{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,10,7]],"date-time":"2026-10-07T16:17:06Z","timestamp":1791389826428,"version":"4.3.3"},"reference-count":35,"publisher":"Wiley","issue":"4","license":[{"start":{"date-parts":[[2024,11,17]],"date-time":"2024-11-17T00:00:00Z","timestamp":1731801600000},"content-version":"vor","delay-in-days":0,"URL":"http:\/\/creativecommons.org\/licenses\/by-nc-nd\/4.0\/"}],"content-domain":{"domain":["analyticalsciencejournals.onlinelibrary.wiley.com"],"crossmark-restriction":true},"short-container-title":["Phytochemical Analysis"],"published-print":{"date-parts":[[2025,6]]},"abstract":"<jats:title>ABSTRACT<\/jats:title><jats:sec><jats:title>Introduction<\/jats:title><jats:p>Nutricosmetics derived from <jats:styled-content style=\"fixed-case\"><jats:italic>Silybum marianum<\/jats:italic><\/jats:styled-content>, known for their anti\u2010inflammatory and hepatoprotective properties, necessitate accurate quantification of silybin, a key bioactive component.<\/jats:p><\/jats:sec><jats:sec><jats:title>Objectives<\/jats:title><jats:p>This study aims to develop a novel high\u2010performance liquid chromatography (HPLC) method with amperometric detection (HPLC\u2010ECD) for the precise determination of silybin. An ultrasound\u2010assisted extraction (UAE) procedure is also established for solid sample preparation prior to chromatographic analysis.<\/jats:p><\/jats:sec><jats:sec><jats:title>Materials and Methods<\/jats:title><jats:p>Chromatographic separation of silybin was performed on a C18 column and using methanol\u20130.035\u2009M potassium phosphate (pH\u20094.0) at 1.0\u2009mL\u2009min<jats:sup>\u22121<\/jats:sup> flow rate as mobile phase in gradient mode. The electrochemical detection (ECD) of silybin was carried out on a glassy carbon electrode (GCE) at +1.10\u2009V versus Ag\/AgCl. The UAE procedure for silybin extraction from solid samples was performed by 15\u2009min sonication in an ultrasonic bath (80\u2009kHz and 100% power) at room temperature.<\/jats:p><\/jats:sec><jats:sec><jats:title>Results<\/jats:title><jats:p>Under the optimal chromatographic conditions, silybin diastereoisomers (silybin A and silybin B) can be separated from other <jats:styled-content style=\"fixed-case\"><jats:italic>S.\u2009marianum<\/jats:italic><\/jats:styled-content> flavonolignans in less than 20\u2009min, with a detection limit (LOD) of 0.060\u2009mg\u2009L<jats:sup>\u22121<\/jats:sup> and a reproducibility (RSD) of 5%. This method was successfully applied to analyze silymarin\u2010containing products with recoveries close to 100%.<\/jats:p><\/jats:sec><jats:sec><jats:title>Conclusions<\/jats:title><jats:p>This work presents the first HPLC method for silybin determination using an amperometric detector with a GCE. The LOD is competitive in comparison with previously published HPLC\u2010DAD methods. This HPLC\u2010ECD method allows silybin diastereoisomers identification without interferences of other flavonolignans present in silymarin extracts.<\/jats:p><\/jats:sec>","DOI":"10.1002\/pca.3478","type":"journal-article","created":{"date-parts":[[2024,11,17]],"date-time":"2024-11-17T20:55:07Z","timestamp":1731876907000},"page":"934-942","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":4,"title":["Determination of the Major Bioactive Component of <scp><i>Silybum marianum<\/i><\/scp> in Nutricosmetics by a HPLC Method With Amperometric Detection and UAE Pretreatment"],"prefix":"10.1002","volume":"36","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-0296-8053","authenticated-orcid":false,"given":"Luc\u00eda","family":"Abad\u2010Gil","sequence":"first","affiliation":[{"name":"Departamento de Qu\u00edmica Anal\u00edtica y An\u00e1lisis Instrumental, Facultad de Ciencias Universidad Aut\u00f3noma de Madrid  Madrid Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6344-0148","authenticated-orcid":false,"given":"M.\u00a0Jes\u00fas","family":"Gismera","sequence":"additional","affiliation":[{"name":"Departamento de Qu\u00edmica Anal\u00edtica y An\u00e1lisis Instrumental, Facultad de Ciencias Universidad Aut\u00f3noma de Madrid  Madrid Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0016-9714","authenticated-orcid":false,"given":"M.\u00a0Teresa","family":"Sevilla","sequence":"additional","affiliation":[{"name":"Departamento de Qu\u00edmica Anal\u00edtica y An\u00e1lisis Instrumental, Facultad de Ciencias Universidad Aut\u00f3noma de Madrid  Madrid Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1200-8408","authenticated-orcid":false,"given":"Jes\u00fas\u00a0R.","family":"Procopio","sequence":"additional","affiliation":[{"name":"Departamento de Qu\u00edmica Anal\u00edtica y An\u00e1lisis Instrumental, Facultad de Ciencias Universidad Aut\u00f3noma de Madrid  Madrid Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2024,11,17]]},"reference":[{"key":"e_1_2_6_2_1","first-page":"583","volume-title":"Handbook of Cosmetic Science and Technology","author":"Taeymans