title: Simultaneous determination of triptolide, tripdiolide and tripterine in human urine by high-performance liquid chromatography coupled with ion trap atmospheric-pressure chemical ionization mass spectrometry.
abstract: An accurate and selective method for the simultaneous determination of triptolide, tripdiolide and tripterine in human urine using hydrocortisone as an internal standard (IS) by high-performance liquid chromatography coupled with atmospheric-pressure chemical ionization mass spectrometry in negative ion mode has been developed. After triptolide, tripdiolide and tripterine in human urine were extracted with ethyl acetate and cleaned by solid-phase extraction with C(18) cartridges, a satisfactory separation was achieved on an XDB C(18) short column (30 x 2.1 mm i.d., 3 microm) using the mobile phase of acetic acid-ammonium acetate (5 mmol/L, pH = 4.5)-acetonitrile-methanol in gradient elution. Detection was operated by APCI in selected ion monitoring mode. The target ions m/z 359, m/z 375, m/z 449 and m/z 419 were selected for the quantification of triptolide, tripdiolide, tripterine and IS, respectively. The linear range was 1.0-100.0 ng mL(-1), and the limits of quantification in human urine were found to be 0.1-0.5 ng mL(-1) for the three compounds. The precisions (CV%) and accuracies were 6.6-12.9 and 85.1-97.0%, respectively. The developed method could be applied to the determination of triptolide, tripdiolide and tripterine in human urine for diagnosis of the intoxication and for forensic purposes.
authors.affiliation: Ningbo Municipal Center for Disease Control and Prevention, People's Republic of China. jmcjc@163.com
authors.forename: Mi-cong
authors.initials: MC
authors.lastname: Jin
authors.forename: Xiao-hong
authors.initials: XH
authors.lastname: Chen
authors.forename: Xiao-kun
authors.initials: XK
authors.lastname: OuYang
mesh_terms: D002851:Chromatography, High Pressure Liquid; D004224:Diterpenes / Q000652:urine*; D004852:Epoxy Compounds / Q000652:urine; D006801:Humans; D006854:Hydrocortisone / Q000032:analysis; D016014:Linear Models; D008956:Models, Chemical; D053978:Pentacyclic Triterpenes; D010616:Phenanthrenes / Q000652:urine*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization; D014315:Triterpenes / Q000652:urine*
chemical_list: D004224:Diterpenes; D004852:Epoxy Compounds; D053978:Pentacyclic Triterpenes; D010616:Phenanthrenes; D014315:Triterpenes; C001899:triptolide; C001898:tripdiolide; C050414:celastrol; D006854:Hydrocortisone