title: Determination of nalbuphine by high-performance liquid chromatography with electrochemical detection: application to clinical samples from postoperative patients.
abstract: A rapid, selective and reproducible high-performance liquid chromatographic assay with electrochemical detection was developed for the determination of nalbuphine in human plasma. The method involves extraction with chloroform-isopropanol at pH 9.4, back-extraction into dilute phosphoric acid and reversed-phase chromatography on a microBondapak phenyl column. The recovery of nalbuphine and naltrexone (internal standard) was greater than 90%. Calibration curves were linear over a concentration range of 3-36 ng/ml with coefficients of variation, within-day or between-day, not exceeding 8% at any level. Although the limit of detection was 0.3 ng/ml based on a signal-to-noise ratio of 3, the reliable limit of quantitation was 1 ng/ml (coefficient of variation 12%) using 1 ml of plasma. The dual-electrode detector was operated in the screening mode of oxidation (electrode 1, 0.3 V and electrode 2, 0.6 V), providing a greater specificity and reducing background noise. This procedure was applied to a large number of clinical samples in an intravenous dose-range pharmacokinetic study in patients.
authors.affiliation: Bureau of Drug Research, Health Protection Branch, Ottawa, Ontario, Canada.
authors.forename: L M
authors.initials: LM
authors.lastname: Dubé
authors.forename: N
authors.initials: N
authors.lastname: Beaudoin
authors.forename: M
authors.initials: M
authors.lastname: Lalande
authors.forename: I J
authors.initials: IJ
authors.lastname: McGilveray
mesh_terms: D002851:Chromatography, High Pressure Liquid; D004563:Electrochemistry; D006207:Half-Life; D006801:Humans; D009019:Morphinans / Q000097:blood*; D009266:Nalbuphine / Q000097:blood* / Q000493:pharmacokinetics; D011184:Postoperative Period
chemical_list: D009019:Morphinans; D009266:Nalbuphine