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Analysis of a basic drug by on‐line solid‐phase extraction liquid chromatography/tandem mass spectrometry using a mixed mode sorbent
Author(s) -
Mallet Claude R,
Lu Ziling,
Mazzeo Jeff,
Neue Uwe
Publication year - 2002
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.639
Subject(s) - chemistry , chromatography , cartridge , sorbent , solid phase extraction , extraction (chemistry) , mass spectrometry , selected reaction monitoring , liquid chromatography–mass spectrometry , calibration curve , analytical chemistry (journal) , sample preparation , tandem mass spectrometry , detection limit , adsorption , mechanical engineering , organic chemistry , engineering
Two on‐line configurations using multiple 6‐ and 10‐port valves were investigated for high‐flow on‐line extraction of a basic drug in rat plasma and human urine using a reversed‐phase and a cation‐exchange SPE sorbent. The first configuration studied was a single reversed‐phase extraction cartridge (2.1 × 20 mm, 25µm) using an optimized washing protocol. The results showed that up to 1.5 mL of sample (urine or plasma diluted 1:1) can be injected with limits of quantification (LOQs) as low as 100 pg/mL. The second configuration studied was the combination of a cation exchanger and a reversed‐phase cartridge using at‐column dilution. The results showed better LOQs than those obtained with the single cartridge at 10 pg/mL with the same injection volume. The mass spectrometer was operated in the multiple reaction monitoring (MRM) mode. All calibration curves gave an average of 5% relative standard deviation (RSD). Copyright © 2002 John Wiley & Sons, Ltd.