Establishment of Specific Chromatogram and Thin-layer Identification Method for Kaixinsan
10.13422/j.cnki.syfjx.20230146
- VernacularTitle:经典名方开心散特征图谱及TLC鉴别方法的建立
- Author:
Wenya GAO
1
;
Min FENG
2
;
Chang GAO
1
;
Haiyu ZHAO
1
;
Yanyan ZHOU
1
;
Hongjie WANG
1
;
Ruipeng YU
3
;
Yipeng ZHAO
3
;
Lili ZHANG
2
;
Yanqing GAO
2
;
Yanhong XIAO
2
;
Cuina CHENG
2
;
Xiaolu WEI
1
;
Nan SI
1
;
Baolin BIAN
1
Author Information
1. Institute of Chinese Materia Medica，China Academy of Chinese Medical Sciences，Beijing 100700，China
2. Sunflower Pharmaceutical Group Co. Ltd.，Tangshan 064400，China
3. Beijing Institute for Drug Control，Beijing 102206，China
- Publication Type:Journal Article
- Keywords:
famous classical formulas;
Kaixinsan;
high performance liquid chromatography（HPLC） specific chromatogram;
quality control;
thin layer chromatography（TLC）;
Ginseng Radix et Rhizoma;
Poria
- From:
Chinese Journal of Experimental Traditional Medical Formulae
2023;29(13):37-44
- CountryChina
- Language:Chinese
-
Abstract:
ObjectiveTo establish the specific chromatogram and thin layer chromatography（TLC） identification method of Kaixinsan（KXS） samples， in order to clarify the key quality attributes and provide reference for the quality evaluation of KXS. MethodHigh performance liquid chromatography（HPLC） specific chromatogram of KXS was developed with YMC Hydrosphere C18 column（4.6 mm×250 mm， 5 μm）， the mobile phase was acetonitrile（A）-0.2% formic acid aqueous solution（B） for gradient elution（0-15 min， 2%-20%A； 15-25 min， 20%-25%A； 25-30 min， 25%-30%A； 30-45 min， 30%-31%A； 45-50 min， 31%-44%A； 50-65 min， 44%-45%A； 65-73 min， 45%-75%A； 73-95 min， 75%-100%A； 95-105 min， 100%A； 105-105.1 min， 100%-2%A； 105.1-120 min， 2%A）， the detection wavelength was 320 nm. Ultra high performance liquid chromatography-linear ion trap-electrostatic field orbitrap mass spectrometry（UHPLC-LTQ-Orbitrap MS） was used to identify the chemical components of KXS with electrospray ionization（ESI）， negative ion mode and scanning range of m/z 50-2 000. TLC identification methods for Poria and Ginseng Radix et Rhizoma in KXS were established. ResultThere were 11 common peaks in the specific chromatogram of KXS， attributed to Polygalae Radix， Poria and Acori Tatarinowii Rhizoma. Taking peak 9（α-asarone） as the reference peak， the relative standard deviations of the retention times of 15 batches of KXS samples were<0.2%. A total of 34 compounds were identified by UHPLC-LTQ-Orbitrap MS， including terpenoids， phenylpropanoids， oligosaccharides and ketones. The established TLC had good separation and was rapid， reliable， simple， feasible， suitable for the identification of Poria and Ginseng Radix et Rhizoma in KXS. ConclusionThe specific chromatogram and TLC of KXS are stable and reproducible. The material basis of KXS is basically clarified by MS， which can provide a reference for the development and quality control of KXS.
