Determination of haloperidol and reduced haloperidol in human serum by liquid chromatography after fluorescence labeling based on the Suzuki coupling reaction

A simultaneous method for the determination of haloperidol (HP) and its metabolite, reduced haloperidol (RHP), in human serum was developed by means of high-performance liquid chromatography (HPLC) with fluorescence detection. Suzuki coupling reaction with a fluorescent arylboronic acid, 4-(4,5-diph...

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Bibliographic Details
Published in:Analytical and bioanalytical chemistry 2006-10, Vol.386 (3), p.719-724
Main Authors: Kishikawa, Naoya, Hamachi, Chiyuki, Imamura, Yoshihiro, Ohba, Yoshihito, Nakashima, Kenichiro, Tagawa, Yashuhiro, Kuroda, Naotaka
Format: Article
Language:English
Subjects:
Boron Compounds - chemistry
Chromatography, High Pressure Liquid - methods
Drug Monitoring
Female
Fluorescence
Fluorescence derivatization
Fluorescent arylboronic acid
haloperidol
Haloperidol - analogs & derivatives
Haloperidol - blood
Haloperidol - chemistry
Humans
Male
Molecular Structure
Oxidation-Reduction
Reduced haloperidol
Reference Values
Reproducibility of Results
Schizophrenia - blood
Sensitivity and Specificity
Suzuki coupling reaction
Therapeutic drug monitoring
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Summary:A simultaneous method for the determination of haloperidol (HP) and its metabolite, reduced haloperidol (RHP), in human serum was developed by means of high-performance liquid chromatography (HPLC) with fluorescence detection. Suzuki coupling reaction with a fluorescent arylboronic acid, 4-(4,5-diphenyl-1H-imidazol-2-yl)phenylboronic acid (DPA), was employed to convert HP and RHP into highly fluorescent compounds. HP and RHP were extracted from human serum by liquid-liquid extraction with a mixture of n-hexane and isoamyl alcohol (99:1, v/v) and subsequently labeled by reaction with DPA. Separation of DPA derivatives of HP and RHP was performed on a silica column with a mixture of acetonitrile and H₂O (90:10, v/v) containing triethylamine and acetic acid as a mobile phase. The proposed method allowed sensitive detection of HP and RHP in human serum with a detection limit (at a signal to noise ratio of 3) of 0.22 and 0.20 ng/mL, respectively. The applicability of the method for therapeutic drug monitoring (TDM) was demonstrated by analyzing human serum samples from schizophrenic patients receiving HP.
ISSN:1618-2642
1618-2650
DOI:10.1007/s00216-006-0755-0