Development of an HPLC-MS/MS method for the determination of silybin in human plasma, urine and breast tissue

Matteo Lazzeroni, Giovanna Petrangolini, José Antonio Legarreta Iriberri, Jaume Pascual Avellana, Digna Tost Robusté, Sara Cagnacci, Debora Macis, Valentina Aristarco, Bernardo Bonanni, Paolo Morazzoni, Harriet Johansson, Antonella Riva

Research output: Contribution to journalArticlepeer-review

Abstract

Silybin is a flavonolignan extracted from Silybum marianum with chemopreventive activity against various cancers, including breast. This study was designed to develop an HPLC-MS/MS method for the determination of silybin in human plasma, urine and breast tissue in early breast cancer patients undergoing Siliphos® supplementation, an oral silybin-phosphatidylcholine complex. The determination of silybin was carried out by liquid–liquid extraction with methyl-tert-butyl ether (MTBE); total silybin concentration was determined by treating the samples with β–glucuronidase, while for the determination of free silybin, the hydrolytic step was omitted. Naringenin and naproxen were selected as internal standards. The detection of the analyte was carried out by mass spectrometry and by chromatography. The HPLC-MS/MS method was evaluated in terms of selectivity, linearity, limit of quantification, precision and accuracy, and carryover. The method proved to be selective, linear, precise and accurate for the determination of silybin. To the best of our knowledge, this presents the first analytical method with the capacity to quantify the major bioactive components of milk thistle in three different biological matrices with a lower limit of quantification of 0.5 ng/mL for plasma. Silybin phosphatidylcholine, taken orally, can deliver high blood concentrations of silybin, which selectively accumulates in breast tumor tissue.

Original languageEnglish
Article number2918
JournalMolecules
Volume25
Issue number12
DOIs
Publication statusPublished - Jun 2020

Keywords

  • Breast cancer
  • HPLC-MS/MS method
  • Silibinin
  • Siliphos
  • Silybin

ASJC Scopus subject areas

  • Analytical Chemistry
  • Chemistry (miscellaneous)
  • Molecular Medicine
  • Pharmaceutical Science
  • Drug Discovery
  • Physical and Theoretical Chemistry
  • Organic Chemistry

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