A method for purifying citrus glycosides

A technology of citrus glycosides and citrus fruit, which is applied in the field of purification of natural plant monomers, can solve the problems of large consumption of eluents and inability to produce continuously and automatically, and achieve the effect of reducing the cost of purification

Active Publication Date: 2020-09-01
UNIV OF SCI & TECH LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing process for purifying citrus glycosides by column chromatography is a batch process, which consumes a lot of eluent and cannot be continuously and automatically produced

Method used

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  • A method for purifying citrus glycosides
  • A method for purifying citrus glycosides
  • A method for purifying citrus glycosides

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] 1. Prepare the crude extract of philodendron

[0058] Take 100g of crushed sympathetic fruit raw material, add 1L of ethanol, and ultrasonically leach twice at 60°C for 60min each time to obtain the leach solution; then concentrate the leach solution to 75mL, add 25mL of H 2 0, standing for stratification, removing the precipitate produced by the mixed solution, and getting the filtrate; diluting the filtrate with water-ethanol (5:5 by volume) to obtain the sample injection solution of the citrus citrus crude extract, wherein the citrus glycoside concentration is 0.56mg / mL, its chromatographic purity is 23.79%, see figure 1 .

[0059] 2. Using SMBC to purify xigoside from the crude extract of xigae fruit

[0060] 1) SMBC separation conditions are as follows:

[0061] Chromatographic column: 6 pieces, 1cm in diameter, 20cm in length;

[0062] Stationary phase: octadecylsilane bonded silica gel ODS, 20-30 μm;

[0063] Operation mode: 1-3-2, that is, eluting band: 1 c...

Embodiment 2

[0073] Except the following content, other conditions and steps are all with embodiment 1;

[0074] Preparation of sample solution for the crude extract of symphylla: crush 100 g of symphylla, then use a mixed solution of ethanol and water (volume ratio 7:3) for ultrasonic leaching twice at 60°C, each time for 60 min. The liquid ratio is 1:15 to obtain the leaching solution; after the leaching solution is concentrated and dried, add ethanol and water (7:3 by volume) 100mL to obtain a mixed solution, remove the precipitate of the mixed solution, and take the filtrate; use ethanol and water (volume Ratio of 5:5) to dilute the filtrate to obtain the sample injection solution of the crude extract of citrus citrus fruit, wherein the concentration of citrus glycosides is 1.14mg / mL.

[0075] The citrus extract was obtained from the outlet of the SMBC extract E, and the chromatographic purity and yield of citrus were 91.07% and 99.34%, respectively.

[0076] Post-processing the extra...

Embodiment 3

[0078] Except the following content, other conditions and steps are all with embodiment 1;

[0079] Preparation of sample solution for the crude extract of sympathetic fruit: After crushing 100g of sympathetic fruit, use a mixed solution of ethanol and water (volume ratio 7:3) for ultrasonic leaching twice, each ultrasonic leaching for 60min, the ratio of solid to liquid is 1 : 15, obtain leaching solution; Add ethanol and water (volume ratio 6: 4) 150mL after leaching solution thickening, obtain mixed solution, remove the precipitation of mixed solution, obtain filtrate; Use ethanol and water (volume ratio 6: 4) ) to dilute the filtrate to obtain the sample injection solution of the crude extract of citrus fruit, wherein the concentration of citrus glycosides is 1.0 mg / mL.

[0080] Chromatographic columns: 4 pieces, 2cm in diameter, 20cm in length;

[0081] Stationary phase: octadecylsilane bonded silica gel ODS, 30-40 μm;

[0082] Operating mode: 1-1-2;

[0083] Eluent P ...

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Abstract

The invention provides a method for purifying citrus glycosides, which belongs to the technical field of purification of natural plant monomers. In the method, firstly, the maggotin is extracted with an aqueous ethanol solution to obtain a crude extract of the maggot, and then three-band simulated moving bed chromatography is used to separate and purify the citrus in the crude extract of the citrus to obtain an extract of the citrus, and then the The extract is concentrated and crystallized to obtain high-purity citrusin. The method can purify citrus glycosides on a large scale and efficiently, and the simulated moving bed chromatographic separation process realizes robust, continuous and automatic operation, and the stationary phase and mobile phase can be used repeatedly, reducing the purification cost.

Description

technical field [0001] The invention belongs to the technical field of purification of natural plant monomers, and in particular relates to a method for purifying citrus glycosides. Background technique [0002] Campylocarpus is the fruit of a unique tree species of Campylodon chinensis in my country. Since ancient times, Campylodont cuba has been an important medicinal material among the people, and it can be used as a medicine for the whole plant to treat malignant toxins and tumors. The main chemical components in camptothecin include: camptothecin, 10-hydroxycamptothecin, 11-methoxycamptothecin, deoxycamptothecin, camptothecin, betulinic acid and citrusin. Studies have found that both citrus and camptothecin compounds have anticancer activity, and citrus also has the functions of antibacterial, antiviral, anti-inflammatory, labor pain and antipyretic. [0003] The citrus glycosides are extracted from the citrus citrus fruit, which has important practical value. The met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/00C07H1/08
CPCC07H1/08C07H17/00
Inventor 王绍艳姚海旭张伟石爽魏伯峰李守江
Owner UNIV OF SCI & TECH LIAONING
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