CN101906169B - Process combination for preparing bletilla polysaccharide - Google Patents

Process combination for preparing bletilla polysaccharide Download PDF

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CN101906169B
CN101906169B CN2009103029373A CN200910302937A CN101906169B CN 101906169 B CN101906169 B CN 101906169B CN 2009103029373 A CN2009103029373 A CN 2009103029373A CN 200910302937 A CN200910302937 A CN 200910302937A CN 101906169 B CN101906169 B CN 101906169B
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bsp
preparation
filtration
bletilla striata
water
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CN101906169A (en
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宋力飞
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ZELI MEDICINE TECH Co Ltd GUANGZHOU
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ZELI MEDICINE TECH Co Ltd GUANGZHOU
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Abstract

The invention mainly relates to a low-temperature preparation method for bletilla polysaccharide, in particular to a process combination for preparing high-purity bletilla polysaccharide at a low temperature by adopting a core process of homogenization-based extraction and ceramic membrane micro-filtration concentration and using water as a solvent.

Description

A kind of process combination of BSP preparation
Technical field
The present invention relates generally to a kind of low temperature preparation method of BSP, especially a kind of process combination that combines ceramic membrane micro-filtration simmer down to core process low temperature to prepare BSP of extracting based on homogenization.
Background technology
The bletilla striata (Bletilla striata (Thunb.) Reichb.f) is a orchid family bletilla striata platymiscium, claims the little bletilla striata, lotus and grass, snow such as end etc. again, uses as traditional Chinese medicine over the past thousands of years always, and its major function is to hold back sore hemostasis, tonifying lung, detumescence and promoting granulation etc.Contain a large amount of water-soluble fluidity polysaccharide in the bletilla striata bulb, its chemical ingredients is a glucomannan, is the main function composition of the bletilla striata.
Purity of polysaccharide is greater than 90% bletilla striata glue, can in water, dissolve to form heavy-gravity wetting ability glue, and 2% bletilla striata glue solution viscosity is 9~12mm 2/ s is a kind of good whole food thickening material.Bletilla striata glue pharmaceutically has the effect anti-oxidant, that external application promotes the keratinocyte migration of taking orally; Can be used as arterial embolic agent and be used for liver cancer treatment, also can be used for treating hemostasis in ulcerative colitis, the operation, upper gastrointestinal massive hemorrhage and promotion wound skin healing etc.; In foodstuffs industry, can be used as the natural fruit coating antistaling agent important source material, can improve systems such as oil-in-water type essence, water-latex type local flavor flavor oil, milk-contained drink stability; Bletilla striata glue still is natural daily use chemicals additive of a kind of ideal and functional ingredient.Bletilla striata glue makeup split, stimulate circulation, improve the skin-nourishing situation, prevent that the wrinkle generation from having obvious effect control skin pernio and glass, and do not have toxic side effects.
Extract BSP usually with water or the hot extracting mode of aqueous ethanol; Because the viscosity and the water-soluble bloated characteristic of BSP; In leaching process, must replenish new extraction solvent in good time or increase and extract batch; Production cycle is long, quantity of solvent is big, energy consumption is higher, and the purity of BSP generally is lower than 80% in the product of preparation, and needs employing ethanol repeatedly measures such as deposition, ether and acetone class organic solvent washing all improves with its purity.
Summary of the invention
The low temperature preparation method that the purpose of this invention is to provide a kind of BSP, especially a kind of extraction combines the low temperature of ceramic membrane micro-filtration simmer down to core process to prepare the process combination of BSP based on homogenization.。
The present invention realizes through adopting following technical proposals: bletilla striata raw material through clean, pulverizing, homogenization, centrifugal, filtering, micro-filtration concentrate, process gelationus liquid BSP, or further liquid concentrator alcohol precipitation, drying processed the solid BSP.
The present invention adopts following concrete steps:
1. clean: with the inorganic impurities such as silt of extract at room temperature with the most plant material of washing.
2. pulverize: the bletilla striata is crushed to below the 1.5mm.
3. mix: in the bletilla striata of pulverizing, add the extraction water of the following temperature of normal temperature, making total amount of water is 20~300 times of bletilla striata medicinal material powder charging capacity, and mixes into uniform suspension.
4. homogenization: uniform suspension is used the clarifixator homogenization.
5. sedimentation is centrifugal: through the centrifugal water-insoluble particle of removing of sedimentation.
6. media filtration: centrifugate is no visual visible particle in media filtration to filtrating.
7. micro-filtration concentrates: the ceramic membrane filter device with filtering accuracy 2000~100nm carries out tangential flow filtration, and collection needs the micro-filtration of concentration to keep liquid.Get the colloidal liquid BSP.
8. alcohol precipitation: in gluey BSP, add ethanol, collecting precipitation.
9. dry: deposition vacuum-drying to the moisture of alcohol precipitation below 8%, is pulverized, the solid BSP.
Pulverizing according to the invention is meant that the kibbler with the following aperture of prepackage 2mm web plate is ground into the powder below the 1.5mm with the bletilla striata, generally pre-installs the web plate of 0.5~1.5mm, and the best is the web plate of 0.8~1.2mm.
The extraction water of the following temperature of normal temperature according to the invention is meant the primary reverse osmosis water below 30 ℃, general 15~30 ℃, and best 20~25 ℃.
The consumption of extraction water according to the invention is 20~300 times of bletilla striata medicinal material powder charging capacity, is generally 50~200 times, and the best is 80~120 times.
Homogenization according to the invention is meant with high pressure homogenizer and handles bletilla striata powder and the suspension that extracts water, homogenate after the processing is left standstill do not produce tangible deposition in 2 hours; The processing pressure of high pressure homogenizer can be selected between 5~75MPa, is generally 20~60MPa, and the best is 45~55MPa.
