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

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• 作者：Bing-Chung Liau ; Shun-Sheng Hsiao ; Maw-Rong Lee ; Ting-Ting Jong ; Shu-Tuan Chiang
• 关键词：Bupleuri radixes ; Chaihu ; Saikosaponin-a ; Saikosaponin-c ; LC/ESI(+)/MS/MS
• 刊名：Journal of Pharmaceutical and Biomedical Analysis
• 出版年：2007
• 出版时间：19 February 2007
• 年：2007
• 卷：43
• 期：3
• 页码：1174-1178
• 全文大小：444 K

文摘

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 μM sodium acetate as an additive in the mobile phase. We observed good linearity over the range from 0.02 to 2 μg/ml for saikosaponin-a and from 0.02 to 1 μg/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 μg/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 μg/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.