CN108424940A - A kind of production method of the medicinal pectin of targeted therapy - Google Patents

A kind of production method of the medicinal pectin of targeted therapy Download PDF

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CN108424940A
CN108424940A CN201810329355.3A CN201810329355A CN108424940A CN 108424940 A CN108424940 A CN 108424940A CN 201810329355 A CN201810329355 A CN 201810329355A CN 108424940 A CN108424940 A CN 108424940A
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pectin
filter residue
volume
added
production method
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谢保明
刘帅
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Anhui Yu Ning Pectin Ltd By Share Ltd
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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/14Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/04Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds

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  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
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Abstract

The present invention provides a kind of production method of the medicinal pectin of targeted therapy, is related to pectin extraction technical field.Citrus pomace mainly boil filtering, EDTMPS water-baths are impregnated and filter residue is divided into two parts respectively by merging extraction pectin after complex enzyme a and complex enzyme b fermentation process by the pectin product, product of the present invention improves pectin when targeted drug is made and the calcification degree of the compound of calcium binding, enhances the therapeutic effect of drug.

Description

A kind of production method of the medicinal pectin of targeted therapy
Technical field
The present invention relates to pectin extraction technical fields, and in particular to a kind of production method of the medicinal pectin of targeted therapy.
Background technology
Nowadays very extensive in the application of field of medicaments pectin, wherein the segmented intestine targeted treatment in targeted therapy is used It is especially prominent, since the drug of segmented intestine targeted treatment mainly realizes therapeutic effect by oral drugs, after drug administration Upper gi tract does not discharge, and drug is delivered to after human body ileocecus and starts to be disintegrated or lose solution and release, is played in colon Locally or systemically therapeutic effect.Oral colon-target drug-delivery preparation is usually used in treating colonic diseases, such as colitis, colon cancer, Drug can be made directly to be discharged in diseased region, drug is made more effectively to play a role.
Pectin is a kind of natural macromolecular substance being present in plant cell wall, can be used as medicine controlled releasing or oral colon The carrier of target administration.And targeted drug positioning made from pectin is more accurate and reliable in medical research and application, is not easy It is influenced by other conditions, high stability.But pectin makes it be easy to carry due to swelling in environment in vivo because of it with hydrophily Preceding release drug.So calcium ion would generally be added when drug is made for general pectin makes its calcification, pectin water solubility is reduced, it is existing It is mostly used pectin common in the market in targeted drug preparation process, is not directed to the pectin production that medicinal property specially produces Product.
Invention content
In view of the shortcomings of the prior art, the present invention provides a kind of production method of the medicinal pectin of targeted therapy, pectin is improved Viscosity, increase pectin purity, while making pectin preferably and calcium binding.
In order to achieve the above object, the present invention provides a kind of production method of the medicinal pectin of targeted therapy, it is as follows:
(1) it chooses orange peel and cleans crushing, be placed in boiling water and boil 15-20min, pomace is obtained by filtration;(2) by step (1) the pomace squeezing removal excessive moisture in, adds EDTMPS aqueous solutions, adjusts pH value 3.5, be warming up to 30-40 DEG C, heat preservation 60-70min is stirred, filter residue is obtained by filtration, filter residue is divided into two parts, respectively filter residue a and filter residue b;
(3) the filter residue a in above-mentioned steps (2) is added to the deionized water of 2-3 times of volume, adds 0.001-0.03 times of body Long-pending complex enzyme a is warming up to 60-70 DEG C, and filter residue c is obtained by filtration after keeping the temperature 12-15h;
(4) the filter residue b in above-mentioned steps (2) is added to the deionized water of 2-3 times of volume, adds 0.001-0.03 times of body Long-pending complex enzyme b is warming up to 60-70 DEG C, and filter residue d is obtained by filtration after keeping the temperature 12-15h;
