title: Development and validation of a high-throughput based on liquid chromatography with ultraviolet absorption and mass spectrometry detection method for quantitation of cichoric acid in Echinacea purpurea aerial-based dietary supplements.
abstract: A new, rapid, and reproducible reversed-phased liquid chromatography (LC) method with ultraviolet (UV) absorption and/or mass spectrometry (MS) detection has been developed and validated for quantitation of cichoric acid, a major constituent of Echinacea spp. The method involves the use of a short Phenomenex Hydro-RP C18 column (4 microm, 50 mm x 3.0 mm id) and a simple isocratic mobile phase profile. Both UV (diode array detector) and selective-ion monitoring (SIM) at m/z 472.8 were used for quantitation of cichoric acid. The limit of detection was 0.75 ng for UV and 0.15 ng for MS-SIM, and the limit of quantitation was is 2.5 ng for UV and 0.5 ng for MS-SIM. Water-methanol (1 + 1) soluble extracts of 6 commercially available Echinacea purpurea aerial parts-based dietary supplements (EPADS). EPADS were first profiled using a traditional HPLC-UV method. Their UV chromatograms were compared, and cichoric acid was identified to be a key biomarker for EPADS. Then the samples were analyzed by the fast LC-UV/MS method. The turnaround time for a single analysis was 3 min, compared to 15 to 60 min needed for traditional reported LC methods. The high-throughput method was able to separate the cichoric acid peak from peaks of other components in extracts of complex matrixes of EPADS.
authors.affiliation: U.S. Department of Agriculture, Agricultural Research Service, Beltsville Human Nutrition Research Center, Food Composition Laboratory, Bldg 161, BARC-East, Beltsville, MD 20705, USA. chenp@ba.ars.usda.gov
authors.forename: Pei
authors.initials: P
authors.lastname: Chen
mesh_terms: D002109:Caffeic Acids / Q000032:analysis* / Q000302:isolation & purification; D002623:Chemistry Techniques, Analytical / Q000379:methods; D002853:Chromatography, Liquid / Q000379:methods*; D019587:Dietary Supplements / Q000032:analysis*; D020900:Echinacea / Q000378:metabolism*; D013058:Mass Spectrometry / Q000379:methods*; D000432:Methanol / Q000032:analysis; D015203:Reproducibility of Results; D013056:Spectrophotometry, Ultraviolet / Q000379:methods*; D013386:Succinates / Q000032:analysis* / Q000302:isolation & purification; D013997:Time Factors; D014466:Ultraviolet Rays; D014867:Water / Q000032:analysis
chemical_list: D002109:Caffeic Acids; D013386:Succinates; D014867:Water; C100435:chicoric acid; D000432:Methanol