中国中药杂志

2020, v.45(14) 3475-3480

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基于高效液相色谱-电雾式检测的三七及人参、西洋参中水溶性非皂苷类部位的指纹图谱表征分析和三七素的含量测定
Fingerprinting analysis of non-saponins from water-soluble part and determination of dencichine from Panax notoginseng, P. ginseng and P. quinquefolium based on liquid chromatography coupled with charged aerosol detection

张艳海;杨远贵;施磊;金燕;王峥涛;
ZHANG Yan-hai;YANG Yuan-gui;SHI Lei;JIN Yan;WANG Zheng-tao;the Ministry of Education Key Laboratory for Standardization, Institute of Chinese Material Medica, Shanghai University of Traditional Chinese Medicine;ThermoFisher Scientific Corporation;East China University of Science and Technology;

摘要(Abstract):

建立三七、人参和西洋参的水溶性非皂苷部位的指纹图谱和三七素的含量测定方法。样品采用水作为溶剂,超声提取30 min,水提取液经过Retain PEP柱净化,收集不保留和水洗脱部位,作为分析溶液。采用多孔石墨化碳Hypercarb色谱柱(3.0 mm×150 mm,3μm)作为分析柱,流动相为乙腈和0.1%九氟戊酸,梯度洗脱,流速0.8 mL·min~(-1);电雾式检测器雾化温度50℃,氮气压力60.1 psi(1 psi≈6.895 kPa)。结果显示,三七素及其他极性组分的保留和分离良好,三七素在0.019 2~0.48μg·mL~(-1),线性相关系数为0.998 2,定量限为7.4 ng·mL~(-1),平均回收率在95.52%~102.7%。3种药材在该部位的化学组成上整体相近,但三七素及其他部分组分的相对含量差异较大。该法可有效表征三七、人参和西洋参中水溶性非皂苷部位的化学组成,并同时完成三七素的定量,完善药材的质量评价标准。
This work describes the holistic fingerprinting method based on liquid chromatography coupled with charged aerosol detection(CAD) to profile non-saponin from water-soluble parts and determination of dencichine in Panax ginseng(PG), P. quinquefolium(PQ) and P. notoginseng(PNG). Sample extraction was carried out by water with ultra sonication for 30 min, which was eluted by Retain PEP for further analysis. The analysis was performed on a Hypercarb of porous graphitized carbon(3.0 mm×150 mm, 3 μm) column with acetonitrile and 0.1% perfluoropentanoic acid as mobile phase at a flow rate of 0.8 mL·min~(-1). Temperature of evaporator and nitrogen pressure for CAD were set at 50 ℃and 60.1 psi(1 psi≈6.895 kPa), respectively. As a result, dencichine and other polar components had a good performance on resolution and retention. The correlation coefficient(R~2) of dencichine was 0.998 2 in the concentration from 0.019 2 to 0.48 μg·mL~(-1). Limit of quantitation calculated by signal to noise of 10 was 7.4 ng·mL~(-1), and the recovery ranged from 95.52% to 102.7%. Chemical profile of the water-soluble part from PG, PQ and PNG was similar holistically, while the relative content for dencichine and other partial components varied significantly. The proposed method was used for characteristic of chemical profiling for non-saponin from water-soluble part, and determination of dencichine in PG, PQ and PNG.

关键词(KeyWords): 三七;电雾式检测;三七素;水溶性成分;指纹图谱
Panax notoginseng;charged aerosol detection;dencichine;water-soluble components;fingerprint

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基金项目(Foundation): 国家中医药标准化项目(ZYBZH-C-YN-58)

作者(Author): 张艳海;杨远贵;施磊;金燕;王峥涛;
ZHANG Yan-hai;YANG Yuan-gui;SHI Lei;JIN Yan;WANG Zheng-tao;the Ministry of Education Key Laboratory for Standardization, Institute of Chinese Material Medica, Shanghai University of Traditional Chinese Medicine;ThermoFisher Scientific Corporation;East China University of Science and Technology;

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