Simultaneous determination of rupatadine and its metabolite desloratadine in human plasma by a sensitive LC-MS/MS method: application to the pharmacokinetic study in healthy Chinese volunteers

J Pharm Biomed Anal. 2009 Feb 20;49(2):347-53. doi: 10.1016/j.jpba.2008.10.014. Epub 2008 Nov 1.

Abstract

A sensitive liquid chromatography/tandem mass spectrometry (LC-MS/MS) method was developed for simultaneous determination of rupatadine and its metabolite desloratadine in human plasma. After the addition of diphenhydramine, the internal standard (IS), plasma samples were extracted with a mixture of methyl tert-butyl ether and n-hexane (1:1, v/v). The analysis was performed on a Ultimate AQ-C18 (4.6mm x 100mm, 5microm) column using a mobile phase consisting of a 80/20 mixture of methanol/water containing 0.0005% formic acid pumped at 0.3mlmin(-1). The analytes and the IS were detected in positive ionization mode and monitoring their precursor-->product ion combinations of m/z 416-->309, 311-->259, and 256-->167, respectively, in multiple reaction monitoring mode. The linear ranges of the assay were 0.1-50 and 0.1-20ngml(-1) for rupatadine and desloratadine, respectively. The lower limits of reliable quantification for both rupatadine and desloratadine were 0.1ngml(-1), which offered high sensitivity and selectivity. The within- and between-run precision was less than 7.2%. The accuracy ranged from -9.2% to +6.4% and -7.2% to +7.2% for rupatadine and desloratadine in quality control samples at three levels, respectively. The method has been successfully applied to a pharmacokinetic study of rupatadine and its major metabolite after oral administration of 10, 20 and 40mg rupatadine tablets to healthy Chinese volunteers.

MeSH terms

  • Adult
  • Asian People
  • Calibration
  • Chromatography, Liquid / instrumentation
  • Chromatography, Liquid / methods
  • Cyproheptadine / analogs & derivatives*
  • Cyproheptadine / blood
  • Cyproheptadine / chemistry
  • Cyproheptadine / pharmacokinetics
  • Drug Stability
  • Female
  • Formates / chemistry
  • Freezing
  • Histamine H1 Antagonists, Non-Sedating / blood*
  • Histamine H1 Antagonists, Non-Sedating / chemistry
  • Histamine H1 Antagonists, Non-Sedating / pharmacokinetics
  • Humans
  • Loratadine / analogs & derivatives*
  • Loratadine / blood
  • Loratadine / chemistry
  • Loratadine / pharmacokinetics
  • Male
  • Methanol / chemistry
  • Molecular Structure
  • Platelet Activating Factor / antagonists & inhibitors*
  • Platelet Activating Factor / chemistry
  • Quality Control
  • Reference Standards
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Tablets
  • Tandem Mass Spectrometry / methods*
  • Time Factors
  • Water / chemistry
  • Young Adult

Substances

  • Formates
  • Histamine H1 Antagonists, Non-Sedating
  • Platelet Activating Factor
  • Tablets
  • Water
  • formic acid
  • rupatadine
  • Cyproheptadine
  • Loratadine
  • desloratadine
  • Methanol