqueous ammonium carbonate, with detection at 245 nm. Analytical recoveries from serum averaged 86.7%. The CV at 50 micrograms/L was 2.9% (n = 8). For urine samples containing very high concentrations of 4-aminopyridine, we mixed urine and potassium carbonate in an automatic injector vial, extracted the drug into dichloromethane, centrifuged, and injected an aliquot of the extract into the chromatograph. Analytical recoveries averaged 92%, and the CV was about 2% for drug concentrations of 0.1-8 mg/L of urine.
mesh_terms: D015761:4-Aminopyridine; D000631:Aminopyridines / Q000032:analysis* / Q000097:blood / Q000652:urine; D002851:Chromatography, High Pressure Liquid; D006801:Humans; D012463:Saliva / Q000032:analysis
chemical_list: D000631:Aminopyridines; D015761:4-Aminopyridine