竹节参HPLC-ELSD指纹图谱和化学成分分析HPLC-ELSD fingerprint and chemical constituents of Rhizoma Panacis Japonici
胡远浪;袁丁;何毓敏;王洪武;孙志伟;张长城;
HU Yuanlang,YUAN Ding,HE Yumin,WANG Hongwu,SUN Zhiwei,ZHANG Changcheng* (Medical College of China Three Gorges University,Yichang 443002,China)
摘要(Abstract):
目的:建立竹节参药材HPLC-ELSD液相指纹图谱,分离纯化鉴定其主要特征峰的单体化合物,客观评价竹节参内在质量差异。方法:采用高效液相色谱-蒸发光散射检测器(HPLC-ELSD),梯度洗脱,测定了10批竹节参样品。色谱条件为YMC-pack ODS-AQ色谱柱(4.6 mm×250 mm,5μm),乙腈(A)-0.5%乙酸水溶液(B)为流动相,梯度洗脱(0~5 min,20%~40%A;5~20 min,40%~40%A),流速为1.0 mL.min-1,柱温30℃。ELSD检测器:漂移管温度为40℃,氮气释放压力为33 Psi。通过采用反复硅胶柱色谱和半制备HPLC的方法分离纯化竹节参的化学成分,并根据理化性质和波谱数据进行结构鉴定。结果:建立了10批竹节参样品HPLC-ELSD指纹图谱,分离纯化鉴定了5个主要化学成分,分别为人参皂苷Re,竹节参皂苷Ⅳ,Ⅳa,Ⅴ,Pjs-2。结论:综合竹节参指纹图谱和化学成分分析,能较全面的表征不同产地竹节参内在成分的差异,为竹节参内在质量评价提供依据。
The aim was to establish the chromatographic fingerprint of Rhizoma Panacis Japonici for its quality evaluation.Analysis was performed on a YMC-Pack ODS-AQ column(4.6 mm×250 mm,5 μm)eluted with the mobile phases of acetonitrile(A)and 5% acetic acid solution(B)at in gradient a flow rate of 1.0 mL·min-1.The elution program was as follow: 0-5 min,changed from 20%A to 40%A,5-20 min,kept 40%A.The temperature of column was 30 ℃.The temperate of drift tube was 40 ℃,and the nitrogen pressure was 33 Psi.Ten batches of Rhizoma Panacis japonici were determined.The HPLC-ELSD chromatographic fingerprint of chemical constituents was established from the 10 batches of Rhizoma Panacis japonici and it had 9 characteristic common peaks.The 10 batches of samples were classified into 2 cluster by cluster analysis.Furthermore,five known chemical constuituents were identified after isolation and purification by means of silica gel column chromatography,and semi-preparative high performance liquid chromatography.They were panaxsaponins Re,chikusetsusaponins Ⅳ,Ⅳa,Ⅴand pjs-2,respectively.This study provided experimental data for comprehensive evaluation of the quality of Rhizoma Panacis japonici.
关键词(KeyWords):
竹节参;HPLC-ELSD;指纹图谱;化学成分
Rhizoma Panacis Japonici;HPLC-ELSD;fingerprint;chemical composition
基金项目(Foundation): 国家自然科学基金项目(30873383)
作者(Author):
胡远浪;袁丁;何毓敏;王洪武;孙志伟;张长城;
HU Yuanlang,YUAN Ding,HE Yumin,WANG Hongwu,SUN Zhiwei,ZHANG Changcheng* (Medical College of China Three Gorges University,Yichang 443002,China)
Email:
DOI:
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- 胡远浪
- 袁丁
- 何毓敏
- 王洪武
- 孙志伟
- 张长城
HU Yuanlang- YUAN Ding
- HE Yumin
- WANG Hongwu
- SUN Zhiwei
- ZHANG Changcheng* (Medical College of China Three Gorges University
- Yichang 443002
- China)
- 胡远浪
- 袁丁
- 何毓敏
- 王洪武
- 孙志伟
- 张长城
HU Yuanlang- YUAN Ding
- HE Yumin
- WANG Hongwu
- SUN Zhiwei
- ZHANG Changcheng* (Medical College of China Three Gorges University
- Yichang 443002
- China)