Validation of an LC-MS/MS method for the determination of epirubicin in human serum of patients undergoing Drug Eluting Microsphere-Transarterial Chemoembolization (DEM-TACE)

Cristina Sottani, Emanuela Leoni, Benedetta Porro, Benedetta Montagna, Alessio Amatu, Federico Sottotetti, Pietro Quaretti, Guido Poggi, Claudio Minoia

Research output: Contribution to journalArticlepeer-review

Abstract

Drug Eluting Microsphere-Transarterial Chemoembolization (DEM-TACE) is a new delivery system to administrate drugs in a controlled manner useful for application in the chemoembolization of colorectal cancer metastases to the liver. DEM-TACE is focused to obtain higher concentrations of the drug to the tumor with lower systemic concentrations than traditional cancer chemotherapy. Therefore a specific, precise and sensitive LC-ESI-MS/MS assay procedure was properly designed to detect and quantify epirubicin at the concentrations expected from a transarterial chemoembolization with microspheres. Serum samples were kept acidic (pH approximately of 3.5) and sample preparation consisted of a solid phase extraction (SPE) procedure with HLB OASIS® cartridges using a methylene chloride/2-propanol/methanol mixture solution to recover epirubicin. The analyses consisted of reversed-phase high-performance liquid chromatography (rp-HPLC) coupled with tandem mass spectrometry (MS/MS). Accuracy, precision and matrix effect of this procedure were carried out by analyzing four quality control samples (QCs) on five separate days. The validation parameters were assessed by recovery studies of spiked serum samples. Recoveries were found to vary between 92 and 98% at the QC levels (5, 40, 80 and 150 μg/L) with relative standard deviation (RSD) always less than 3.7%. The limit of detection (LOD) was set at 1 μg/L. The developed procedure has been also applied to investigate the different capability of two types of commercially available microspheres to release epirubicin into the human circulatory system.

Original languageEnglish
Pages (from-to)3543-3548
Number of pages6
JournalJournal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences
Volume877
Issue number29
DOIs
Publication statusPublished - Nov 1 2009

Keywords

  • DC-Beads
  • Drug eluting microspheres
  • Epirubicin
  • Hepaspheres
  • LC-MS/MS
  • Validation

ASJC Scopus subject areas

  • Biochemistry
  • Analytical Chemistry
  • Cell Biology
  • Clinical Biochemistry

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