高效液相色谱法同时测定细辛中7种主要成分的含量

doi:10.5246/jcps.2015.08.067

中国药学(英文版) ›› 2015, Vol. 24 ›› Issue (8): 530-537.DOI: 10.5246/jcps.2015.08.067

高效液相色谱法同时测定细辛中7种主要成分的含量

曹晨, 王静哲, 王璐, 尚明英^*, 刘广学, 徐风, 王璇, 蔡少青^*

北京大学医学部药学院, 北京 100191

收稿日期:2015-05-03 修回日期:2015-05-15 出版日期:2015-08-22 发布日期:2015-05-28
通讯作者: Tel./Fax: 86-10-82802534, 86-10-82801693, E-mail: myshang@bjmu.edu.cn, sqcai@bjmu.edu.cn
基金资助:
National Basic Research Program of China (Grant No. 2006CB504707), National Science and Technology Major Projects for “Major New Drugs Innovation and Development” (Grant No. 2013ZX09508104) and National Natural Science Foundation of China (Grant No. 81274073).

Simultaneous determination of seven principal constituents in Asari Radix et Rhizoma by HPLC

Chen Cao, Jingzhe Wang, Lu Wang, Mingying Shang^*, Guangxue Liu, Feng Xu, Xuan Wang, Shaoqing Cai^*

School of Pharmaceutical Sciences, Peking University Health Science Center, Beijing 100191, China

Received:2015-05-03 Revised:2015-05-15 Online:2015-08-22 Published:2015-05-28
Contact: Tel./Fax: 86-10-82802534, 86-10-82801693, E-mail: myshang@bjmu.edu.cn, sqcai@bjmu.edu.cn
Supported by:
National Basic Research Program of China (Grant No. 2006CB504707), National Science and Technology Major Projects for “Major New Drugs Innovation and Development” (Grant No. 2013ZX09508104) and National Natural Science Foundation of China (Grant No. 81274073).

摘要/Abstract

摘要：

建立了同时测定细辛中花椒酚、卡枯醇、甲基丁香酚、l–芝麻脂素、黄樟醚、细辛素和l–细辛脂素7种主要成分含量的HPLC方法, 并测定了55份不同来源的细辛药材(35份北细辛、3份汉城细辛和17份华细辛)中这7种成分的含量, 比较了不同品种细辛中7种成分含量差异。采用Agilent Zorbax SB–C₁₈色谱柱(4.6 mm×25 cm, 5 μm), 水(A)–乙腈(B)为流动相进行梯度洗脱55 min, DAD检测器检测, 柱温20 °C, 检测波长287 nm。被测成分在测试范围内线性关系良好, r²>0.999; 加样回收率96.0%–103.1%, RSD小于2.54%。该方法准确、灵敏、重复性好。测定结果表明不同来源的细辛样品中7种成分的含量差异显著, 其中挥发性成分甲基丁香酚在辽细辛(汉城细辛与北细辛的根及根茎)中的含量为(6.17±5.13) mg/g, 显著高于其在华细辛(华细辛的根及根茎)中的含量(0.58±0.39) mg/g, 有毒成分黄樟醚在辽细辛中的含量为(2.66±2.16) mg/g, 低于其在华细辛的含量(6.44±3.88) mg/g。本文首次报道了细辛中花椒酚和细辛素的含量。

关键词: 细辛, HPLC-DAD, 多成分含量测定, 花椒酚, 细辛素

Abstract:

A method using high-performance liquid chromatography for the simultaneous determination of seven principal constituentsincluding xanthoxylol, kakuol, methyleugenol, l-sesamin, safrole, sarisan, and l-asarinin in Asari Radix et Rhizoma (Xixin in Chinese) was developed. Fifty five samples of Asari Radix et Rhizoma from different sources (35 samples from Asarum heterotropoides var. mandshuricum, 3 samples from Asarum sieboldii var. seoulense, and 17 samples from Asarum sieboldii) were analyzed with this method. Chromatographic separation was achieved on an Agilent Zorbax SB-C₁₈ column (4.6 mm×25 cm, 5 μm) using a gradient elution with mobile phase of aqueous (A) and acetonitrile (B). The assay was carried out at 20 °C and with detection at 287 nm. All calibration curves showed good linearity (r²>0.999) within the tested ranges. The average recoveries were in the range of 96.0%-103.1% with relative standard deviation (RSD) less than 2.54%. The developed method was accurate with high sensitivity and good reproducibility. The content of volatile methyleugenol in LiaoXixin(the root and rhizome of A. heterotropoides var. mandshuricum and A. sieboldii var. seoulense) was (6.17±5.13) mg/g, which was higher than (0.58±0.40) mg/g in HuaXixin (the root and rhizome of A. sieboldii). The toxic safrole in LiaoXixin was (2.66±2.16) mg/g, which was lower than (6.44±3.89) mg/g in HuaXixin. This is the first report on the simultaneous and quantitative determination of anthoxylol and sarisan in Asari Radix et Rhizoma.

Key words: Asari Radix et Rhizoma, HPLC-DAD, determination, Anthoxylol, Sarisan

中图分类号:

R284

Supporting:

曹晨, 王静哲, 王璐, 尚明英, 刘广学, 徐风, 王璇, 蔡少青. 高效液相色谱法同时测定细辛中7种主要成分的含量[J]. 中国药学(英文版), 2015, 24(8): 530-537.

Chen Cao, Jingzhe Wang, Lu Wang, Mingying Shang, Guangxue Liu, Feng Xu, Xuan Wang, Shaoqing Cai . Simultaneous determination of seven principal constituents in Asari Radix et Rhizoma by HPLC[J]. Journal of Chinese Pharmaceutical Sciences, 2015, 24(8): 530-537.

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高效液相色谱法同时测定细辛中7种主要成分的含量

Simultaneous determination of seven principal constituents in Asari Radix et Rhizoma by HPLC

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