HPLC-QqQ-MS测定珠子参中5种皂苷类成分的含量Research on concentration of 5 different ginsenosides in Panax japonica collected from different cultivated geographic regions
宁张弛;刘振丽;宋志前;王淳;曾鸿莲;赵思宇;舒一崧;董运茁;刘元艳;
NING Zhang-chi;LIU Zhen-li;SONG Zhi-qian;WANG Chun;ZENG Hong-lian;ZHAO Si-yu;SHU Yi-song;DONG Yun-zhuo;LIU Yuan-yan;School of Chinese Pharmacy,Beijing University of Chinese Medicine;Institute of Basic Theory,China Academy of Chinese Medical Sciences;
摘要(Abstract):
该文采用HPLC-Qq Q-MS技术对不同产地珠子参中的5种成分建立含量测定方法。色谱条件为Zorbax XDB-C18(4.6mm×100 mm,1.8μm),流动相乙腈(含0.1%甲酸)-0.1%甲酸水梯度洗脱,流速0.5 m L·min-1,柱温30℃。质谱条件为正离子检测模式,采用电喷雾电离源(ESI),扫描方式为多反应离子监测模式(MRM),定量分析离子分别为人参皂苷Re m/z 203.2,人参皂苷Rg1m/z 202.9,人参皂苷Rf m/z 365.0,人参皂苷Rd m/z 789.1,人参皂苷Ro m/z 360.9,干燥气流速10L·min-1,干燥气温度300℃,雾化气压力45 psi(1 psi=6.895 k Pa),毛细管电压4 000 V。结果显示5种人参皂苷的含量在一定范围内线性关系良好(r>0.9991)。人参皂苷Re、人参皂苷Rg1、人参皂苷Rf、人参皂苷Rd、人参皂苷Ro线性范围分别在3.33~66.60μg(r=0.999 1),2.83~56.54μg(r=0.999 2),0.32~6.51μg(r=0.999 2),12.55~251.00μg(r=0.999 3),0.85~16.90μg(r=0.999 5),范围与色谱峰面积呈良好的线性关系,加样回收率(n=6)均在100.8%~104.6%,RSD均<3.0%。该方法简单、准确,重复性好,可用于人参皂苷类成分的含量测定。
In this paper,an HPLC-Qq Q-MS method for determination of 5 different ginsenosides of Panax japonica collected from different cultivated geographic regions was established. The separation was performed on a Zorbax XDB-C18( 4. 6 mm × 100 mm,1. 8μm) column with the gradient elution of acetonitrile( contained 0. 1% formic acid)-0. 1% formic acid water. The flow rate was 0. 5m L·min-1. The colunm temperature was maintained at 30 ℃. The analytes were detected using electrospray ionization( ESI) in multiple reaction monitoring( MRM) modes. Reaction selected ions were 203. 2 for ginsenoside Re,202. 9 for ginsenoside Rg1,365. 0 for ginsenoside Rf,789. 1 for ginsenoside Rd,360. 9 for ginsenoside Ro. Ginsenosides Re,ginsenosides Rg1,ginsenosides Rf,ginsenosides Rd,ginsenosides Ro had good linearity in the ranges of 3. 33-66. 60 μg( r = 0. 999 1),2. 83-56. 54 μg( r = 0. 999 2),0. 32-6. 51 μg( r = 0. 999 2),12. 55-251. 00 μg( r = 0. 999 3),0. 85-16. 90 μg( r = 0. 999 5),respectively. The results of recovery were among 100. 8% to 104. 6%,and the values of RSD were blow 3. 0%. This method is simple,reliable and accurate,and can provide basis for P. japonica basic research.
关键词(KeyWords):
HPLC-Qq Q-MS;珠子参;含量测定;皂苷
HPLC-Qq Q-MS;Panax japonica;content determination;saponin
基金项目(Foundation): 国家自然科学基金项目(81573569);; 北京中医药大学校级课题项目(2015-JYB-JSMS021)
作者(Author):
宁张弛;刘振丽;宋志前;王淳;曾鸿莲;赵思宇;舒一崧;董运茁;刘元艳;
NING Zhang-chi;LIU Zhen-li;SONG Zhi-qian;WANG Chun;ZENG Hong-lian;ZHAO Si-yu;SHU Yi-song;DONG Yun-zhuo;LIU Yuan-yan;School of Chinese Pharmacy,Beijing University of Chinese Medicine;Institute of Basic Theory,China Academy of Chinese Medical Sciences;
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DOI:
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- 宁张弛
- 刘振丽
- 宋志前
- 王淳
- 曾鸿莲
- 赵思宇
- 舒一崧
- 董运茁
- 刘元艳
NING Zhang-chi- LIU Zhen-li
- SONG Zhi-qian
- WANG Chun
- ZENG Hong-lian
- ZHAO Si-yu
- SHU Yi-song
- DONG Yun-zhuo
- LIU Yuan-yan
- School of Chinese Pharmacy
- Beijing University of Chinese Medicine
- Institute of Basic Theory
- China Academy of Chinese Medical Sciences
- 宁张弛
- 刘振丽
- 宋志前
- 王淳
- 曾鸿莲
- 赵思宇
- 舒一崧
- 董运茁
- 刘元艳
NING Zhang-chi- LIU Zhen-li
- SONG Zhi-qian
- WANG Chun
- ZENG Hong-lian
- ZHAO Si-yu
- SHU Yi-song
- DONG Yun-zhuo
- LIU Yuan-yan
- School of Chinese Pharmacy
- Beijing University of Chinese Medicine
- Institute of Basic Theory
- China Academy of Chinese Medical Sciences