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A sensitive LC-MS/MS assay for the simultaneous analysis of the major active components of silymarin in human plasma.

Abstract

Silymarin, an extract of crushed achenes of the milk thistle plant Silybum marianum is a multi-constituent mixture, 70-80% of which consists of a complex assortment containing the flavonolignans silybin A and B, isosilybin A and B, silydianin, and silychristin, and the flavonoid taxifolin. To date, numerous pharmacological actions of the silymarin extract have been documented in the biomedical literature, including hepatoprotective, anti-inflammatory, anti-tumor, and anti-fibrotic activities. The present study describes a novel liquid chromatographic-tandem mass spectrometric method for simultaneous analysis of silychristin, silydianin, silybin A and silybin B, isosilybin A and isosilybin B, and taxifolin in human plasma employing liquid-liquid extraction. This assay provides excellent resolution of the individual silymarin constituents via utilization of a 100 A 250 mm × 2 mm, 5 μm C(18) column with the mobile phase consisting of 51% methanol, 0.1% formic acid, and 10mM ammonium acetate. The lower limit of quantification was 2 ng/ml for each constituent. Calibration curves were linear over the range from 2 ng/ml to 100 ng/ml for all analytes (r(2)>0.99). The intra- and inter-day accuracies were 91-106.5% and 95.1-111.9%, respectively. The intra- and inter-day precision was within 10.5%. Additionally, recovery, stability, and matrix effects were fully validated as well. This method was successfully applied to human plasma samples from subjects treated with the milk thistle extract Legalon(®).

Authors+Show Affiliations

Department of Pharmacotherapy and Translational Research, University of Florida, Gainesville, FL 32610-0486 , USA.No affiliation info availableNo affiliation info available

Pub Type(s)

Clinical Trial
Journal Article
Research Support, N.I.H., Extramural

Language

eng

PubMed ID

22766231

Citation

Brinda, Bryan J., et al. "A Sensitive LC-MS/MS Assay for the Simultaneous Analysis of the Major Active Components of Silymarin in Human Plasma." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 902, 2012, pp. 1-9.
Brinda BJ, Zhu HJ, Markowitz JS. A sensitive LC-MS/MS assay for the simultaneous analysis of the major active components of silymarin in human plasma. J Chromatogr B Analyt Technol Biomed Life Sci. 2012;902:1-9.
Brinda, B. J., Zhu, H. J., & Markowitz, J. S. (2012). A sensitive LC-MS/MS assay for the simultaneous analysis of the major active components of silymarin in human plasma. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 902, 1-9. https://doi.org/10.1016/j.jchromb.2012.06.003
Brinda BJ, Zhu HJ, Markowitz JS. A Sensitive LC-MS/MS Assay for the Simultaneous Analysis of the Major Active Components of Silymarin in Human Plasma. J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Aug 1;902:1-9. PubMed PMID: 22766231.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - A sensitive LC-MS/MS assay for the simultaneous analysis of the major active components of silymarin in human plasma. AU - Brinda,Bryan J, AU - Zhu,Hao-Jie, AU - Markowitz,John S, Y1 - 2012/06/12/ PY - 2012/04/03/received PY - 2012/05/30/revised PY - 2012/06/01/accepted PY - 2012/7/7/entrez PY - 2012/7/7/pubmed PY - 2012/11/6/medline SP - 1 EP - 9 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. VL - 902 N2 - Silymarin, an extract of crushed achenes of the milk thistle plant Silybum marianum is a multi-constituent mixture, 70-80% of which consists of a complex assortment containing the flavonolignans silybin A and B, isosilybin A and B, silydianin, and silychristin, and the flavonoid taxifolin. To date, numerous pharmacological actions of the silymarin extract have been documented in the biomedical literature, including hepatoprotective, anti-inflammatory, anti-tumor, and anti-fibrotic activities. The present study describes a novel liquid chromatographic-tandem mass spectrometric method for simultaneous analysis of silychristin, silydianin, silybin A and silybin B, isosilybin A and isosilybin B, and taxifolin in human plasma employing liquid-liquid extraction. This assay provides excellent resolution of the individual silymarin constituents via utilization of a 100 A 250 mm × 2 mm, 5 μm C(18) column with the mobile phase consisting of 51% methanol, 0.1% formic acid, and 10mM ammonium acetate. The lower limit of quantification was 2 ng/ml for each constituent. Calibration curves were linear over the range from 2 ng/ml to 100 ng/ml for all analytes (r(2)>0.99). The intra- and inter-day accuracies were 91-106.5% and 95.1-111.9%, respectively. The intra- and inter-day precision was within 10.5%. Additionally, recovery, stability, and matrix effects were fully validated as well. This method was successfully applied to human plasma samples from subjects treated with the milk thistle extract Legalon(®). SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/22766231/A_sensitive_LC_MS/MS_assay_for_the_simultaneous_analysis_of_the_major_active_components_of_silymarin_in_human_plasma_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(12)00339-X DB - PRIME DP - Unbound Medicine ER -