title: High-performance liquid chromatography-electrospray tandem mass spectrometry for the measurement of 1-(3,4-dichlorobenzyl)-5-octylbiguanide in human serum.
abstract: 1-(3,4-dichlorobenzyl)-5-octylbiguanide (OPB-2045) is a new biguanide antimicrobial agent currently in clinical use as a topical bactericidal antiseptic. A method combining high-performance liquid chromatography (HPLC) with electrospray ionization (triple and quadruple stage) tandem mass spectrometry (ESI-MS/MS) was developed to quantify OPB-2045 in human serum. Solid phase extraction was performed on 0.2 ml of sample to ensure a high level of sensitivity before HPLC-ESI-MS/MS analysis. The limit of quantitation for the method was set at 0.05 ng/ml. Intra-assay and interassay precision were less than 13.7%, with a deviation from the expected value of no greater than 10.5% at a concentration range of 0.05 ng/ml to 5 ng/ml. Decomposition of OPB-2045 in human serum did not occur after storage for 15 months at -20 degrees C, even after three repetitions of freezing and thawing. Application of this method was demonstrated in a pharmacokinetic study of OPB-2045 in healthy patient subjects after a single topical application of 5 g/L preparation of its liquid formulation.
authors.affiliation: Tokushima Research Institute, Otsuka Pharmaceutical Co., Ltd., Japan.
authors.forename: S
authors.initials: S
authors.lastname: Kudo
authors.forename: Y
authors.initials: Y
authors.lastname: Mizooku
authors.forename: G
authors.initials: G
authors.lastname: Miyamoto
authors.forename: M
authors.initials: M
authors.lastname: Odomi
authors.forename: Y
authors.initials: Y
authors.lastname: Sogawa
authors.forename: T
authors.initials: T
authors.lastname: Sugai
mesh_terms: D000328:Adult; D000891:Anti-Infective Agents, Local / Q000097:blood*; D001645:Biguanides / Q000097:blood*; D002851:Chromatography, High Pressure Liquid; D004355:Drug Stability; D005615:Freezing; D006801:Humans; D008297:Male; D013058:Mass Spectrometry / Q000379:methods*; D015394:Molecular Structure; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D000891:Anti-Infective Agents, Local; D001645:Biguanides; C113749:olanexidine