Media filtration according to the invention is meant sedimentation centrifugate through filtration medium filter to clarification, and filtration medium comprises one or more the mixing in filter cloth, filter paper and flocculating aids talcum powder, gac, the zeyssatite.General zeyssatite and the talcous arbitrary ratio mixture of using, the best is selected zeyssatite and 1: 1 mixture of talcum powder for use.
The mode of media filtration according to the invention can be press filtration, vacuum filtration, and flocculating aids can be pre-installed and on strainer, overlay filtration, also can be to mix slurry to filter with sedimentation centrifugate, or overlay filtration and mix the filtering combination of slurry.
Micro-filtration according to the invention is meant the ceramic membrane filter of filtering accuracy 2000nm~100nm, generally selects the ceramic membrane of 800nm~100nm for use, and the best is selected the ceramic membrane combination of 500nm~200nm for use.
Micro-filtration according to the invention keeps liquid, is meant the trapped fluid of ceramic membrane filter, holds back liquid measure and generally is equivalent to 2~20 times of bletilla striata medicinal material powder charging capacity, is generally 5~15 times, and the best is 6~10 times.
The present invention has the following advantages:
1. cold operation: except that drying process, all the other operations are all carried out at normal temperature, have reduced the problems such as color burn in the technological process, have solved the cold cut problem of product simultaneously.
2. adopt high-pressure homogeneous homogenization mode, improve cell crashing ratio as far as possible, extraction efficiency obviously improves.
3. process serialization: all processes can be accomplished in dynamic successive processes.
Embodiment
For better understanding ultimate principle of the present invention, we will specifically set forth principle of the present invention through following examples.Following description, can make the present technique field other people under various situation, use the present invention, deacclimatize the different application of expection with various correction.
Any additional application of explanation that this paper enumerates invention principle all relates to the technology of association area and to the ownership of these open materials, all is considered as included in the scope of claim involved in the present invention.Contents such as the solvent ratio that relates to, filtration medium, micro-filtration precision are to further specific descriptions of the present invention but not limitation of the present invention.
Embodiment 1
The preparation of bletilla striata Crude polysaccharides:
Major equipment: Universalpulverizer, auger tank, high pressure homogenizer, tripod pendulum type batch centrifugal, kieselguhr filter, 500+200nm ceramic membrane filter device, Alcohol-settling tank, vacuum drying oven.
Raw material: bletilla striata medicine materical crude slice 5kg.
The preparation process:
1. pulverizing: the Universalpulverizer with prepackage 1.2mm screen cloth is pulverized bletilla striata medicine materical crude slice, makes all and sieves through No. two, gets bletilla striata meal.
2. mix: bletilla striata meal and 500kg20? Primary reverse osmosis water put altogether in the auger tank, stirred 15 minutes, make to be mixed into bletilla striata suspension.
3. homogenization: bletilla striata suspension input high pressure is pressed clarifixator, regulate high pressure homogenizer pump housing pressure 45 embodiments
For better understanding ultimate principle of the present invention, we will specifically set forth principle of the present invention through following examples.Following description, can make the present technique field other people under various situation, use the present invention, deacclimatize the different application of expection with various correction.
Any additional application of explanation that this paper enumerates invention principle all relates to the technology of association area and to the ownership of these open materials, all is considered as included in the scope of claim involved in the present invention.Contents such as the solvent ratio that relates to, filtration medium, micro-filtration precision are to further specific descriptions of the present invention but not limitation of the present invention.
Embodiment 1
The preparation of bletilla striata Crude polysaccharides:
Major equipment: Universalpulverizer, auger tank, high pressure homogenizer, tripod pendulum type batch centrifugal, kieselguhr filter, 500+200nm ceramic membrane filter device, Alcohol-settling tank, vacuum drying oven.
Raw material: bletilla striata medicine materical crude slice 5kg.
The preparation process:
1. pulverizing: the Universalpulverizer with prepackage 1.2mm screen cloth is pulverized bletilla striata medicine materical crude slice, makes all and sieves through No. two, gets bletilla striata meal.
2. mix: bletilla striata meal and 500kg20? Primary reverse osmosis water put altogether in the auger tank, stirred 15 minutes, make to be mixed into bletilla striata suspension.
3. homogenization: bletilla striata suspension input high pressure is pressed clarifixator, regulate high pressure homogenizer pump housing pressure 45~55MPa.
4. centrifugal: high-pressure homogeneous homogenate is centrifugal through tripod pendulum type batch centrifugal, collects centrifugate.
5. filter: in centrifugate, add talcum powder and each 2kg of zeyssatite, mix, when filtrating a few achromaticity and clarification, collect and filtrate through the kieselguhr filter circulating filtration.
6. micro-filtration is concentrated: medium filtrating is filtered to reservation liquid measure 45kg through the micro-filtration strainer of series connection 500nm and 200nm ceramic membrane, gets gluey BSP liquid concentrator.
7. alcohol precipitation: add ethanol in the liquid concentrator, make to contain the alcohol amount and reach 55%, left standstill 6 hours, sedimentation is centrifugal, collects the deposition of white; Deposition is with washing with alcohol 2~3 times, and sedimentation is centrifugal, collecting precipitation.
9. vacuum-drying: be layered in the drip pan the deposition after the washing with alcohol is uniformly thin ,-0.09MPa, be dried to moisture 7% below 65 ℃, pulverize, white BSP 1.6kg.Yield 32%, it is 96% that sulfuric acid-phynol method is measured polysaccharide content.
Below for example clear application of the present invention; Under the prerequisite of aim of the present invention and scope; On some ins and outs, have some modifications, these modifications are for example equipment tissue, technical qualification, implementation step etc., and can not regard as is limitation of the present invention.

