Method for purifying protocatechuic acid by means of dilute alkali solution extraction and solid phase extraction column

A technology of solid phase extraction column and protocatechuic acid, which is applied in the field of dilute alkali solution extraction-solid phase extraction column purification of protocatechuic acid, can solve the problems that are not suitable for industrialized large-scale production, and achieve good decolorization and impurity removal effects, Good impurity removal effect and low energy consumption

Active Publication Date: 2018-02-27
CHINA AGRI UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The process conditions of the traditional Chinese medicine extraction method are relatively m

Method used

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  • Method for purifying protocatechuic acid by means of dilute alkali solution extraction and solid phase extraction column
  • Method for purifying protocatechuic acid by means of dilute alkali solution extraction and solid phase extraction column
  • Method for purifying protocatechuic acid by means of dilute alkali solution extraction and solid phase extraction column

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Effect test

Embodiment 1

[0034] Take Sijiqingye medicinal material, crush it, put it into an extraction tank, add 8 times the volume of 0.1% NaHCO3 solution to soak for 4 hours, extract at 90°C for 1 hour, filter, concentrate the filtrate to a relative density of 1.12 (60°C), adjust the pH to 2.0, add ethyl acetate Ester extracted 5 times, combined organic phases and concentrated, 5% NaHCO 3 Solution extraction, adjust the pH of the water phase to 2.0, extract with ether, concentrate the organic phase to obtain a yellow powder, dissolve the powder in 5% methanol solution, filter, inject the filtrate into a solid phase extraction column, detect by TLC, collect the effluent, and dissolve it in 5% methanol solution Wash the column, collect the effluent, combine the effluent, extract with ethyl acetate, concentrate, and recrystallize with water to obtain the product with a yield of 62.5% and a protocatechuic acid content of 99.1%.

[0035] The present embodiment provides the ultraviolet scan spectrum of p...

Embodiment 2

[0037] Take Sijiqingye medicinal material, crush it, put it into the extraction tank, add 8 times the volume of 0.08% NaHCO3 solution to soak for 4 hours, extract at 95°C for 2 hours, filter, concentrate the filtrate to a relative density of 1.12 (60°C), adjust the pH to 2.0, add ethyl acetate Extract the ester three times, combine the organic phases and concentrate, extract with 5% NaHCO3 solution, adjust the pH of the water phase to 2.0, extract with ether, concentrate the organic phase to obtain a yellow powder, dissolve the powder in 5% methanol solution, filter, and inject the filtrate into a solid phase extraction column. TLC detection, collecting the effluent, then washing the column with 5% methanol solution, collecting the effluent, combining the effluent, extracting with ethyl acetate, concentrating, recrystallizing with water to obtain the product, the yield is 61.8%, protocatechuic acid The content is 98.5%.

Embodiment 3

[0039] Take Sijiqingye herbs, crush them, put them into an extraction tank, add 10 times the volume of 0.08% NaHCO3 solution to soak for 4 hours, extract at 92°C for 1.5 hours, filter, concentrate the filtrate to a relative density of 1.15 (60°C), adjust the pH to 2.0, and add ethyl acetate Extract the ester 4 times, combine the organic phases and concentrate, extract with 5% NaHCO3 solution, adjust the pH of the water phase to 2.0, extract with ether, concentrate the organic phase to obtain a yellow powder, dissolve the powder in 5% methanol solution, filter, and inject the filtrate into a solid phase extraction column. TLC detection, collecting the effluent, then washing the column with 5% methanol solution, collecting the effluent, combining the effluent, extracting with ethyl acetate, concentrating, recrystallizing with water to obtain the product, the yield is 63.5%, protocatechuic acid The content is 98.3%.

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Abstract

The invention relates to a method for purifying protocatechuic acid by means of dilute alkali solution extraction and a solid phase extraction column. The method comprises the following steps: (1) crushing a raw material, i.e., leaves of ilex purpurea hassk, soaking the raw material into a dilute alkali solution and then carrying out heating extraction, concentrating an extracting solution and adjusting a pH value to be acidic, extracting with ethyl acetate, then collecting an organic phase and concentrating, then extracting with an alkaline solution, collecting a water phase and adjusting thepH value to be acidic, extracting with ethyl ether, and then collecting an organic phase and concentrating to obtain a solid extract; (2) dissolving the extract, obtained in the step (1), with a methanol aqueous solution, loading a sample onto the solid phase extraction column for purifying, and recrystallizing to obtain the protocatechuic acid. The method provided by the invention adopts the wayof dilute alkali solution extraction, thus achieving lower energy consumption; extraction is carried out under different pH conditions, so that the impurity removal effect is good; the used organic solvent can be repeatedly used after being recycled; the solid phase extraction column has good effects of decoloration and impurity removing, and effluent is directly collected, so that the process issimple; the product purity is more than 98%, the product yield is higher, and the method is simple and easy for industrial production.

Description

technical field [0001] The invention relates to a process method for purifying protocatechuic acid by dilute alkali solution extraction-solid phase extraction column, and a process method for preparing protocatechuic acid by using dilute alkali solution extraction, organic solvent extraction, solid phase extraction column separation and other processes. Background technique [0002] Protocatechuic acid is a phenolic acid compound, which is extracted with a dilute alkali solution to make protocatechuic acid into a salt, increase its water solubility and improve the transfer rate; Solid Phase Extraction (SPE) is based on the theory of liquid-solid phase chromatography , using selective adsorption and selective elution to enrich, separate, and purify samples is a physical extraction process that includes liquid and solid phases, and it can also be regarded as a simple chromatographic process. . The filler retention mechanism is divided into retention of target compounds and re...

Claims

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Application Information

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IPC IPC(8): C07C51/42C07C51/47C07C65/03
CPCC07C51/42C07C51/47C07C65/03
Inventor 何诚张家瑚
Owner CHINA AGRI UNIV
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