title: Determination and pharmacokinetic study of norcantharidin in human serum by HPLC-MS/MS method.
abstract: A sensitive, simple and selective high-performance liquid chromatography-tandem mass spectrometry method was developed and applied to the determination of norcantharidin concentration in human serum. Norcantharidin (NCTD) and cyclophosphamide (IS) in serum were extracted with acetone, separated on a C18 reversed-phase column, gradiently eluted with a mobile phase of acetonitrile-water containing 2 mm ammonium acetate and 0.1% formic acid (pH 3), ionized by positive ion pneumatically assisted electrospray and detected in the multi-reaction monitoring mode using precursor-->product ions of m/z 169.3-->123.1 for NCTD and 261.2-->140.2 for IS, respectively. The linear range of the calibration curve for NCTD was 2.5-50 ng/mL, with a lowest limit of quantification of 2.5 ng/mL, and the intra/inter-day RSD was less than 10%. The method was suitable for determination of low NCTD concentration in human serum after therapeutic oral doses, and has been successfully used for pharmacokinetic studies in healthy Chinese volunteers.
authors.affiliation: Institute of Clinical Pharmacology, Qilu Hospital of Shandong University, Jinan 250012, People's Republic of China.
authors.forename: Chun-min
authors.initials: CM
authors.lastname: Wei
authors.forename: Rui
authors.initials: R
authors.lastname: Zhang
authors.forename: Ben-jie
authors.initials: BJ
authors.lastname: Wang
authors.forename: Gui-yan
authors.initials: GY
authors.lastname: Yuan
authors.forename: Rui-chen
authors.initials: RC
authors.lastname: Guo
mesh_terms: D000096:Acetone / Q000737:chemistry; D000097:Acetonitriles / Q000737:chemistry; D000284:Administration, Oral; D000328:Adult; D019086:Bridged Bicyclo Compounds, Heterocyclic / Q000097:blood* / Q000493:pharmacokinetics; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003520:Cyclophosphamide / Q000097:blood / Q000493:pharmacokinetics; D005260:Female; D006801:Humans; D057927:Hydrophobic and Hydrophilic Interactions; D008297:Male; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014867:Water / Q000737:chemistry
chemical_list: D000097:Acetonitriles; D019086:Bridged Bicyclo Compounds, Heterocyclic; D014867:Water; D000096:Acetone; C069741:norcantharidin; D003520:Cyclophosphamide; C032159:acetonitrile