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Separation method of magnolia officinalis bisphenol

A separation method and Magnolia officinalis technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of difficulty in taking into account yield and purity, large solvent consumption, long production cycle, etc., and achieve high separation efficiency. , the method is simple, the effect of low input cost

Active Publication Date: 2018-02-02
北京国康本草物种生物科学技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the extraction methods of magnolol mainly include: heating reflux extraction, ultrasonic-assisted extraction, microwave-assisted extraction, supercritical CO 2 Fluid extraction, but it is generally difficult to balance the yield and purity, the amount of solvent used in the extraction is large, and the energy waste is serious.
For example: microwave-assisted extraction method has higher yield, but lower purity; while supercritical CO 2 The purity of the product obtained by fluid extraction is relatively high, but the yield is relatively low
However, the heating and reflux extraction method requires a large amount of solvent and a long production cycle.

Method used

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  • Separation method of magnolia officinalis bisphenol
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  • Separation method of magnolia officinalis bisphenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Thin-layer chromatography processes the extract of magnolobisphenol, adopts different solvents respectively, and concrete solvent is as follows:

[0058] PE: ETOH was mixed with volume ratios of 100:1, 50:1, 40:1, 30:1, 20:1 and 10:1, and the results of the thin-layer plates were as follows figure 1 shown. figure 1 The one on the left of each plate is the control group.

[0059] from figure 1 It can be seen that when the volume ratio of PE to ETOH is 10-20:1, magnolol and honokiol are well separated.

Embodiment 2

[0061] A method for separating magnolobisphenols, comprising the following steps:

[0062] Extraction: Magnolia officinalis bark (which contains 2.9% magnolol and 1.9% honokiol as detected by HPLC) is powdered and passed through 50 meshes, and 1000g is refluxed with 90% ethanol aqueous solution 6000g, 5000g and 4000g successively Extraction, the extraction temperature is 60°C, and the extraction time of each reflux is 2h, 1h, 1h;

[0063] The extracts were combined and concentrated to 10% of their volume, 300g of silica gel powder was added, and the concentration was continued until it became a fluid dry powder, about 600g.

[0064] Take a glass column with a volume of about 3000ml, add 200g of silica gel powder for wet packing, that is, mix silica gel powder with petroleum ether with a boiling point of 60-90°C and then wet pack it into the column until there are no bubbles, then add fluid dry powder for about 600g, finally add PE (petroleum ether 60-90°C) and ETOH (absolute ...

Embodiment 3

[0083] A method for separating magnolobisphenols, comprising the following steps:

[0084] Extraction: Magnolia officinalis root bark (the content of magnolol and honokiol in it is detected by HPLC) is powdered and passed through 40 meshes, and 1000g is taken to carry out reflux extraction with 92% ethanol aqueous solution 6000g, 5000g and 4000g successively , the extraction temperature is 50°C, and the extraction time for each reflux is 2h, 1h, and 1h in sequence;

[0085] The extracts were combined and concentrated to 8% of its volume, added with 300 g of silica gel powder, and continued to concentrate until it became a fluid dry powder.

[0086] Take a glass column with a volume of about 3000ml, add 200g of silica gel powder for wet packing, that is, mix silica gel powder with petroleum ether with a boiling point of 60-90°C and then wet pack it into the column until there are no bubbles, then add fluid dry powder for about 600g, finally add PE (petroleum ether 60-90°C) and...

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Abstract

The invention relates to the field of extraction separation, in particular to a separation method of magnolia officinalis bisphenol. A magnolia officinalis extract is separated with a mixed solution of petroleum ether and ethanol as the solvent. Currently, the magnolia officinalis bisphenol extraction technology is undeveloped, the yield is low, magnolol and honokiol have similar polarity and arenot easily separated. Use of resin as the adsorbent, and employment of methanol and ethanol as the eluent cannot acquire a bisphenol monomer, also the efficiency is low, and the solvent dosage is large. Use of silica gel as the carrier and adoption of petroleum ether and ethyl acetate as the eluent can cause serious waste of solvent. The inventor finds that the mixed solution of petroleum ether and ethanol can be employed as the solvent to separate the magnolia officinalis extract, can separate magnolol and honokiol effectively, and the effect is superior.

Description

technical field [0001] The invention relates to the field of extraction and separation, in particular to a method for separating magnolobisphenol. Background technique [0002] Magnolia officinalis is the dry dry bark, root bark and branch bark of Magnolia officinalis or Magnolia officinale. Bitter in the mouth, pungent, warm in nature. Return spleen, stomach, lung, large intestine channel. It is used for the treatment of dampness stagnation, vomiting and diarrhea, food stagnation and stagnation of Qi, abdominal distension and constipation, phlegm-retention asthma and cough. According to literature reports, magnolia officinalis also has the effect of relaxing muscles pharmacologically; small doses can excite intestinal smooth muscle, while large doses have inhibitory effect on intestinal smooth muscle; anti-ulcer effect, significant central inhibitory effect, lowering blood pressure, anti-pathogen Microorganisms, anti-tumor; anti-platelet and inhibition of intracellular c...

Claims

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Application Information

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IPC IPC(8): C07C37/82C07C39/21
CPCC07C37/82C07C39/21
Inventor 王代军陈松
Owner 北京国康本草物种生物科学技术研究院有限公司
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