Quality control of Chinese medicinal preparations LC/ESI(+)/MS/MS analyses of saikosaponins-a and -c as markers of bupleuri radix samples

• Published in: Journal of pharmaceutical and biomedical analysis 2007-02, Vol.43 (3), p.1174-1178
• Main Authors: LIAU, Bing-Chung, HSIAO, Shun-Sheng, LEE, Maw-Rong, JONG, Ting-Ting, CHIANG, Shu-Tuan
• Format: Article
• Language: English
• Subjects: Analysis; Analytical, structural and metabolic biochemistry; Biological and medical sciences; Calibration; Chromatography, High Pressure Liquid; Drugs, Chinese Herbal - analysis; Drugs, Chinese Herbal - standards; Fundamental and applied biological sciences. Psychology; General pharmacology; Medical sciences; Oleanolic Acid - analogs & derivatives; Oleanolic Acid - analysis; Pharmacology. Drug treatments; Quality Control; Reference Standards; Saponins - analysis; Spectrometry, Mass, Electrospray Ionization
• ISSN: 0731-7085; 1873-264X
• DOI: 10.1016/j.jpba.2006.10.002

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.