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Quantitative Ionspray Liquid Chromatographic/Tandem Mass Spectrometric Determination of Reserpine in Equine Plasma
Author(s) -
Anderson Melissa A.,
Wachs Timothy,
Henion Jack D.
Publication year - 1997
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(199702)32:2<152::aid-jms456>3.0.co;2-w
Subject(s) - chemistry , chromatography , extraction (chemistry) , solid phase extraction , liquid chromatography–mass spectrometry , mass spectrometry , tandem mass spectrometry , high performance liquid chromatography
A method based on ionspray liquid chromatography/tandem mass spectrometry (LC/MS/MS) was developed for the determination of reserpine in equine plasma. A comparison was made of the isolation of reserpine from plasma by liquid–liquid extraction and by solid‐phase extraction. A structural analog, rescinnamine, was used as the internal standard. The reconstituted extracts were analyzed by ionspray LC/MS/MS in the selected reaction monitoring (SRM) mode. The calibration graph for reserpine extracted from equine plasma obtained using liquid–liquid extraction was linear from 10 to 5000 pg ml ‐1 and that using solid‐phase extraction from 100 to 5000 pg ml ‐1 . The lower level of quantitation (LLQ) using liquid–liquid and solid‐phase extraction was 50 and 200 pg ml ‐1 , respectively. The lower level of detection for reserpine by LC/MS/MS was 10 pg ml ‐1 . The intra‐assay accuracy did not exceed 13% for liquid–liquid and 12% for solid‐phase extraction. The recoveries for the LLQ were 68% for liquid–liquid and 58% for solid‐phase extraction. © 1997 by John Wiley & Sons, Ltd.