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A kind of preparation method of milk thistle extract with high content and low solvent 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, high production cost, etc., and achieve the effect of simple process and low solvent consumption

Active Publication Date: 2019-03-22
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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  • A kind of preparation method of milk thistle extract with high content and low solvent residue
  • A kind of preparation method of milk thistle extract with high content and low solvent residue

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preparation example Construction

[0015] Such as figure 1 As shown, the preparation method of high-content and low-soluble residue milk thistle extract disclosed in the present invention includes the following steps, (1), pressing: squeezing the washed and dried milk thistle seeds through a screw oil press, Obtain the milk thistle residue cake; (2) Extraction: pulverize the milk thistle residue cake obtained in step (1), mix with the extraction solvent to obtain a mixture, and extract the mixture through a reverse gradient circulation extraction equipment, and filter to obtain the extract; (3) Concentration: the extract obtained in step (2) is pumped into the outer circulation concentrator for concentration to obtain a concentrated liquid; (4), refining: the concentrated liquid obtained in step (3) is pumped into the spiral mixer Extraction is carried out in the liquid, and add n-hexane to the concentrated solution, heat and stir for 1 hour, the organic layer is pumped out, and the extraction operation is repea...

Embodiment 1

[0022] (1) Squeezing: Take 6 tons of milk thistle seeds and put them into a screw oil press at 150-200kg per hour for squeezing.

[0023] (2) Extraction: crush the squeezed milk thistle residue cake, extract with butanone 95±5% (V / V) and reverse gradient circulation extraction equipment, and filter the extract.

[0024] (3) Concentration: The extract is pumped into the external circulation concentrator for concentration, the concentration vacuum degree is -0.06Mpa, and the concentration temperature is 55°C.

[0025] (4) Refining: pump the concentrated liquid into a ribbon mixer for extraction, add 4 times the amount (V / V) of n-hexane to the concentrated liquid, heat at 45°C, stir and extract for 1 hour, and pass the organic layer through the pump Extraction and repeat the extraction operation 2 times; the water layer is concentrated under reduced pressure until solvent-free distillation to obtain liquid extract I; liquid extract I is dissolved with 20 times (V / V) 1% sodium hydroxide ...

Embodiment 2

[0030] (1) Squeezing: Take 6 tons of milk thistle seeds and put them into a screw oil press at 150-200kg per hour for squeezing.

[0031] (2) Extraction: crush the pressed milk thistle residue cake, extract with acetone 95±5% (V / V) and reverse gradient circulation extraction equipment, and filter the extract.

[0032] (3) Concentration: the extract is pumped into the external circulation concentrator for concentration, the concentration vacuum degree is -0.05Mpa, and the concentration temperature is 60℃.

[0033] (4) Refining: pump the concentrated liquid into a ribbon mixer for extraction, add 4 times the amount (V / V) of n-hexane to the concentrated liquid, heat at 48°C, stir and extract for 1 hour, and pass the organic layer through the pump Extraction and repeat the extraction operation 2 times; the water layer is concentrated under reduced pressure to solvent-free distillation to obtain the liquid extract I; the liquid extract I is dissolved with 20 times (V / V) 1.5% sodium hydrox...

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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

Technical field [0001] The invention relates to a preparation process of a milk thistle extract in the field of fine chemicals, in particular to a preparation method of a milk thistle extract with high content and low solubility. Background technique [0002] Silybum marianum is a one-year or two-year-old herbaceous plant of the Compositae family. Alias ​​Milk Thistle (Milk Thistle). Seeds are used as medicine. It is native to Western Europe and North Africa. China is cultivated in Shaanxi, Gansu, Heilongjiang and Hebei provinces. Silybum marianum seeds mainly contain flavonol compounds: silibinin, silibinin, silibinin, and silibinol. The above ingredients are now collectively referred to as silymarin or silymarin. They are the main ingredients for the treatment of liver diseases. [0003] [0004] Silymarin (structure as shown above), synonym: silymarin, silybin, etc., chemical name: 2α-[2,3-trans-2,3-dihydro-3-(4-hydroxy -3-Methoxyphenyl)-2-hydroxymethyl-1,4-benzodioxane-6-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D407/04
CPCC07D407/04
Inventor 戴珊媛
Owner NINGBO GREEN HEALTH PHARMACEUTICAL CO LTD