(5) the filter residue c in above-mentioned steps (3) is added to the deionized water of 10-15 times of volume, is warming up to 80-90 DEG C of stirring Be filtered after 10-15min, obtain pectin solution a, by the filter residue d in step (4) be added 10-15 times of volume go from Sub- water is filtered after being warming up to 80-90 DEG C of stirring 10-15min, obtains pectin solution b;
(6) pectin solution a and pectin solution b are mixed evenly, are concentrated in vacuo to the 3%-4% of original volume, obtain To mixed concentrated liquid;
(7) mixed concentrated liquid in above-mentioned steps (6) is added under 95% ethanol solution room temperature of 1.5-3 times of volume and is stirred It is filtered after 10-15min, obtains crude pectin, after crude pectin is rinsed 2 times repeatedly with the ethanol solution of 70%-75% Pectin is obtained, vacuum drying chamber is put into and exists
6-7h is dried at a temperature of 80-85 DEG C and obtains solid-state pectin, then solid-state pectin be crushed into 150 mesh sieve to get to originally Invention product.
The composition and mass ratio of complex enzyme a wherein described in step (3) be:Cellulase: hemicellulase: protopectinase : transmethylase=3: 2: 1: 1;The composition and mass ratio of complex enzyme b described in step (4) be:Cellulase: glycosidase: Portugal Grape sugar former times transferase: fumarase=4: 2: 1: 1;And it is small every half during heat preservation 12-15h in step (3) and step (4) When stir 3-5min.
The present invention provides a kind of production method of the medicinal pectin of targeted therapy, and advantage is compared with prior art:
(1) pomace is divided into two parts by the present invention in pomace processing procedure, respectively with after different mixed enzyme fermentation processing Merge, is conducive to stablize the effect of drug is made in later stage pectin, increases the purity that pectin is made.
(2) complex enzyme that the present invention uses can effectively increase the adhesiveness of product pectin, while increase pectin and calcium ion Calcification degree in conjunction with after, to enhance the effect that the later stage synthesizes targeted drug.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, with reference to the embodiment of the present invention pair Technical solution in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is a part of the invention Embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making wound The every other embodiment obtained under the premise of the property made labour, shall fall within the protection scope of the present invention.
Embodiment 1:
A kind of production method of the medicinal pectin of targeted therapy, is as follows:
(1) it chooses orange peel and cleans crushing, be placed in boiling water and boil 15-20min, pomace is obtained by filtration;(2) by step (1) the pomace squeezing removal excessive moisture in, adds EDTMPS aqueous solutions, adjusts pH value 3.5, be warming up to 30-40 DEG C, heat preservation 60-70min is stirred, filter residue is obtained by filtration, filter residue is divided into two parts, respectively filter residue a and filter residue b;
(3) the filter residue a in above-mentioned steps (2) is added to the deionized water of 2-3 times of volume, adds 0.001-0.03 times of body Long-pending complex enzyme a is warming up to 60-70 DEG C, and filter residue c is obtained by filtration after keeping the temperature 12-15h;
(4) the filter residue b in above-mentioned steps (2) is added to the deionized water of 2-3 times of volume, adds 0.001-0.03 times of body Long-pending complex enzyme b is warming up to 60-70 DEG C, and filter residue d is obtained by filtration after keeping the temperature 12-15h;
(5) the filter residue c in above-mentioned steps (3) is added to the deionized water of 10-15 times of volume, is warming up to 80-90 DEG C of stirring Be filtered after 10-15min, obtain pectin solution a, by the filter residue d in step (4) be added 10-15 times of volume go from Sub- water is filtered after being warming up to 80-90 DEG C of stirring 10-15min, obtains pectin solution b;
(6) pectin solution a and pectin solution b are mixed evenly, are concentrated in vacuo to the 3%-4% of original volume, obtain To mixed concentrated liquid;
(7) mixed concentrated liquid in above-mentioned steps (6) is added under 95% ethanol solution room temperature of 1.5-3 times of volume and is stirred It is filtered after 10-15min, obtains crude pectin, after crude pectin is rinsed 2 times repeatedly with the ethanol solution of 70%-75% Pectin, be put into baking box and dry 6-7h at a temperature of 80-85 DEG C and obtain solid-state pectin, then solid-state pectin be crushed into 150 mesh Sieve is to get to product of the present invention.
The composition and mass ratio of complex enzyme a wherein described in step (3) be:Cellulase: hemicellulase: protopectinase : transmethylase=3: 2: 1: 1;The composition and mass ratio of complex enzyme b described in step (4) be:Cellulase: glycosidase: Portugal Grape sugar former times transferase: fumarase=4: 2: 1: 1;And it is small every half during heat preservation 12-15h in step (3) and step (4) When stir 3-5min.
