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

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.

Chemical Fingerprinting of Valeriana Species: Simultaneous Determination of Valerenic Acids, Flavonoids, and Phenylpropanoids Using Liquid Chromatography with Ultraviolet Detection

The roots and rhizomes of various valeriana species are currently used as a sleeping aid or mild sedative. A liquid chromatography method has been developed that permits the analysis of chlorogenic acid, lignans, flavonoids, valerenic acids, and valpotrates in various valerian samples. The best results were obtained with a Phenomenex Luna C18(2) column using gradient elution with a mobile phase consisting of water and 0.05% phosphoric acid and 2100% acetonitrilemethanol (1 + 1) with 0.05% phosphoric acid. The flow rate was 0.8 mL/min and ultraviolet detection was at 207, 225, 254, 280, and 325 nm. Different valerian species and commercial products showed remarkable quantitative variations. Chlorogenic acid (0.21.2%), 3 lignans, linarin (0.0020.24%), and valepotriates were detected in all the valeriana species analyzed. Highest amounts of valerenic acids were detected in V. officinalis L., trace amounts in V. sitchensis, and none in the other species analyzed.