Claims (17)

1. the preparation method of a BSP is characterized in that adopting following steps:
(1) cleans: with the inorganic impurities such as silt of extract at room temperature with the most plant material of washing;
(2) pulverize: the bletilla striata is crushed to below the 1.5mm;
(3) mix: in the bletilla striata of pulverizing, add the extraction water of the following temperature of normal temperature, making total amount of water is 20~300 times of bletilla striata medicinal material powder charging capacity, and mixes into uniform suspension;
(4) homogenization: uniform suspension is used the clarifixator homogenization;
(5) sedimentation is centrifugal: through the centrifugal water-insoluble particle of removing of sedimentation;
(6) media filtration: centrifugate is no visual visible particle in media filtration to filtrating;
(7) micro-filtration concentrates: the ceramic membrane filter device with filtering accuracy 2000~100nm carries out tangential flow filtration, and collection needs the micro-filtration of concentration to keep liquid, gets the colloidal liquid BSP;
(8) alcohol precipitation: in gluey BSP, add ethanol, collecting precipitation;
(9) drying: deposition vacuum-drying to the moisture of alcohol precipitation below 8%, is pulverized, the solid BSP;
Wherein the extraction water of the following temperature of normal temperature in the step (3) is meant the primary reverse osmosis water below 30 ℃;
The homogenization of step (4) is meant with high pressure homogenizer and handles bletilla striata powder and the suspension that extracts water, homogenate after the processing is left standstill do not produce tangible deposition in 2 hours; The processing pressure of high pressure homogenizer is between 5~75MPa;
Micro-filtration keeps liquid in the step (7), is meant the trapped fluid of ceramic membrane filter, holds back liquid measure and is equivalent to 2~20 times of bletilla striata medicinal material powder charging capacity.
2. BSP preparation method as claimed in claim 1, it is characterized in that pulverizing is to use the kibbler of the following web plate of prepackage 2mm that the bletilla striata is ground into the powder below the 1.5mm.
3. BSP preparation method as claimed in claim 2 is characterized in that the web plate aperture is 0.5~1.5mm.
4. BSP preparation method as claimed in claim 3 is characterized in that the web plate aperture is 0.8~1.2mm.
5. BSP preparation method as claimed in claim 1 is characterized in that the extraction water of the following temperature of normal temperature being meant 15~30 ℃ primary reverse osmosis water.
6. BSP preparation method as claimed in claim 5 is characterized in that the extraction water of the following temperature of normal temperature being meant 20~25 ℃ primary reverse osmosis water.
7. BSP preparation method as claimed in claim 1, the consumption that it is characterized in that extraction water in the step (3) is 50~200 times of bletilla striata medicinal material powder charging capacity.
8. BSP preparation method as claimed in claim 7, the consumption that it is characterized in that extraction water in the step (3) is 80~120 times of bletilla striata medicinal material powder charging capacity.
9. BSP preparation method as claimed in claim 1, the processing pressure that it is characterized in that high pressure homogenizer is 20~60MPa.
10. BSP preparation method as claimed in claim 9, the processing pressure that it is characterized in that high pressure homogenizer is 45~55Mpa.
11. BSP preparation method as claimed in claim 1; It is characterized in that media filtration; Be meant with sedimentation centrifugate through filtration medium filter that to clarification filtration medium comprises one or more the mixing in filter cloth, filter paper and flocculating aids talcum powder, gac, the zeyssatite.
12. BSP preparation method as claimed in claim 11 is characterized in that filtration medium is the mixture of zeyssatite and talcum powder 1:1.
13. BSP preparation method as claimed in claim 1, the mode that it is characterized in that media filtration are press filtration or vacuum filtration.
14. BSP preparation method as claimed in claim 1, the filtering accuracy that it is characterized in that ceramic membrane is 800nm~100nm.
15. BSP preparation method as claimed in claim 14, the filtering accuracy that it is characterized in that ceramic membrane is 500nm~200nm.
16. BSP preparation method as claimed in claim 1 is characterized in that holding back liquid measure and is equivalent to 5~15 times of bletilla striata medicinal material powder charging capacity.
17. BSP preparation method as claimed in claim 16 is characterized in that holding back liquid measure and is equivalent to 6~10 times of bletilla striata medicinal material powder charging capacity.
CN2009103029373A 2009-06-05 2009-06-05 Process combination for preparing bletilla polysaccharide Active CN101906169B (en)