Embodiment 2:
A kind of production method of the medicinal pectin of targeted therapy, is as follows:
(1) it chooses orange peel and cleans crushing, be placed in boiling water and boil 15-20min, pomace is obtained by filtration;(2) by step (1) the pomace squeezing removal excessive moisture in, adds EDTMPS aqueous solutions, adjusts pH value 3.5, be warming up to 30-40 DEG C, heat preservation 60-70min is stirred, filter residue is obtained by filtration, filter residue is divided into two parts, respectively filter residue a and filter residue b;
(3) the filter residue a in above-mentioned steps (2) is added to the deionized water of 2-3 times of volume, adds 0.001-0.03 times of body Long-pending complex enzyme a is warming up to 60-70 DEG C, and filter residue c is obtained by filtration after keeping the temperature 12-15h;
(4) the filter residue b in above-mentioned steps (2) is added to the deionized water of 2-3 times of volume, adds 0.001-0.03 times of body Long-pending complex enzyme b is warming up to 60-70 DEG C, and filter residue d is obtained by filtration after keeping the temperature 12-15h;
(5) the filter residue c in above-mentioned steps (3) is added to the deionized water of 10-15 times of volume, is warming up to 80-90 DEG C of stirring Be filtered after 10-15min, obtain pectin solution a, by the filter residue d in step (4) be added 10-15 times of volume go from Sub- water is filtered after being warming up to 80-90 DEG C of stirring 10-15min, obtains pectin solution b;
(6) pectin solution a and pectin solution b are mixed evenly, are concentrated in vacuo to the 3%-4% of original volume, obtain To mixed concentrated liquid;
(7) mixed concentrated liquid in above-mentioned steps (6) is added under 95% ethanol solution room temperature of 1.5-3 times of volume and is stirred It is filtered after 10-15min, obtains crude pectin, after crude pectin is rinsed 2 times repeatedly with the ethanol solution of 70%-75% Pectin is obtained, vacuum drying chamber is put into and exists
6-7h is dried at a temperature of 80-85 DEG C and obtains solid-state pectin, then solid-state pectin be crushed into 150 mesh sieve to get to originally Invention product.
The composition and mass ratio of complex enzyme a wherein described in step (3) be:Cellulase: hemicellulase: protopectinase : transmethylase=3: 1: 1: 1;The composition and mass ratio of complex enzyme b described in step (4) be:Cellulase: glycosidase: Portugal Grape sugar former times transferase: fumarase=4: 2: 1: 1;And it is small every half during heat preservation 12-15h in step (3) and step (4) When stir 3-5min.
Embodiment 3:
A kind of production method of the medicinal pectin of targeted therapy, is as follows:
(1) it chooses orange peel and cleans crushing, be placed in boiling water and boil 15-20min, pomace is obtained by filtration;(2) by step (1) the pomace squeezing removal excessive moisture in, adds EDTMPS aqueous solutions, adjusts pH value 3.5, be warming up to 30-40 DEG C, heat preservation 60-70min is stirred, filter residue is obtained by filtration, filter residue is divided into two parts, respectively filter residue a and filter residue b;
(3) the filter residue a in above-mentioned steps (2) is added to the deionized water of 2-3 times of volume, adds 0.001-0.03 times of body Long-pending complex enzyme a is warming up to 60-70 DEG C, and filter residue c is obtained by filtration after keeping the temperature 12-15h;
(4) the filter residue b in above-mentioned steps (2) is added to the deionized water of 2-3 times of volume, adds 0.001-0.03 times of body Long-pending complex enzyme b is warming up to 60-70 DEG C, and filter residue d is obtained by filtration after keeping the temperature 12-15h;
(5) the filter residue c in above-mentioned steps (3) is added to the deionized water of 10-15 times of volume, is warming up to 80-90 DEG C of stirring Be filtered after 10-15min, obtain pectin solution a, by the filter residue d in step (4) be added 10-15 times of volume go from Sub- water is filtered after being warming up to 80-90 DEG C of stirring 10-15min, obtains pectin solution b;
(6) pectin solution a and pectin solution b are mixed evenly, are concentrated in vacuo to the 3%-4% of original volume, obtain To mixed concentrated liquid;
(7) mixed concentrated liquid in above-mentioned steps (6) is added under 95% ethanol solution room temperature of 1.5-3 times of volume and is stirred It is filtered after 10-15min, obtains crude pectin, after crude pectin is rinsed 2 times repeatedly with the ethanol solution of 70%-75% Pectin, be put into baking box and dry 6-7h at a temperature of 80-85 DEG C and obtain solid-state pectin, then solid-state pectin be crushed into 150 mesh Sieve is to get to product of the present invention.
The composition and mass ratio of complex enzyme a wherein described in step (3) be:Cellulase: hemicellulase: protopectinase : transmethylase=3: 2: 1: 1;The composition and mass ratio of complex enzyme b described in step (4) be:Cellulase: glycosidase: Portugal Grape sugar former times transferase: fumarase=3: 2: 1: 1;And it is small every half during heat preservation 12-15h in step (3) and step (4) When stir 3-5min.
