摘要
为了建立测定中药黄姜中薯蓣皂素含量的反相高效液相色谱法，从而为黄姜原料的质量控制提供参考，采用了双相联合酸水解法从黄姜原料中萃取薯蓣皂素，然后使用Waters XBridge ShieldRP18色谱柱（4．6mm×150toni，5μm），以乙腈-水（75：25，v／v）为流动相等度洗脱，流速为1．0mL／min，检测波长为203nm，柱温为40℃。结果表明：黄姜样品溶液中的薯蓣皂素可以与各干扰组分达到基线分离；薯蓣皂素的线性范围为2—1024μg／mL，r2=0．9999；精密度为1．02％；重复性实验RSD=1．78％；平均加样回收率为96．2％（RSD=1．17％）、100．4％（RSD=2．47％）和101．6％（RSD=1．09％）；该法制备的样品溶液在24h内测定，RSD〈2％；试验中测得黄姜中薯蓣皂素的平均含量为3．83％（RSD=2．21％）。本文采用的供试品溶液制备方法简便，薯蓣皂素得率比传统方法高；此外，建立的色谱分析方法稳定、可靠，适合于黄姜中薯蓣皂素的含量测定。
The objective of this study was to establish an RP-HPLC method for the determination of diosgenin in Di- oseorea zingiberensis C. H. Wright, and hence to provide a reference for the quality control of the herb. Dioagenin was ex- tracted by two-phase combined acid hydrolysis from raw material, followed by the analysis on a Waters XBridge Shield RP18 column （4.6 mm × 150 ram,5 μm） at 40℃ with aeetonitrile and distilled water （75：25 ,v/v） as mobile pha- ses. The UV deteetion wavelength was set at 203 nm,and flow rate was 1.0 mlVmin throughout the analysis. Under this condition, diosgenin can be satisfactorily separated from the interferential components in the sample. The linearity of the ealihration curve was good （ r2 =0. 9999） within the range of 2 × 1024 μg/mL for the analyte. The precision was tested to be 1.02%. The repeatability was 1.78% with the average recovery reached 96.2% （ RSD = 1.17% ）, 100.4% （ RSD = 2.47% ） and 101.6% （ RSD = 1.09% ）. In addition, the sample solution prepared was stable within 24 h （RSD 〈2% ）. The average content of diosgenin in the tubers of D. zingiberensis was 3.83% （ RSD = 2.21% ）. The method for sample solution preparation was convenient and the extraction yield of diosgenin was higher than three con- ventional methods. Moreover, the HPLC method developed in the study was stable and reliable, and henee can be used to determine diosgenin in the tubers of D. zingiberensis.
出处
《天然产物研究与开发》
CAS
CSCD
北大核心
2013年第12期1699-1703,共5页
Natural Product Research and Development
基金
常州市科技支撑计划(CE20125042)
2013年江苏省大学生创新创业训练计划项目(201310299059Y)
江苏大学高级人才科研启动基金(11JDG073)
国家中医药管理局中药口服制剂释药系统重点研究室开放基金项目(2011NDDCM01002)
关键词
黄姜
薯蓣皂素
双相联合酸水解法
反相高效液相色谱法
Dioscorea zingiberensis C. H. Wright
diosgenin
.two-phase combined acid hydrolysis
RP-HPLC
