Development of an HPLC-MS/MS Method for the Determination of Silybin in Human Plasma, Urine and Breast Tissue
Silybin is a flavonolignan extracted from <i>Silybum marianum</i> 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 can...
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doaj-c807306d567b4bfdb6f64dd27a2bdecb2020-11-25T03:55:43ZengMDPI AGMolecules1420-30492020-06-01252918291810.3390/molecules25122918Development of an HPLC-MS/MS Method for the Determination of Silybin in Human Plasma, Urine and Breast TissueMatteo Lazzeroni0Giovanna Petrangolini1José Antonio Legarreta Iriberri2Jaume Pascual Avellana3Digna Tost Robusté4Sara Cagnacci5Debora Macis6Valentina Aristarco7Bernardo Bonanni8Paolo Morazzoni9Harriet Johansson10Antonella Riva11IEO-European Institute of Oncology, Division of Cancer Prevention and Genetics, IRCCS, Via Ripamonti 435, 20141 Milan, ItalyResearch and Development Department, Indena S.p.A., Viale Ortles 12, 20139 Milan, ItalyBioanalysis Department, Kymos Pharma Services S.L., Ronda Can Fatjó 7-B, 08290 Cerdanyola del Vallès, SpainBioanalysis Department, Kymos Pharma Services S.L., Ronda Can Fatjó 7-B, 08290 Cerdanyola del Vallès, SpainBioanalysis Department, Kymos Pharma Services S.L., Ronda Can Fatjó 7-B, 08290 Cerdanyola del Vallès, SpainIEO-European Institute of Oncology, Division of Cancer Prevention and Genetics, IRCCS, Via Ripamonti 435, 20141 Milan, ItalyIEO-European Institute of Oncology, Division of Cancer Prevention and Genetics, IRCCS, Via Ripamonti 435, 20141 Milan, ItalyIEO-European Institute of Oncology, Division of Cancer Prevention and Genetics, IRCCS, Via Ripamonti 435, 20141 Milan, ItalyIEO-European Institute of Oncology, Division of Cancer Prevention and Genetics, IRCCS, Via Ripamonti 435, 20141 Milan, ItalyResearch and Development Department, Indena S.p.A., Viale Ortles 12, 20139 Milan, ItalyIEO-European Institute of Oncology, Division of Cancer Prevention and Genetics, IRCCS, Via Ripamonti 435, 20141 Milan, ItalyResearch and Development Department, Indena S.p.A., Viale Ortles 12, 20139 Milan, ItalySilybin is a flavonolignan extracted from <i>Silybum marianum</i> 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<sup>®</sup> 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.https://www.mdpi.com/1420-3049/25/12/2918silybinsilibininSiliphos<sup>®</sup>breast cancerHPLC-MS/MS method |
collection |
DOAJ |
language |
English |
format |
Article |
sources |
DOAJ |
author |
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 |
spellingShingle |
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 Development of an HPLC-MS/MS Method for the Determination of Silybin in Human Plasma, Urine and Breast Tissue Molecules silybin silibinin Siliphos<sup>®</sup> breast cancer HPLC-MS/MS method |
author_facet |
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 |
author_sort |
Matteo Lazzeroni |
title |
Development of an HPLC-MS/MS Method for the Determination of Silybin in Human Plasma, Urine and Breast Tissue |
title_short |
Development of an HPLC-MS/MS Method for the Determination of Silybin in Human Plasma, Urine and Breast Tissue |
title_full |
Development of an HPLC-MS/MS Method for the Determination of Silybin in Human Plasma, Urine and Breast Tissue |
title_fullStr |
Development of an HPLC-MS/MS Method for the Determination of Silybin in Human Plasma, Urine and Breast Tissue |
title_full_unstemmed |
Development of an HPLC-MS/MS Method for the Determination of Silybin in Human Plasma, Urine and Breast Tissue |
title_sort |
development of an hplc-ms/ms method for the determination of silybin in human plasma, urine and breast tissue |
publisher |
MDPI AG |
series |
Molecules |
issn |
1420-3049 |
publishDate |
2020-06-01 |
description |
Silybin is a flavonolignan extracted from <i>Silybum marianum</i> 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<sup>®</sup> 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. |
topic |
silybin silibinin Siliphos<sup>®</sup> breast cancer HPLC-MS/MS method |
url |
https://www.mdpi.com/1420-3049/25/12/2918 |
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