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Publication number Priority date Publication date Assignee Title
CN102150704B (en) * 2011-01-05 2013-02-13 中山火炬职业技术学院 Fruit and vegetable fresh-keeping agent and preparation method thereof
CN102977220B (en) * 2012-11-20 2015-12-09 安徽大学 Pure physical preparation method of plant and microbial polysaccharide
CN109134685A (en) * 2018-09-30 2019-01-04 广西益谱检测技术有限公司 A method of extracting polysaccharide from beautiful millettia root
CN110642960B (en) * 2019-11-07 2021-12-10 皖西学院 Double-aqueous-phase extraction method of bletilla striata glucomannan
CN111471118A (en) * 2020-05-22 2020-07-31 中山火炬职业技术学院 Preparation method of bletilla striata polysaccharide
CN113278085B (en) * 2021-05-24 2023-01-24 福建宏泰莱生物科技有限公司 Non-ethanol precipitated high molecular weight tremella polysaccharide and preparation method thereof

Citations (3)

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Publication number Priority date Publication date Assignee Title
KR20030091582A (en) * 2002-05-28 2003-12-03 주식회사 바이오랜드 Cosmtic composition containing polysaccharides extracted from Bletilla striata Reichb. fil.
CN1709915A (en) * 2005-06-23 2005-12-21 南京大学医学院附属鼓楼医院 Polysaccharide material for promoting cell tactophily and preparation thereof
CN101429254A (en) * 2008-12-05 2009-05-13 云南植物药业有限公司 Bletilla striata polysaccharide, preparation method and new uses thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030091582A (en) * 2002-05-28 2003-12-03 주식회사 바이오랜드 Cosmtic composition containing polysaccharides extracted from Bletilla striata Reichb. fil.
CN1709915A (en) * 2005-06-23 2005-12-21 南京大学医学院附属鼓楼医院 Polysaccharide material for promoting cell tactophily and preparation thereof
CN101429254A (en) * 2008-12-05 2009-05-13 云南植物药业有限公司 Bletilla striata polysaccharide, preparation method and new uses thereof

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Denomination of invention: Process combination for preparing bletilla polysaccharide

Effective date of registration: 20190920

Granted publication date: 20120523

Pledgee: Bank of China, Limited by Share Ltd, Guangzhou, Panyu branch

Pledgor: Zeli Medicine Tech Co., Ltd., Guangzhou

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Date of cancellation: 20191120

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