title: Automated on-line in-tube solid-phase microextraction coupled with HPLC/MS/MS for the determination of butyrophenone derivatives in human plasma.
abstract: This paper describes a fully automated on-line method combining in-tube solid-phase microextraction (SPME) in which sample clean-up and enrichment are conducted through an open tubular fused-silica capillary column and high-performance liquid chromatography (HPLC)/tandem mass spectrometry (MS/MS) detection for the determination of six butyrophenone derivatives (moperone, floropipamide, haloperidol, spiroperidol, bromperidol, and pimozide) in human plasma samples. The six butyrophenones were extracted by repeatedly aspirating and dispensing plasma sample solutions on a DB-17 capillary column (60 cm x 0.32 mm i.d., film thickness 0.25 microm). The analytes retained on the inner surface of the capillary column were then eluted into an acetonitrile-rich mobile phase using a gradient separation technique. Extraction efficiencies ranged from 12.7% to 31.8% for moperone, spiroperidol, and pimozide, and from 1.08% to 4.86% for floropipamide, haloperidol, and bromperidol. The regression equations for all compounds showed excellent linearity, ranging from 0.05 to 50 ng/0.1 mL of plasma, except for moperone and spiroperidol (0.01 to 50 ng/0.1 mL). The limits of detection and quantification in plasma for each drug were 0.03-0.2 and 0.1-0.5 ng/mL, respectively. The intra- and inter-day coefficients of variation for all compounds in plasma were not greater than 13.7%.
authors.affiliation: Department of Legal Medicine, Showa University School of Medicine, 1-5-8 Hatanodai, Shinagawa-ku, Tokyo, 142-8555, Japan. kumazawa@med.showa-u.ac.jp
authors.forename: Takeshi
authors.initials: T
authors.lastname: Kumazawa
authors.forename: Koichi
authors.initials: K
authors.lastname: Saeki
authors.forename: Isao
authors.initials: I
authors.lastname: Yanagisawa
authors.forename: Seisaku
authors.initials: S
authors.lastname: Uchigasaki
authors.forename: Chika
authors.initials: C
authors.lastname: Hasegawa
authors.forename: Hiroshi
authors.initials: H
authors.lastname: Seno
authors.forename: Osamu
authors.initials: O
authors.lastname: Suzuki
authors.forename: Keizo
authors.initials: K
authors.lastname: Sato
mesh_terms: D002090:Butyrophenones / Q000097:blood*; D002851:Chromatography, High Pressure Liquid; D006801:Humans; D012016:Reference Values; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052617:Solid Phase Microextraction / Q000379:methods*; D053719:Tandem Mass Spectrometry; D013997:Time Factors
chemical_list: D002090:Butyrophenones