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LC-MS method for the determination of albuterol enantiomers in human plasma using manual solid-phase extraction and a non-deuterated internal standard

journal contribution
posted on 2023-05-16, 14:43 authored by Glenn JacobsonGlenn Jacobson, Chong, FV, Noel DaviesNoel Davies
A sensitive enantioselective liquid chromatography–mass spectrometry (LC–MS) assay using a manual solid-phase extraction (SPE) procedure, a non-deuterated internal standard and an ion trap LC–MS was developed to measure (R)- and (S)-albuterol in plasma. Sample extraction from plasma was achieved by a manual SPE extraction procedure with methoxyphenamine added as the internal standard. Chiral separation was achieved using a teicoplanin-based stationary phase and a mobile phase consisting of methanol, acetic acid and 28% (w/v) ammonia (1000:5:1, v/v/v). Samples were analyzed by selected reaction monitoring of product ions from the protonated molecular ions. The detection limit of the assay was 0.1 ng/ml with a conservative lower limit of quantification of 0.25 ng/ml for each enantiomer. Recovery of albuterol enantiomers from plasma spiked at 10 ng/ml of racemate was determined to be 89±5.8% (mean±S.D.). Reproducibility at 10 ng/ml of racemate assessed by the coefficient of variation was found to be 6.5% (n=5). Instrument precision (measured as coefficient of variation) was 1.4% (n=5). The correlation coefficient r2 determined from the calibration curve over the range 0.5–50.0 ng/ml racemate in plasma was 0.998. This assay allows adequate sensitivity, recovery and reproducibility for the application to studies of inhaled albuterol.


Publication title

Journal of Pharmaceutical and Biomedical Analysis










School of Pharmacy and Pharmacology


Pergamon-Elsevier Science Ltd

Place of publication

Oxford, England

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Socio-economic Objectives

Other health not elsewhere classified

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