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

Abstract:

: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 r(2) 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.

journal_name

J Pharm Biomed Anal

authors

Jacobson GA,Chong FV,Davies NW

doi

10.1016/s0731-7085(02)00734-3

subject

Has Abstract

pub_date

2003-04-10 00:00:00

pages

1237-43

issue

6

eissn

0731-7085

issn

1873-264X

pii

S0731708502007343

journal_volume

31

pub_type

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