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A liquid chromatography-mass spectrometry assay method for simultaneous determination of amiodarone and desethylamiodarone in rat specimens.
Biomed Chromatogr. 2007 Mar; 21(3):284-90.BC

Abstract

A liquid chromatographic-mass spectrometry (LC/MS) assay method was developed for the determination of amiodarone and desethylamiodarone in rat specimens. Analytes were extracted using liquid-liquid extraction in hexane. The LC/MS system consisted of a Waters Micromass ZQtrade mark 4000 spectrometer with an autosampler and pump. A C(18) 3.5 microm (2.1 x 50 mm) column heated to 45 degrees C was used for separation. The mobile phase consisted of methanol and 0.2% aqueous formic acid pumped at 0.2 mL/min as a linear gradient. Components eluted within 12 min. The concentrations of ethopropazine (internal standard), desethylamiodarone and amiodarone were monitored for m/z of 313.10, combination of 546.9 and 617.73, and 645.83, respectively. In plasma (0.1 mL), linearity was achieved between the peak area ratios and concentrations over the range of 2.5-1000 ng/mL for both amiodarone and desethylamiodarone (r(2) > 0.999). The intraday and interday CV were equal or less than 18%, and mean error was <12%. Similarly, in homogenates containing 0.1 g of rat tissue, linearity was observed in standards ranging from 5 to 5000 ng/g. The method was successfully used to measure tissue and plasma concentrations of drug. The validated lower limit of quantitation was 2.5 ng/mL for drug and metabolite, based on 0.1 mL of plasma.

Authors+Show Affiliations

Shayeganpour A
Faculty of Pharmacy and Pharmaceutical Sciences, University of Alberta, Edmonton, Alberta, Canada T6G 2N8.
Somayaji V
No affiliation info available
Brocks DR
No affiliation info available

MeSH

AmiodaroneAnimalsCalibrationChromatography, High Pressure LiquidInjections, IntravenousLinear ModelsMolecular StructurePhenothiazinesRatsRats, Sprague-DawleyReproducibility of ResultsSensitivity and SpecificitySpectrometry, Mass, Electrospray IonizationTissue Distribution

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

17221913

Citation

Shayeganpour, Anooshirvan, et al. "A Liquid Chromatography-mass Spectrometry Assay Method for Simultaneous Determination of Amiodarone and Desethylamiodarone in Rat Specimens." Biomedical Chromatography : BMC, vol. 21, no. 3, 2007, pp. 284-90.
Shayeganpour A, Somayaji V, Brocks DR. A liquid chromatography-mass spectrometry assay method for simultaneous determination of amiodarone and desethylamiodarone in rat specimens. Biomed Chromatogr. 2007;21(3):284-90.
Shayeganpour, A., Somayaji, V., & Brocks, D. R. (2007). A liquid chromatography-mass spectrometry assay method for simultaneous determination of amiodarone and desethylamiodarone in rat specimens. Biomedical Chromatography : BMC, 21(3), 284-90.
Shayeganpour A, Somayaji V, Brocks DR. A Liquid Chromatography-mass Spectrometry Assay Method for Simultaneous Determination of Amiodarone and Desethylamiodarone in Rat Specimens. Biomed Chromatogr. 2007;21(3):284-90. PubMed PMID: 17221913.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - A liquid chromatography-mass spectrometry assay method for simultaneous determination of amiodarone and desethylamiodarone in rat specimens. AU - Shayeganpour,Anooshirvan, AU - Somayaji,Vishwa, AU - Brocks,Dion R, PY - 2007/1/16/pubmed PY - 2007/6/6/medline PY - 2007/1/16/entrez SP - 284 EP - 90 JF - Biomedical chromatography : BMC JO - Biomed Chromatogr VL - 21 IS - 3 N2 - A liquid chromatographic-mass spectrometry (LC/MS) assay method was developed for the determination of amiodarone and desethylamiodarone in rat specimens. Analytes were extracted using liquid-liquid extraction in hexane. The LC/MS system consisted of a Waters Micromass ZQtrade mark 4000 spectrometer with an autosampler and pump. A C(18) 3.5 microm (2.1 x 50 mm) column heated to 45 degrees C was used for separation. The mobile phase consisted of methanol and 0.2% aqueous formic acid pumped at 0.2 mL/min as a linear gradient. Components eluted within 12 min. The concentrations of ethopropazine (internal standard), desethylamiodarone and amiodarone were monitored for m/z of 313.10, combination of 546.9 and 617.73, and 645.83, respectively. In plasma (0.1 mL), linearity was achieved between the peak area ratios and concentrations over the range of 2.5-1000 ng/mL for both amiodarone and desethylamiodarone (r(2) > 0.999). The intraday and interday CV were equal or less than 18%, and mean error was <12%. Similarly, in homogenates containing 0.1 g of rat tissue, linearity was observed in standards ranging from 5 to 5000 ng/g. The method was successfully used to measure tissue and plasma concentrations of drug. The validated lower limit of quantitation was 2.5 ng/mL for drug and metabolite, based on 0.1 mL of plasma. SN - 0269-3879 UR - https://www.unboundmedicine.com/medline/citation/17221913/A_liquid_chromatography_mass_spectrometry_assay_method_for_simultaneous_determination_of_amiodarone_and_desethylamiodarone_in_rat_specimens_ L2 - https://doi.org/10.1002/bmc.754 DB - PRIME DP - Unbound Medicine ER -