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A rapid and sensitive liquid chromatography/positive ion tandem mass spectrometry method for the determination of cimetropium in human plasma by liquid–liquid extraction
Author(s) -
Lee HeonWoo,
Park WanSu,
Kim YongWon,
Cho SungHee,
Kim SungSu,
Seo JiHyung,
Lee KyungTae
Publication year - 2006
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/jms.1043
Subject(s) - chemistry , chromatography , ammonium formate , formic acid , selected reaction monitoring , detection limit , mass spectrometry , analyte , electrospray ionization , extraction (chemistry) , liquid chromatography–mass spectrometry , tandem mass spectrometry , high performance liquid chromatography , liquid–liquid extraction , electrospray , analytical chemistry (journal)
We have developed and validated a simple detection system with high‐performance liquid chromatography (HPLC) with positive ion electrospray ionization tandem mass spectrometry (ESI‐MS/MS) for determining cimetropium levels in human plasma using scopolamine butyl bromide as an internal standard (I.S.). The acquisition was performed in the multiple reaction monitoring (MRM) mode, by monitoring the transitions: m / z 357.9 > 103.1 for cimetropium and m / z 359.9 > 103.1 for butyl‐scopolamine. The method involves a simple single‐step liquid–liquid extraction with dichloromethane. The analyte was chromatographed on an YMC C18 reversed‐phase chromatographic column by isocratic elution with 10 m M ammonium formate buffer–methanol (19 : 81, v/v; adjusted to pH 4.0 with formic acid). The results were linear over the studied range (0.2–100 ng ml −1 ), with r 2 = 1.0000, and the total analysis time for each run was 2 min. Intra‐ and interassay precisions were 0.70–8.54% and 1.08–4.85%, respectively, and intra‐ and interassay accuracies were 97.56–108.23% and 97.48–103.91%, respectively. The lower limit of quantification (LLOQ) was 0.2 ng ml −1 . At this concentration, mean intra‐ and interassay precisions were 8.54% and 4.85%, respectively, and mean intra‐ and interassay accuracies were 97.56% and 98.91%, respectively. The mean recovery ranged from 62.71 ± 4.06 to 64.23 ± 2.32%. Cimetropium was found to be stable in plasma samples under typical storage and processing conditions. The devised assay was successfully applied to a pharmacokinetic study of cimetropium bromide administered as a single oral dose (150 mg) to healthy volunteers. Copyright © 2006 John Wiley & Sons, Ltd.