title: Quality control of Chinese medicinal preparations LC/ESI(+)/MS/MS analyses of saikosaponins-a and -c as markers of Bupleuri radix samples.
abstract: We have used LC/ion trap tandem MS analysis to determine saikosaponin-a and -c as target markers in crude 70% methanol extracts from three different species of Bupleuri radix and the 10 most-popular Chinese medicinal preparations containing "Chaihu" (B. radix) without any clean-up. The optimal ionization characteristics were obtained when using positive-ion electrospray ionization (ESI) with 50 microM sodium acetate as an additive in the mobile phase. We observed good linearity over the range from 0.02 to 2 microg/ml for saikosaponin-a and from 0.02 to 1 microg/ml for saikosaponin-c. The intra-day precisions varied between 3.3 and 8.8% for saikosaponin-a and 0.3 and 11.1% for saikosaponin-c. The limits of detection were 0.01 microg/ml for both markers. The recoveries of saikosaponin-a and -c from the extract of a medicinal preparation sample (Chai-Hu-Ching-Gan-Tang, No. 13 in the table of section Analysis on actual samples) were 97 and 100%, respectively, at a 1 microg/ml spiking concentration of each marker. The highest concentrations of saikosaponin-a and -c among the three B. radixes were found in B. kaoi Liu Chao & Chuang (10.1 mg/g) and in B. falcatum (3.4 mg/g), respectively. The amounts of these saikosaponins in the 10 Chinese medicinal preparations ranged between 0.11 and 1.22 mg/g for saikosaponin-a and between 0.01 and 0.33 mg/g for saikosaponin-c.
authors.affiliation: Department of Chemistry, National Chung-Hsing University, Taichung, Taiwan.
authors.forename: Bing-Chung
authors.initials: BC
authors.lastname: Liau
authors.forename: Shun-Sheng
authors.initials: SS
authors.lastname: Hsiao
authors.forename: Maw-Rong
authors.initials: MR
authors.lastname: Lee
authors.forename: Ting-Ting
authors.initials: TT
authors.lastname: Jong
authors.forename: Shu-Tuan
authors.initials: ST
authors.lastname: Chiang
mesh_terms: D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D004365:Drugs, Chinese Herbal / Q000032:analysis / Q000592:standards*; D009828:Oleanolic Acid / Q000031:analogs & derivatives* / Q000032:analysis; D011786:Quality Control; D012015:Reference Standards; D012503:Saponins / Q000032:analysis*; D021241:Spectrometry, Mass, Electrospray Ionization
chemical_list: D004365:Drugs, Chinese Herbal; D012503:Saponins; D009828:Oleanolic Acid; C025759:saikosaponin D