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Preparation method of milk thistle extract with high content and low soluble residue

A milk thistle, high-content technology, applied in organic chemistry and other fields, can solve the problems of difficult separation and purification, high price, large consumption of auxiliary raw materials, etc., and achieve the effect of simple process and low solvent consumption

Active Publication Date: 2014-03-19
NINGBO GREEN HEALTH PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the shell and kernel separation technology of milk thistle seeds is still a difficult technical problem, the method of preparing silybin can only use the traditional method of extracting active ingredients from the pressed cake of whole milk thistle seeds , the follow-up separation and purification of this traditional method is difficult, the content of the prepared silibinin is usually about 96%, and it can never exceed 98%, the residual amount of solvent in the finished product is large, the consumption of auxiliary raw materials is large, and the production cost is high
High-purity silibinin can only be obtained in a small amount in the laboratory, and its content is much higher than that of silibinin produced by traditional processes, which is expensive

Method used

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  • Preparation method of milk thistle extract with high content and low soluble residue
  • Preparation method of milk thistle extract with high content and low soluble residue

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preparation example Construction

[0018] Such as figure 1 As shown, the preparation method of milk thistle extract with high content and low solvent residue disclosed in the present invention includes the following steps, (1), pressing: pressing the cleaned and dried milk thistle seeds through a screw oil press, Obtaining milk thistle residue cake; (2), extraction: pulverizing the milk thistle residue cake obtained in step (1), mixing it with an extraction solvent to obtain a mixture, extracting through a reverse gradient circulation extraction device, and filtering to obtain an extract; (3) Concentration: pump the extract obtained in step (2) into an external circulation concentrator for concentration to obtain a concentrate; (4) Refining: pump the concentrate obtained in step (3) into a ribbon mixer Extraction was carried out in the concentrated solution, and n-hexane was added to the concentrated solution, heated and stirred for 1 hour, the organic layer was pumped off, and the extraction operation was ...

Embodiment 1

[0025] (1) Pressing: Take 6 tons of milk thistle seeds, put them in at 150-200 kg per hour and press them through a screw press.

[0026] (2) Extraction: crush the pressed milk thistle residue cake, extract with butanone 95±5% (V / V) and reverse gradient circulation extraction equipment, and filter to obtain the extract.

[0027] (3) Concentration: pump the extract into the external circulation concentrator for concentration, the concentration vacuum is -0.06Mpa, and the concentration temperature is 55°C.

[0028] (4) Refining: pump the concentrated solution into a ribbon mixer for extraction, add 4 times the amount (V / V) of n-hexane to the concentrated solution, heat at 45°C, stir and extract for 1 hour, and the organic layer passes through the pump Extract and repeat the extraction operation twice; the water layer is concentrated under reduced pressure until solvent-free distillation is obtained to obtain the liquid extract I; the liquid extract I is dissolved with 20 times t...

Embodiment 2

[0033] (1) Pressing: Take 6 tons of milk thistle seeds, put them in at 150-200 kg per hour and press them through a screw press.

[0034] (2) Extraction: crush the pressed milk thistle residue cake, extract with acetone 95±5% (V / V) and reverse gradient circulation extraction equipment, and filter to obtain the extract.

[0035] (3) Concentration: pump the extract into the external circulation concentrator for concentration, the concentration vacuum is -0.05Mpa, and the concentration temperature is 60°C.

[0036](4) Refining: pump the concentrated solution into a ribbon mixer for extraction, add 4 times the amount (V / V) of n-hexane to the concentrated solution, heat at 48°C, stir and extract for 1 hour, and the organic layer passes through the pump Extract and repeat the extraction operation twice; the water layer is concentrated under reduced pressure until solvent-free distillation is obtained to obtain the liquid extract I; the liquid extract I is dissolved with 20 times the...

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Abstract

The invention discloses a preparation method of a milk thistle extract with a high content and low soluble residue. The method comprises the following steps: (1) squeezing; (2) extracting; (3) condensing; (4) refining: pumping the condensed liquid obtained in the step (3) into a ribbon mixer to carry out an extracting treatment, adding n-hexane into the condensed liquid, heating, stirring and extracting for 1 hour, pumping out the organic layer, repeating the extracting operation twice, vacuum condensing the water layer until no solvent is distilled out so as to obtain paste I; dissolving the paste I by adopting an alkali-solution and acid-isolation method, adjusting the pH value of the solution to a range of 4 to 5 by using hydrochloric acid so as to obtain a mixed solution; pumping the mixed solution into a centrifugation machine to carry out a centrifugation treatment so as to obtain a sediment; (5) vacuum drying the sediment; (6) grinding, sieving, and mixing so as to obtain the target product. The preparation method of the milk thistle extract with a high content and low soluble residue has the advantages of simple technology, large processing amount, sufficient stirring, low solvent consumption, and high mixing efficiency, can shorten the extracting time, reduces the consumption of raw materials and auxiliary materials, reduces the solvent residue of milk thistle extract, and improves the content of milk thistle extract.

Description

[0001] technical field [0002] The invention relates to a preparation process of milk thistle extract in the field of fine chemical industry, in particular to a preparation method of milk thistle extract with high content and low dissolved residue. Background technique [0003] Milk thistle is an annual or biennial herb of the Asteraceae family. Alias ​​milk thistle (Milk Thistle). The seeds are used as medicine. Native to Western Europe and North Africa. China is cultivated in Shaanxi, Gansu, Heilongjiang and Hebei provinces. Milk thistle seeds mainly contain flavonol compounds: silybin, silybinin, silymarin, and silymarin. The above ingredients are now collectively called silymarin or silymarin, which are the main ingredients in the treatment of liver diseases. [0004] [0005] Silymarin (Silymarin) (structural formula shown above), synonym: Silymarin, silybin, etc., chemical name: 2α-[2,3-trans-2,3-dihydro-3-(4-hydroxy -3-methoxyphenyl)-2-hydroxymethyl-1,4-benz...

Claims

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Application Information

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IPC IPC(8): C07D407/04
CPCC07D407/04
Inventor 戴珊媛
Owner NINGBO GREEN HEALTH PHARMACEUTICAL CO LTD
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