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Determination of ( R )‐ and ( S )‐ketoprofen in human plasma by liquid chromatography/tandem mass spectrometry following automated solid‐phase extraction in the 96‐well format
Author(s) -
Eichhold Thomas H.,
Bailey Ruth E.,
Tanguay Suzanne L.,
Hoke Steven H.
Publication year - 2000
Publication title -
journal of mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 1076-5174
DOI - 10.1002/(sici)1096-9888(200004)35:4<504::aid-jms958>3.0.co;2-l
Subject(s) - chemistry , chromatography , extraction (chemistry) , solid phase extraction , mass spectrometry , tandem mass spectrometry , ketoprofen , tandem , liquid chromatography–mass spectrometry , human plasma , materials science , composite material
A sensitive and selective method was developed for the determination of ( R )‐ketoprofen (( R )‐kt) and ( S )‐ketoprofen (( S )‐kt) in human plasma using chiral liquid chromatography/tandem mass spectrometry (LC/MS/MS). Plasma samples spiked with stable‐isotope‐labeled [ 13 C 1 , 2 H 3 ]‐( R and S )‐ketoprofen, for use as the internal standards, were prepared for analysis using automated solid‐phase extraction (SPE) in the 96‐well microtiter format. The enantiomers were separated on an ( R )‐1‐naphthylglycine and 3,5‐dinitrobenzoic acid (Chirex 3005) 250 × 2.0 mm i.d. analytical column, equipped with a 30 × 2.0 mm i.d. guard column using isocratic mobile phase conditions. The ( R )‐ and ( S )‐kt levels were quantifiable from 0.05 to 2500 ng ml −1 by constructing two separate curves from calibration standards covering the same range. The first curve ranged from 0.05 to 100 and the second from 100 to 2500 ng ml −1 . A concentration of 0.05 ng ml −1 of either enantiomer was easily detected using a 1 ml plasma sample volume. The average method accuracy, evaluated at four levels over an extended period, was better than ±3 % over the entire range. The precision for the same set of quality control samples ranged from 4.0 to 7.0 % RSD ( n = 24). The method was applied to the evaluation of pharmacokinetic parameters in human plasma obtained from volunteers who received 25 mg of kt by peroral administration of Actron caplets or by topical administration of Oruvail gel. Copyright © 2000 John Wiley & Sons, Ltd.