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Simultaneous Determination of Asperosaponins and Iridoid Glycosides from Dipsaci Radix by Using LC-ESI-MS Spectrometry  

Cho, Hwang-Eui (College of Pharmacy, Chungbuk National University)
Son, In-Seop (College of Pharmacy, Chungbuk National University)
Kim, Sun-Cheun (National Forensic Service)
Son, Kun-Ho (College of Life Science, Andong National University)
Woo, Mi-Hee (College of Pharmacy, Catholic University of Daegu)
Moon, Dong-Cheul (College of Pharmacy, Chungbuk National University)
Publication Information
Korean Journal of Pharmacognosy / v.43, no.2, 2012 , pp. 137-146 More about this Journal
Abstract
Dipsaci Radix (Dipsacaceae) has been used as a tonic, an analgesic, anti-inflammatory and anti-complement agents in traditional herbal medicine for the therapy of low back pain, knee pain, rheumatic arthritis, traumatic hematoma, and bone fractures. A high-performance liquid chromatography-electrospray ionization-mass spectrometric method (HPLC-ESI-MS) was developed for the simultaneous quantitation method of the five compounds from the herbal drug: asperosaponin VI and asperosaponin XII (terpene glycosides), sweroside, loganin and dipsacus A(iridoid glycosides). HPLC separation of the analytes was achieved on a C18 column ($150{\times}2.0$ mm i.d., 5 ${\mu}m$) using the aqueous methanol containing 5 mM ammonium acetate with gradient flow of the mobile phase. Detection of the analytes was performed by positive ion electrospray ionization, and selected ion monitoring was used for data acquisition using m/z corresponding molecular adduct ion, $[M+NH_4]^+$ and $[M+H]^+$. Calibration graphs showed good linearity ($r^2$=0.9997) over the wide range of the analytes; intra- and inter-day precisions (RSD, %) were within 9.1% and the accuracy between 94.0-111.0%. Recoveries of the analytes through the assay procedure were in the range of 93.7-110.8%. Analytical results of the herbal drugs of Dipsaci Radix (17 samples) show wide distribution of the five marker compounds and clear difference of the species from Phlomidis Radix (4 samples). The developed method would provide a practical guide for the quality control of the herbal drug.
Keywords
Dipsacci radix; HPLC-ESI-MS; Selected ion monitoring; Simultaneous determination; Asperosaponins; Iridoid glycosides; Quality control;
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