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