title: [An approach to complete the manual for determination of serum pirmenol levels].
abstract: In order to complete TDM manual for pirmenol in Sapporo Medical Center NTT East, we developed HPLC method and pretreatment procedure for pirmenol samples obtained from patients. Serum (250 microliters) was alkalinized and pirmenol was extracted into n-hexane, and then the drug was again extracted into an acidic solvent, 0.044 M KH2PO4 (pH 2.6) including 0.5% triethylamine. The aqueous extract was used for quantitative determination of the drug by HPLC. The mobile phase consisted of the above acidic solvent-acetonitrile (5:1, v/v) was delivered at 45 degrees C with a flow rate of 1 ml/min through a 4.6 mm x 25 cm ODS-3, a reversed-phase column. Detection of pirmenol and the internal standard (disopyramide) was achieved at 263 nm. Pirmenol and disopyramide was eluted at 5 and 11 min, respectively. Assay limit (25 ng/ml) and accuracy of the analytical method were satisfactory for TDM of pirmenol. During the HPLC analysis of patient samples, no substances that interfered with pirmenol detection were found. It was shown that 1) hemolysis did not affect pirmenol assay at all, 2) pirmenol was stable in the blood samples for at least 24 h even if they were stood at room temperature, and 3) pirmenol was stable for at least 3 days in frozen serum but there significant decrease was observed in pirmenol concentration after 7 days.
authors: Department of Pharmacy, Department of Cardiovascular Medicine, Sapporo Medical Center NTT East, South 1, West 15, Chuo-ku, Sapporo 060-0061, Japan.
authors: Junji
authors: J
authors: Asano
authors: Masakazu
authors: M
authors: Kojima
authors: Yuichi
authors: Y
authors: Sekizawa
authors: Toshiharu
authors: T
authors: Ooe
authors: Noriyuki
authors: N
authors: Miyamoto
authors: Yoshiyuki
authors: Y
authors: Suzuki
authors: Tetsuro
authors: T
authors: Kohya
authors: Michiya
authors: M
authors: Kobayashi
authors: Hiroshi
authors: H
authors: Saitoh
mesh_terms: D018927:Anti-Asthmatic Agents / Q000097:blood*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D016903:Drug Monitoring / Q000379:methods*; D006801:Humans; D010880:Piperidines / Q000097:blood*; D013048:Specimen Handling / Q000379:methods*
chemical_list: D018927:Anti-Asthmatic Agents; D010880:Piperidines; C024318:pirmenol