Determination of the Major Bioactive Component of Silybum marianum in Nutricosmetics by a HPLC Method With Amperometric Detection and UAE Pretreatment.
Lucía Abad-Gil, M Jesús Gismera, M Teresa Sevilla, Jesús R Procopio
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引用次数: 0
Abstract
Introduction: Nutricosmetics derived from Silybum marianum, known for their anti-inflammatory and hepatoprotective properties, necessitate accurate quantification of silybin, a key bioactive component.
Objectives: This study aims to develop a novel high-performance liquid chromatography (HPLC) method with amperometric detection (HPLC-ECD) for the precise determination of silybin. An ultrasound-assisted extraction (UAE) procedure is also established for solid sample preparation prior to chromatographic analysis.
Materials and methods: Chromatographic separation of silybin was performed on a C18 column and using methanol-0.035 M potassium phosphate (pH 4.0) at 1.0 mL min-1 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 V versus Ag/AgCl. The UAE procedure for silybin extraction from solid samples was performed by 15 min sonication in an ultrasonic bath (80 kHz and 100% power) at room temperature.
Results: Under the optimal chromatographic conditions, silybin diastereoisomers (silybin A and silybin B) can be separated from other S. marianum flavonolignans in less than 20 min, with a detection limit (LOD) of 0.060 mg L-1 and a reproducibility (RSD) of 5%. This method was successfully applied to analyze silymarin-containing products with recoveries close to 100%.
Conclusions: 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-DAD methods. This HPLC-ECD method allows silybin diastereoisomers identification without interferences of other flavonolignans present in silymarin extracts.
期刊介绍：
Phytochemical Analysis is devoted to the publication of original articles concerning the development, improvement, validation and/or extension of application of analytical methodology in the plant sciences. The spectrum of coverage is broad, encompassing methods and techniques relevant to the detection (including bio-screening), extraction, separation, purification, identification and quantification of compounds in plant biochemistry, plant cellular and molecular biology, plant biotechnology, the food sciences, agriculture and horticulture. The Journal publishes papers describing significant novelty in the analysis of whole plants (including algae), plant cells, tissues and organs, plant-derived extracts and plant products (including those which have been partially or completely refined for use in the food, agrochemical, pharmaceutical and related industries). All forms of physical, chemical, biochemical, spectroscopic, radiometric, electrometric, chromatographic, metabolomic and chemometric investigations of plant products (monomeric species as well as polymeric molecules such as nucleic acids, proteins, lipids and carbohydrates) are included within the remit of the Journal. Papers dealing with novel methods relating to areas such as data handling/ data mining in plant sciences will also be welcomed.
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