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Keywords:

  • liquid chromatography–ion trap mass spectrometry;
  • triptolide;
  • tripdiolide;
  • tripterine;
  • Tripterygium Wilfordii Hook. f;
  • human urine

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 C18 cartridges, a satisfactory separation was achieved on an XDB C18 short column (30 × 2.1 mm i.d., 3 µm) 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. Copyright © 2008 John Wiley & Sons, Ltd.