title: Simultaneous determination of chromones and coumarins in Radix Saposhnikoviae by high performance liquid chromatography with diode array and tandem mass detectors.
abstract: Methods using high performance liquid chromatography with diode array detection (HPLC-DAD) and tandem mass spectrometry (HPLC-MS/MS) were developed and validated for the simultaneous determination of 5 chromones and 6 coumarins: prim-O-glucosylcimifugin (1), cimifugin (2), nodakenin (3), 4'-O-β-d-glucosyl-5-O-methylvisamminol (4), sec-O-glucosylhamaudol (5), psoralen (6), bergapten (7), imperatorin (8), phellopterin (9), 3'-O-angeloylhamaudol (10) and anomalin (11), in Radix Saposhnikoviae. The separation conditions for HPLC-DAD were optimized using an Ascentis Express C18 (4.6 mm×100 mm, 2.7 μm particle size) fused-core column. The mobile phase was composed of 10% aqueous acetonitrile (A) and 90% acetonitrile (B) and the elution was performed under a gradient mode at a flow rate of 1.0 mL/min. The detection wavelength was set at 300 nm. The HPLC-DAD method yielded a base line separation of the 11 components in 50% methanol extract of Radix Saposhnikoviae with no interfering peaks detected. The HPLC-DAD method was validated in terms of linearity, accuracy and precision (intra- and inter-day), limit of quantification (LOQ), recovery, and robustness. Specific determination of the 11 components was also accomplished by a triple quadrupole tandem mass spectrometer equipped with an electrospray ionization (ESI) source. This HPLC-MS/MS method was also validated by determining the linearity, limit of quantification, accuracy, and precision. Quantification of the 11 components in 51 commercial Radix Saposhnikoviae samples was successfully performed using the developed HPLC-DAD method. The identity, batch-to-batch consistency, and authenticity of Radix Saposhnikoviae were successfully monitored by the proposed HPLC-DAD and HPLC-MS/MS methods.
authors.affiliation: College of Pharmacy, Chung-Ang University, 221 Heukseok-Dong, Dongjak-Gu, Seoul 156-756, South Korea.
authors.forename: Min Kyung
authors.initials: MK
authors.lastname: Kim
authors.forename: Dong-Hyug
authors.initials: DH
authors.lastname: Yang
authors.forename: Mihye
authors.initials: M
authors.lastname: Jung
authors.forename: Eun Ha
authors.initials: EH
authors.lastname: Jung
authors.forename: Han Young
authors.initials: HY
authors.lastname: Eom
authors.forename: Joon Hyuk
authors.initials: JH
authors.lastname: Suh
authors.forename: Jung Won
authors.initials: JW
authors.lastname: Min
authors.forename: Unyong
authors.initials: U
authors.lastname: Kim
authors.forename: Hyeyoung
authors.initials: H
authors.lastname: Min
authors.forename: Jinwoong
authors.initials: J
authors.lastname: Kim
authors.forename: Sang Beom
authors.initials: SB
authors.lastname: Han
mesh_terms: D019661:Apiaceae / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D002867:Chromones / Q000032:analysis*; D003374:Coumarins / Q000032:analysis*; D016014:Linear Models; D010936:Plant Extracts / Q000737:chemistry*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry
chemical_list: D002867:Chromones; D003374:Coumarins; D010936:Plant Extracts