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Chiral analysis of butaclamol enantiomers in human plasma by HPLC using a macrocyclic antibiotic (vancomycin) chiral stationary phase and solid phase extraction
Author(s) -
AboulEnein Hassan Y.,
Hefnawy Mohamed M.
Publication year - 2004
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.20001
Subject(s) - chemistry , chromatography , high performance liquid chromatography , enantiomer , solid phase extraction , detection limit , extraction (chemistry) , triethylamine , acetic acid , stereochemistry , organic chemistry
An enantioseparation of the antipsychotic drug butaclamol in human plasma by high‐performance liquid chromatography (HPLC) with solid phase extraction is presented. The separation was achieved on the vancomycin macrocyclic antibiotic chiral stationary phase (CSP) Chirobiotic V with a polar ionic mobile phase (PIM) consisting of methanol : glacial acetic acid : triethylamine (100:0.2:0.05, v/v/v) at a flow rate of 0.5 ml/min. The detection wavelength was 262 nm. Bond Elut C18 solid phase extraction cartridges were used in the sample preparation of butaclamol samples from plasma. The method was validated over the range of 100–3,000 ng/ml for each enantiomer concentration (R 2 > 0.999). Recoveries for (+)‐ and (−)‐butaclamol were in the range of 94–104% at the 300–2,500 ng/ml level. The method proved to be precise (within‐run precision ranged from 1.1–2.6% and between‐run precision ranged from 1.9–3.2%) and accurate (within‐run accuracies ranged from 1.5–5.8% and between‐run accuracies ranged from 2.7–7.7%). The limit of quantitation (LOQ) and limit of detection (LOD) for each enantiomer in human plasma were 100 ng/ml and 50 ng/ml, respectively. Chirality 16:147–152, 2004 . © 2004 Wiley‐Liss, Inc.