Validation of a Liquid Chromatographic/Tandem Mass Spectrometric Method for the Determination of Scopolamine Butylbromide in Human Plasma: Application of the Method to a Bioequivalence Study

Validation of a Liquid Chromatographic/Tandem Mass Spectrometric Method for the Determination of Scopolamine Butylbromide in Human Plasma: Application of the Method to a Bioequivalence Study

A sensitive and specific LC/MS/MS method was developed and validated for the determination of scopolamine butylbromide in human plasma. Scopolamine butylbromide and propanolol (internal standard) were extracted from the plasma by liquid-liquid extraction with dichloromethane as the extraction solven...

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Bibliographic Details
Published in:Journal of AOAC International Vol. 92; no. 5; pp. 1366 - 1372
Main Authors: LARGER MANFIO, Josélia, BEDIM DOS SANTOS, Mauricio, JANN FAVRETO, Wagner Alex, HOFFMANN, Fabiane Ines, MERTIN, Adriana Cristina
Format: Journal Article
Language:English
Published: Gaithersburg, MD AOAC International 01-09-2009
Oxford University Press
Subjects:
Acetates - analysis
Adolescent
Adult
Biological and medical sciences
Chemistry Techniques, Analytical
Chemistry, Pharmaceutical - methods
Chromatography, Liquid - methods
Female
Food industries
Formates - analysis
Fundamental and applied biological sciences. Psychology
Humans
Hydrocarbons, Brominated - analysis
Hydrocarbons, Brominated - blood
Identification and classification
Liquid chromatography
Male
Mass spectrometry
Methods
Plasma - drug effects
Reproducibility of Results
Scopolamine
Scopolamine - analysis
Scopolamine - blood
Solvents - chemistry
Spectrometry, Mass, Electrospray Ionization - methods
Tandem Mass Spectrometry - methods
Temperature
United States
Human
Mass
Validation
Liquid chromatography
Application method
Method
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Summary:A sensitive and specific LC/MS/MS method was developed and validated for the determination of scopolamine butylbromide in human plasma. Scopolamine butylbromide and propanolol (internal standard) were extracted from the plasma by liquid-liquid extraction with dichloromethane as the extraction solvent and separated on a C18 analytical column (50 x 4.6 mm id) maintained at 40 degrees C. The analytes were eluted at a constant flow rate of 0.45 mL/min; the mobile phase consisted of acetonitrile and a buffer of 5 mM ammonium acetate and 0.1% formic acid (60 + 40, v/v). The mass spectrometer, equipped with an electrospray source in the positive ionization mode, was set up in the multiple-reaction monitoring mode to monitor the transitions m/z 360.6 > 102.5 (scopolamine butylbromide) and m/z 259.7 > 115.6 (propanolol). The chromatographic separation was obtained within 2.0 min, and the responses were linear over the concentration range of 0.10-40.00 ng/mL. The mean extraction recoveries of scopolamine butylbromide and propanolol from plasma were 69.00 and 80.76%, respectively. Method validation parameters, such as specificity, linearity, precision, accuracy, and stability, were within the acceptable range. Moreover, when the proposed method was successfully applied to a pharmacokinetic study of healthy human volunteers, the results showed that the two scopolamine butylbromide formulations tested are not bioequivalent in rate and extent of absorption.
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ISSN:1060-3271
1944-7922
DOI:10.1093/jaoac/92.5.1366