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Simultaneous quantitative analysis of ketanserin and ketanserinol in plasma by RP‐HPLC with fluorescence detection
Author(s) -
Yassen A.,
Hanff L. M.,
Vulto A. G.
Publication year - 2003
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.265
Subject(s) - chromatography , ketanserin , repeatability , chemistry , detection limit , calibration curve , extraction (chemistry) , analyte , analytical chemistry (journal) , reproducibility , high performance liquid chromatography , solid phase extraction , quantitative analysis (chemistry) , coefficient of variation , receptor , 5 ht receptor , biochemistry , serotonin
A sensitive and selective high‐performance liquid chromatographic assay for the quantication of ketanserin and ketanserinol in human plasma was developed and validated. The procedure involves extraction of ketanserin and ketanserinol from plasma using an Extrelut NT‐1 solid‐phase extraction column. The chromatograph was equipped with a Hypersil BDS column (100 × 4.5 mm, 3 µm particle size). Separation was performed with a mixture of acetate buffer 0.01 M, pH 4.9–methanol–acetonitrile (52:40:8, v/v/v). Detection was performed with uorescence detection ( λ ex = 332 nm and λ em = 410 nm). Calibration curves were linear ( r 2 = 0.999) in the range 0–400 ng/mL for both ketanserin and ketanserinol. The repeatability coefcient for ketanserin and ketanserinol was 3.1 and 3.0%, respectively. The reproducibility coefcient for ketanserin and ketanserinol was 10.5 and 9.1%, respectively. The limit of quantication for both ketanserin and ketanserinol was 2.0 ng/mL. The mean recovery yield for both ketanserin and ketanserinol was 60%. In an 8 h work day approximately 60 samples, including calibration and reference standards, could be processed. Copyright © 2003 John Wiley & Sons, Ltd.