Embodiment 4:
Pectin of the present invention and common pectin is detected with the mixed compound of calcium ion situation miscible with water to change:
Choose resulting product pectin of the present invention and three parts of pectin and calcium ion compound be made, be respectively labeled as experimental group 1, Experimental group 2, experimental group 3;Take on the market common pectin be control group, be divided into trisection, Pectin calcium be made in the same fashion Ion complex is designated as control group 1, control group 2 and control group 3.Again by experimental group and control group in identical temperature and environment Under be placed in the deionized water of 10 times of volume parts of compound, at the uniform velocity stirred with the speed of 40r/s, respectively 5min, 10min, (degree of being dissolved into is divided into no dissolving, oligodynamical, Shao Liangrong to the dissolving situation of measurement compound when 20min, 40min, 100min Solution, a large amount of dissolvings).
The production method of pectin wherein of the present invention is:
A kind of production method of the medicinal pectin of targeted therapy, is as follows:
(1) it chooses orange peel and cleans crushing, be placed in boiling water and boil 15-20min, pomace is obtained by filtration;(2) by step (1) the pomace squeezing removal excessive moisture in, adds EDTMPS aqueous solutions, adjusts pH value 3.5, be warming up to 30-40 DEG C, heat preservation 60-70min is stirred, filter residue is obtained by filtration, filter residue is divided into two parts, respectively filter residue a and filter residue b;
(3) the filter residue a in above-mentioned steps (2) is added to the deionized water of 2-3 times of volume, adds 0.001-0.03 times of body Long-pending complex enzyme a is warming up to 60-70 DEG C, and filter residue c is obtained by filtration after keeping the temperature 12-15h;
(4) the filter residue b in above-mentioned steps (2) is added to the deionized water of 2-3 times of volume, adds 0.001-0.03 times of body Long-pending complex enzyme b is warming up to 60-70 DEG C, and filter residue d is obtained by filtration after keeping the temperature 12-15h;
(5) the filter residue c in above-mentioned steps (3) is added to the deionized water of 10-15 times of volume, is warming up to 80-90 DEG C of stirring Be filtered after 10-15min, obtain pectin solution a, by the filter residue d in step (4) be added 10-15 times of volume go from Sub- water is filtered after being warming up to 80-90 DEG C of stirring 10-15min, obtains pectin solution b;
(6) pectin solution a and pectin solution b are mixed evenly, are concentrated in vacuo to the 3%-4% of original volume, obtain To mixed concentrated liquid;
(7) mixed concentrated liquid in above-mentioned steps (6) is added under 95% ethanol solution room temperature of 1.5-3 times of volume and is stirred It is filtered after 10-15min, obtains crude pectin, after crude pectin is rinsed 2 times repeatedly with the ethanol solution of 70%-75% Pectin is obtained, vacuum drying chamber is put into and exists
6-7h is dried at a temperature of 80-85 DEG C and obtains solid-state pectin, then solid-state pectin be crushed into 150 mesh sieve to get to originally Invention product.
The composition and mass ratio of complex enzyme a wherein described in step (3) be:Cellulase: hemicellulase: protopectinase : transmethylase=3: 2: 1: 1;The composition and mass ratio of complex enzyme b described in step (4) be:Cellulase: glycosidase: Portugal Grape sugar former times transferase: fumarase=4: 2: 1: 1;And it is small every half during heat preservation 12-15h in step (3) and step (4) When stir 3-5min.
The production method of Pectin calcium ion complex is:
The calcium hydroxide solution that pectin and calcium ion concentration are 0.02mol/L is taken fully to be mixed with the ratio that mass ratio is 1: 3 Filter residue is filtered to obtain after conjunction, and filter residue is dried into obtain Pectin calcium ion complex.
Specific experiment situation such as following table:
By upper table test result it is found that the pectin obtained by the present invention in the compound formed with calcium ion than common pectin More stablize with calcium ion formation compound and hydrophobicity is more preferable, is i.e. calcification is more complete, for the pharmaceutical synthesis of targeted therapy Using effect is more perfect.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although with reference to the foregoing embodiments Invention is explained in detail, it will be understood by those of ordinary skill in the art that:It still can be to aforementioned each implementation Technical solution recorded in example is modified or equivalent replacement of some of the technical features;And these modification or It replaces, the spirit and scope for various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution.