J.","year":"2014"},{"key":"e_1_2_6_3_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.tifs.2019.11.015"},{"key":"e_1_2_6_4_1","doi-asserted-by":"publisher","DOI":"10.1111\/j.1473\u20102165.2011.00600.x"},{"key":"e_1_2_6_5_1","doi-asserted-by":"publisher","DOI":"10.3390\/molecules22111942"},{"key":"e_1_2_6_6_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.jpba.2016.05.034"},{"key":"e_1_2_6_7_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.jff.2023.105502"},{"key":"e_1_2_6_8_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.biopha.2021.112024"},{"key":"e_1_2_6_9_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.jddst.2023.104378"},{"key":"e_1_2_6_10_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.clindermatol.2021.05.007"},{"key":"e_1_2_6_11_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.clindermatol.2009.05.012"},{"key":"e_1_2_6_12_1","doi-asserted-by":"publisher","DOI":"10.20307\/nps.2021.27.2.68"},{"key":"e_1_2_6_13_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.biopha.2022.113593"},{"key":"e_1_2_6_14_1","doi-asserted-by":"publisher","DOI":"10.3390\/ijms22157885"},{"key":"e_1_2_6_15_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.bbapap.2022.140772"},{"key":"e_1_2_6_16_1","doi-asserted-by":"publisher","DOI":"10.3390\/antiox9050455"},{"key":"e_1_2_6_17_1","doi-asserted-by":"publisher","DOI":"10.1002\/elsc.201800066"},{"issue":"3","key":"e_1_2_6_18_1","first-page":"103","article-title":"New Validated Method for Analysis of Silymarin in Polyherbal Formulation (Aqueous Extract, Oral Liquid and Solid Dosage Form)","volume":"1","author":"Gul S.","year":"2015","journal-title":"Chemistry International"},{"key":"e_1_2_6_19_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.snb.2020.128544"},{"key":"e_1_2_6_20_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.biopha.2021.111763"},{"key":"e_1_2_6_21_1","doi-asserted-by":"publisher","DOI":"10.1021\/acsaelm.3c01460"},{"key":"e_1_2_6_22_1","doi-asserted-by":"publisher","DOI":"10.3390\/foods9020116"},{"key":"e_1_2_6_23_1","doi-asserted-by":"publisher","DOI":"10.3390\/molecules25122918"},{"key":"e_1_2_6_24_1","doi-asserted-by":"publisher","DOI":"10.3390\/molecules24112180"},{"key":"e_1_2_6_25_1","doi-asserted-by":"publisher","DOI":"10.1093\/chromsci\/bmaa035"},{"key":"e_1_2_6_26_1","first-page":"111","volume-title":"Studies in Natural Products Chemistry","author":"Lorenzo J. M.","year":"2020"},{"key":"e_1_2_6_27_1","doi-asserted-by":"publisher","DOI":"10.1080\/08327823.2017.1320265"},{"key":"e_1_2_6_28_1","doi-asserted-by":"publisher","DOI":"10.3390\/antiox8080304"},{"key":"e_1_2_6_29_1","doi-asserted-by":"publisher","DOI":"10.1002\/elan.201300102"},{"key":"e_1_2_6_30_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.talanta.2011.01.027"},{"key":"e_1_2_6_31_1","doi-asserted-by":"publisher","DOI":"10.1002\/elps.202100212"},{"key":"e_1_2_6_32_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.arabjc.2013.06.021"},{"key":"e_1_2_6_33_1","doi-asserted-by":"publisher","DOI":"10.1007\/s00216\u2010019\u201002274\u20103"},{"key":"e_1_2_6_34_1","doi-asserted-by":"publisher","DOI":"10.3390\/molecules29132949"},{"issue":"8","key":"e_1_2_6_35_1","first-page":"L 221\/8","article-title":"COMMISSION DECISION of 12 August 2002 Implementing Council Directive 96\/23\/EC Concerning the Performance of Analytical Methods and the Interpretation of Results","volume":"17","year":"2002","journal-title":"Official Journal of the European Communities"},{"key":"e_1_2_6_36_1","volume-title":"Eurachem Guide: The Fitness for Purpose of Analytical Methods \u2013 A Laboratory Guide to Method Validation and Related Topics","author":"Magnusson B.","year":"2024"}],"container-title":["Phytochemical Analysis"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/analyticalsciencejournals.onlinelibrary.wiley.com\/doi\/pdf\/10.1002\/pca.3478","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,21]],"date-time":"2025-10-21T11:31:19Z","timestamp":1761046279000},"score":1,"resource":{"primary":{"URL":"https:\/\/analyticalsciencejournals.onlinelibrary.wiley.com\/doi\/10.1002\/pca.3478"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2024,11,17]]},"references-count":35,"journal-issue":{"issue":"4","published-print":{"date-parts":[[2025,6]]}},"alternative-id":["10.1002\/pca.3478"],"URL":"https:\/\/doi.org\/10.1002\/pca.3478","archive":["Portico"],"relation":{},"ISSN":["0958-0344","1099-1565"],"issn-type":[{"value":"0958-0344","type":"print"},{"value":"1099-1565","type":"electronic"}],"subject":[],"published":{"date-parts":[[2024,11,17]]},"assertion":[{"value":"2024-07-17","order":0,"name":"received","label":"Received","group":{"name":"publication_history","label":"Publication History"}},{"value":"2024-10-22","order":2,"name":"accepted","label":"Accepted","group":{"name":"publication_history","label":"Publication History"}},{"value":"2024-11-17","order":3,"name":"published","label":"Published","group":{"name":"publication_history","label":"Publication History"}}]}}