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Micellar LC Separation of Sesquiterpenic Acids and Their Determination in Valeriana officinalis L. Root and Extracts

DOI: 10.1155/2012/564243

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Abstract:

A simple micellar liquid chromatography (MLC) method was developed and validated according to ICH Guidelines for the determination of sesquiterpenic acids (valerenic, hydroxyvalerenic, and acetoxyvalerenic acids) in root and rhizome extract from Valeriana officinalis L. and valerian dry hydroalcoholic extract. Samples were analyzed on Nucleosil C18 column ( , 5?μm) using an isocratic mobile phase which consisted of Brij 35 (5% (w/v) aqueous solution; pH? by phosphoric acid) and 1-butanol (6% (v/v)); UV detection was at 220?nm. Micellar mobile phase using allows to fully separate valerenic acids within 25 minutes. Linearity for hydroxyvalerenic, acetoxyvalerenic, and valerenic acids was 1.9–27.9, 4.2–63.0, and 6.1–91·3?μg.mL?1, and limit of detection was 0.14, 0.037, and 0.09?μg·mL?1, respectively. Intraday and interday precisions were not less than 2% for all investigated compounds. The proposed method was found to be reproducible and convenient for quantitative analysis of sesquiterpenic acids in valerian root and related preparations. 1. Introduction Valeriana officinalis L. is the most common species of the genus Valeriana that is used for its medicinal properties [1]. The root and rhizome of the valerian plant is used medicinally for its sedative properties with indications including nervous tension, insomnia, anxiety, and stress. Valerian is also considered to have antispasmodic, anticonvulsant, and antidepressant effects. The roots and rhizomes of Valeriana officinalis contain two main groups of constituents: sesquiterpenes of the volatile oil (valerenic acid and its derivatives, valeranone, valeranal, and kessyl esters) and valepotriates (valtrate, didrovaltrate, acevaltrate, and isovaleroxyhydroxyvaltrate), in addition to other constituents such as flavonoids, triterpenes, lignans, and alkaloids [2, 3]. Valerian is available in a variety of formulations, including tablets, capsules, liquid, teas, and tinctures. Products may contain whole herb and/or a proprietary blend or may also be combined with other herbal supplements (e.g., lemon balm, hops, kava, St. John’s worth, etc.). Valerian root and some commercial products (drugs) are standardized according to the content of valerenic acid, but concentrations vary among products. Valerenic acids are sesquiterpenes based on the dual ring valerane structure with the main representatives being valerenic acid ((2E)-3-[(4S,7R,7aR)-3,7-dimethyl-2, 4,5,6,7,7a-hexahydro-1H-inden-4-yl]-2-methylacrylic acid; C15H22O2), acetoxyvalerenic acid, and hydroxyvalerenic acid. Chemical structures of these acids are

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