摘要
目的 建立柴胡中酰化柴胡皂苷含量的测定方法。方法 采用单因素分析和正交实验设计法,选择氨水浓度、超声时间、超声功率为因素各取3 水平,按L9(34) 正交表进行实验,优化柴胡中酰化柴胡皂苷的水解方法。采用HPLC测定柴胡皂苷的含量。色谱条件为WondaSil C18 色谱柱(4.6 mm×250 mm,5 μm);流动相:甲醇-水(53∶47);流速:1.0 mL·min-1;检测波长:210 nm。结果 优化的柴胡中酰化柴胡皂苷水解方法为浓氨水的浓度为23%,超声25 min,超声的功率为350 W。基于所测定的样品中酰化柴胡皂苷的含量结果,柴胡药材中酰化柴胡皂苷的含量相低于柴胡皂苷,且在柴胡皂苷含量的70%以下。结论 该方法简便可靠,可用于柴胡中酰化柴胡皂苷的含量测定。为准确评价柴胡药材质量提供参考。
Abstract
OBJECTIVE To establish the determination method of acyl-saikosaponin in Radix Bupleuri. METHODS Single factor analysis and orthogonal experimental design were used to optimize the acyl-saikosaponin hydrolysis parameters such as concentration of aqueous ammonia, time of ultrasound-assisted hydrolysis and ultrasound power by L9(34) orthogonal test. An HPLC method was employed to determine the saikosaponins contents, which was carried out on a WondaSil C18 column (4.6 mm×250 mm, 5 μm) with the mobile phase of methanol-water (53∶47) at the flow rate of 1.0 mL·min-1 and the wavelength of 210 nm. RESULTS The optimized conditions of acyl-saikosaponin hydrolysis were as follows: the concentration of aqueous ammonia was 23%, the time of ultrasound-assisted hydrolysis was 25 min, and the ultrasound power was 350 W. The content of acyl-saikosaponin in the Radix Bupleuri samples purchased in 12 different drug stores was lower than that of saikosaponin in Radix Bupleuri. CONCLUSION This method is simple and reliable, which can be used for the determination of acyl-saikosaponin in Radix Bupleuri and provides clues for the quality assessment of Radix Bupleuri.
关键词
柴胡 /
酰化柴胡皂苷 /
含量测定
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Key words
Radix Bupleuri /
acyl-saikosaponin /
content determination
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李军,姜华,张延萍,周冬菊,陈丽娜,张倩,薛娟娟.
柴胡中酰化柴胡皂苷的含量测定[J]. 中国药学杂志, 2015, 50(8): 722-726 https://doi.org/10.11669/cpj.2015.08.015
LI Jun, JIANG Hua, ZHANG Yan-ping, ZHOU Dong-ju, CHEN Li-na, ZHANG Qian, XUE Juan-juan.
Determination of Acyl-Saikosaponin in Radix Bupleuri[J]. Chinese Pharmaceutical Journal, 2015, 50(8): 722-726 https://doi.org/10.11669/cpj.2015.08.015
中图分类号：
R284
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参考文献
[1] Ch.P (2010) VolⅠ(2010年版. 中国药典一部). 2010:992. [2] HUANG H Q,ZHANG X,LIN M,et al. Characterization and identification of saikosaponins in crude extracts from three Bupleurum species using LC-ESI-MS . J Sep Sci, 2008,31(18):3190-3201. [3] LIANG Z T,ZHANG J,YANG G Y,et al. Chemical profiling and histochemical analysis of Bupleurum marginatum roots from different growing areas of Hubei province . Acta Pharm Sin B(药学学报B辑), 2013,3(3):193-204. [4] LI J,JIANG H,ZHANG Y P,et al. Determination of five saikosaponins in the leftovers from the preparation process of Radix Bupleuri oral liquid. Chin Pharm J (中国药学杂志),2012,47(16):1337-1340. [5] LI J,JIANG H,ZHANG Y P,et al. Determination of saikodaponin b1 b2 in Chai-Huang tablet by HPLC . Chin Pharm J (中国药学杂志),2011,46(1):61-63.
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脚注
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基金
国家自然科学基金资助项目(81001615);河南科技大学大学生研究训练计划(2014093)
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