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Simultaneous estimation of E ‐ and Z ‐isomers of guggulsterone in rabbit plasma using liquid chromatography tandem mass spectrometry and its application to pharmacokinetic study
Author(s) -
Bhatta R. S.,
Kumar D.,
Chhonker Y. S.,
Jain G. K.
Publication year - 2011
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.1574
Subject(s) - chemistry , chromatography , formic acid , selected reaction monitoring , liquid chromatography–mass spectrometry , electrospray ionization , pharmacokinetics , analyte , calibration curve , mass spectrometry , tandem mass spectrometry , extraction (chemistry) , analytical chemistry (journal) , detection limit , medicine
Abstract A sensitive and selective liquid chromatography/tandem mass spectrometric method was developed for simultaneous determination of E ‐ and Z ‐guggulsterone isomers (antihyperlipidemic drug) in rabbit plasma. Both the isomers were resolved on a Symmetry‐Shield C 18 (5 µm, 4.6 × 150 mm) column, using gradient elution comprising a mobile phase of methanol, 0.5% v/v formic acid and acetonitrile. With dexamethasone as internal standard, plasma samples were extracted by an automated solid‐phase extraction method using C 18 cartridges. Detection was performed by electrospray ionization in multiple reaction monitoring (MRM) in positive mode. The calibration curve was linear over the concentration range of 1.56–200 ng/mL ( r 2 ≥ 0.998) for both analytes. The intra‐day and inter‐day accuracy and precision were within −0.96 to 4.12 (%bias) and 2.73 to 8.00 (%RSD) respectively. The analytes were stable after three freeze–thaw cycles. The method was successfully applied to study steriospecific pharmacokinetics of E ‐ and Z ‐guggulsterone in NZ rabbit. Copyright © 2011 John Wiley & Sons, Ltd.