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Use of online‐dual‐column extraction in conjunction with chiral liquid chromatography tandem mass spectrometry for determination of terbutaline enantiomers in human plasma
Author(s) -
Xia YuanQing,
Liu David Q.,
Bakhtiar Ray
Publication year - 2002
Publication title -
chirality
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.43
H-Index - 77
eISSN - 1520-636X
pISSN - 0899-0042
DOI - 10.1002/chir.10135
Subject(s) - chemistry , chromatography , bioanalysis , extraction (chemistry) , mass spectrometry , tandem mass spectrometry , detection limit , atmospheric pressure chemical ionization , selected reaction monitoring , sample preparation , liquid chromatography–mass spectrometry , solid phase extraction , terbutaline , chemical ionization , analytical chemistry (journal) , ionization , medicine , asthma , ion , organic chemistry
An online sample extraction chiral bioanalytical method was developed and validated for the quantification of terbutaline, a β2‐selective adrenoceptor agonist, spiked into human plasma by using two extraction columns and a chiral stationary phase (CSP) in conjunction with liquid chromatography tandem mass spectrometry (LC‐MS/MS). In this method, two Oasis HLB extraction columns were used in parallel for plasma sample purification and a Chirobiotic T CSP was used for enantiomeric separation. Atmospheric pressure chemical ionization MS/MS was employed in multiple reaction monitoring mode for the detection and quantification. Subsequent to the addition of an internal standard solution, the plasma samples were directly injected onto the system for extraction and analysis. This method allowed the use of one of the extraction columns for purification while the other was being equilibrated. Hence, the time required for reconditioning the extraction columns did not contribute to the total analysis time per sample, which resulted in a shorter run time and higher throughput. A lower limit of quantification of 1.0 ng/mL was achieved using only 50 microliter of human plasma. The method was validated with a dynamic range of 1.0–200 ng/mL. The intra‐ and interday precision was no more than 11% CV and the assay accuracy was between 94–106%. Chirality 14:742–749, 2002. © 2002 Wiley‐Liss, Inc.