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Method for extracting brevifolin from Relinqing granula raw material and method for preparation quality control

A technique of brucella phenol and thermal rinsing can be applied in chemical instruments and methods, material separation, material analysis, etc., and can solve the problems of few research reports on Polygonum cephalus.

Active Publication Date: 2013-12-18
GUIZHOU WARMEN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Relinqing granule, which uses Polygonum cephalosporin as the main raw material, is clinically used to treat urinary system infections, and is included in the first part of the "Chinese Pharmacopoeia" 2010 edition. However, there are few research reports on Polygonum cephalosa at home and abroad. The literature preliminarily believes that flavonoids and phenolic acids are the active ingredients of Polygonum cephalum [1-4]

Method used

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  • Method for extracting brevifolin from Relinqing granula raw material and method for preparation quality control
  • Method for extracting brevifolin from Relinqing granula raw material and method for preparation quality control
  • Method for extracting brevifolin from Relinqing granula raw material and method for preparation quality control

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1: Preparation of Polygonum cephalum water extraction powder ethyl acetate crude extract

[0044] Take 150g of water-extracted Polygonum cephalum powder, soak it in 10 times the amount of 80% ethanol overnight, extract it ultrasonically for 30 minutes, filter, evaporate the filtrate to dryness with a rotary evaporator, add 150mL of water to dissolve, filter, and extract the filtrate to the upper layer with ethyl acetate colorless. The ethyl acetate layers were combined and evaporated to dryness with a rotary evaporator to obtain 12.7 g of ethyl acetate crude extract (extract) of Polygonum cephalosa water extraction powder, which was sealed in a desiccator for future use.

Embodiment 2

[0045] Example 2: Preparation of Polygonum cephalum secondary separation raw material

[0046] Take by weighing 1.0 g of the ethyl acetate extract obtained in Example 1, use the HSCCC solvent system n-hexane: ethyl acetate: methanol: water (1:5:1:5) to separate, collect fractions from 53min to 74min, repeat the process The operation was performed four times, the collected fractions were combined, and the solvent was evaporated to dryness with a rotary evaporator to obtain 0.25 g of the raw material of Polygonum cephalosa secondary separation.

Embodiment 3

[0047] Embodiment 3: the purity of high performance liquid chromatography determination test product

[0048] High performance liquid chromatography conditions: The stationary phase is Venusil MP C 18 Chromatographic column (4.6mm * 250mm, 5 μ m, Agela Technologie company), mobile phase is methanol and 0.2% phosphoric acid aqueous solution, gradient elution, wherein the gradient ratio of organic phase is as follows: 5% (0min)~30% (5min)~ 65% (20min) ~ 65% (24min) ~ 5% (25min) ~ 5% (30min). The detection wavelength is 272 nm, the flow rate is 1.0 mL / min, the column temperature is room temperature, and the injection volume is 20 μL.

[0049] The preparation of the test solution for the secondary separation raw material of Polygonum cephalum for purity determination by dry HPLC: Take 0.0150 g of the secondary separation raw material of Polygonum cephalum water obtained in Example 2, add 50% methanol water to constant volume in a 10 mL volumetric flask, make a solution with...

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Abstract

The invention relates to a method for extracting brevifolin and / or quercitrin from a Relinqing granula raw material such as polygonum capitatum water extract and also relates to a method for quality control of Relinqing granules by brevifolin. The method for extracting brevifolin and / or quercitrin utilizes a high-speed countercurrent chromatograph (HSCCC) and a mixture as a HSCCC solvent system to realize separation, wherein the mixture comprises n-hexane, ethyl acetate, methanol and water and a ratio of n-hexane, ethyl acetate, methanol to water is 1: (4-6): (0.8-1.2): (4-6). The method for extracting brevifolin realizes high purity and high yield extraction of brevifolin from a Relinqing granula raw material and brevifolin can be used as a reference substance in quality monitoring of a polygonum capitatum preparation such as Relinqing granules.

Description

technical field [0001] The invention belongs to the technical field of traditional Chinese medicine, and relates to a method for extracting brevifolia hematoxylin from raw materials of Relinqing granules, for example, a method for extracting brevifolia hematoxylin from the water extract of Polygonum cephalum, and also relates to extracting brevichematoxylin from raw materials of Relinqing granules or flower head A method for extracting brevifolia hematoxylin and quercitrin from Polygonum water extract. The present invention further relates to a method for monitoring the quality of the Relinqing granule preparation by using brevifolia hematoxylin. Background technique [0002] Polygonum capitatum is the dried whole herb or aboveground part of Polygonum capitatum Buch.-Ham.ex D.Don, a plant of the Polygonaceae family. Antibacterial, anti-inflammatory, diuretic and stranguria-relieving effects (Food and Drug Administration of Guizhou Province. Quality Standards of National Tra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/84C07C45/78C07C45/79C07H17/07C07H1/08G01N30/02
Inventor 梁斌黄民刘培庆万金志张丽艳李孟林谢宇陈欣霞唐靖雯
Owner GUIZHOU WARMEN PHARMA