Claims (4)

1. a kind of production method of the medicinal pectin of targeted therapy, which is characterized in that the production method of the pectin includes following step Suddenly:
(1) it chooses orange peel and cleans crushing, be placed in boiling water and boil 15-20min, pomace is obtained by filtration;
(2) by the pomace squeezing removal excessive moisture in step (1), EDTMPS aqueous solutions is added, pH value 3.5, heating are adjusted To 30-40 DEG C, filter residue is obtained by filtration in insulated and stirred 60-70min, and filter residue is divided into two parts, respectively filter residue a and filter residue b;
(3) the filter residue a in above-mentioned steps (2) is added to the deionized water of 2-3 times of volume, adds 0.001-0.03 times of volume Complex enzyme a is warming up to 60-70 DEG C, and filter residue c is obtained by filtration after keeping the temperature 12-15h;
(4) the filter residue b in above-mentioned steps (2) is added to the deionized water of 2-3 times of volume, adds 0.001-0.03 times of volume Complex enzyme b is warming up to 60-70 DEG C, and filter residue d is obtained by filtration after keeping the temperature 12-15h;
(5) the filter residue c in above-mentioned steps (3) is added to the deionized water of 10-15 times of volume, is warming up to 80-90 DEG C of stirring 10- It is filtered after 15min, obtains pectin solution a, the filter residue d in step (4) is added to the deionization of 10-15 times of volume Water is filtered after being warming up to 80-90 DEG C of stirring 10-15min, obtains pectin solution b;
(6) pectin solution a and pectin solution b are mixed evenly, are concentrated in vacuo to the 3%-4% of original volume, are mixed Close concentrate;
(7) mixed concentrated liquid in above-mentioned steps (6) is added under 95% ethanol solution room temperature of 1.5-3 times of volume and stirs 10- It is filtered after 15min, obtains crude pectin, fruit is obtained after crude pectin is rinsed 2 times repeatedly with the ethanol solution of 70%-75% Glue, is put into vacuum drying chamber and dries 6-7h at a temperature of 80-85 DEG C and obtain solid-state pectin, then solid-state pectin crushed 150 mesh Sieve is to get to this product.
2. a kind of production method of the medicinal pectin of targeted therapy according to claim 1, which is characterized in that step (3) institute The composition and mass ratio of the complex enzyme a stated be:Cellulase: hemicellulase: protopectinase: transmethylase=3: 2: 1: 1.
3. according to a kind of production method of the medicinal pectin of targeted therapy described in claim 1, which is characterized in that step (4) is described Complex enzyme b composition and mass ratio be:Cellulase: glycosidase: glucose former times transferase: fumarase=4: 2: 1: 1.
4. according to a kind of production method of the medicinal pectin of targeted therapy described in claim 1, it is characterised in that:Step (3) and step Suddenly in (4) during heat preservation 12-15h 3-5min is stirred every half an hour.
CN201810329355.3A 2018-04-13 2018-04-13 A kind of production method of the medicinal pectin of targeted therapy Pending CN108424940A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN103275242A (en) * 2013-06-18 2013-09-04 烟台安德利果胶股份有限公司 Pectin manufacture technology
CN103923225A (en) * 2014-04-23 2014-07-16 赛珂睿德生物医药科技(上海)有限公司 Method for preparing citrus pectin
CN104086667A (en) * 2014-06-11 2014-10-08 安徽农业大学 Method for preparing pectin from citrus fruit peel residues by employing ultrasonic-assisted extraction

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103232555A (en) * 2013-05-16 2013-08-07 内江师范学院 Method for extracting pectin from lemon peel residues by utilizing enzymatic method
CN103275242A (en) * 2013-06-18 2013-09-04 烟台安德利果胶股份有限公司 Pectin manufacture technology
CN103923225A (en) * 2014-04-23 2014-07-16 赛珂睿德生物医药科技(上海)有限公司 Method for preparing citrus pectin
CN104086667A (en) * 2014-06-11 2014-10-08 安徽农业大学 Method for preparing pectin from citrus fruit peel residues by employing ultrasonic-assisted extraction

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
GARY WILLIAMSON等: "Gelation of Sugarbeet and Citrus Pectins using Enzymes Extracted from Orange Peel", 《CARBOHYDRATE POLYMERS》 *
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