CN104072627B - A kind of preparation method of Herba Typhonii gigantei polyoses extract - Google Patents

A kind of preparation method of Herba Typhonii gigantei polyoses extract Download PDF

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CN104072627B
CN104072627B CN201410243448.6A CN201410243448A CN104072627B CN 104072627 B CN104072627 B CN 104072627B CN 201410243448 A CN201410243448 A CN 201410243448A CN 104072627 B CN104072627 B CN 104072627B
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herba typhonii
typhonii gigantei
extract
ethanol
preparation
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CN104072627A (en
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宋艳玲
鲍微泽
贾金龙
孙欢
刘晓娟
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Shenyang Hongqi Pharmaceutical Co Ltd
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Shenyang University of Chemical Technology
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Abstract

A kind of preparation method of Herba Typhonii gigantei polyoses extract, the preparation method relating to a kind of polyoses extract, specifically includes following preparation process: adds in dry Herba Typhonii gigantei rhizome powder and carries out enzymolysis under the compound enzyme of 1-10% weight ratio and the water Ultrasonic Conditions of 3-15 weight ratio;Carry out under Ultrasonic Conditions extract sucking filtration;Concentrate again through centrifuge, adopt the ethanol of 70-95% concentration that above-mentioned concentrated solution is stirred mixing, precipitate with ethanol 6-18 hour, be centrifuged 5-20 minute under 3000 revs/min of rotating speeds, collect polysaccharide bottom Centrifuge Cup;Dry, obtain Herba Typhonii gigantei polyoses extract product.Present invention process practicality simple to operate, applies the Herba Typhonii gigantei polysaccharide saving extraction time that this technique is extracted, and extraction ratio is high, and extract has the biological activitys such as significant anti-tyrosine kinase, antioxidation and antitumor.

Description

A kind of preparation method of Herba Typhonii gigantei polyoses extract
Technical field
The preparation method that the present invention relates to a kind of polyoses extract, the preparation method particularly relating to a kind of Herba Typhonii gigantei polyoses extract.
Background technology
Herba Typhonii gigantei (TyphoniumgiganteumEngl.) is Araeceae (Araceae) Typhonium Schott (TyphoniumSchott) plant, is the distinctive kind of plant of China.Herba Typhonii gigantei mainly originates in the ground such as Henan, Sichuan, Shaanxi, and existing all parts of the country are many cultivations also, and the Northeast's yield is high, and price is less expensive." traditional herbal medicine ", " Chinese medicine voluminous dictionary " are recorded, Herba Typhonii gigantei bulb hyoscine, by cold-damp, the expectorant that dispels the wind, spasmolytic, control middle wind-phlegm and stop up, facial hemiparalysis, tetanus, control traumatic injury, lymphoid tuberculosis.Up to now, the research of this kind of plant is still less, it is only limitted to folk prescription among the people and uses, research and application to its effective active composition are also at the development phase.
Polysaccharide is a kind of natural macromolecular material being widely present in animal cell membrane and plant, microorganism wall, is a kind of important bioenergetic resource and constituent material, also participates in the various activities of cell simultaneously.Research shows, many vegetable polysaccharidess have the biological activitys such as immunomodulating, antitumor, blood sugar lowering, radioprotective and slow down aging.
Proving according to data check and applicant experimental study, the Herba Typhonii gigantei polysaccharide extracted from Herba Typhonii gigantei has functions such as significantly improving immunity, antitumor, antioxidation.Herba Typhonii gigantei polysaccharide is pure natural substance, it is possible to prepare into health product or medicine by forms such as food additive, dissolved granule, oral liquid, capsule, drop pill, soft capsules.The paper that applicant is delivered use decoction and alcohol sedimentation technique extracts Herba Typhonii gigantei polysaccharide, the purification process of Sevag method removing protein, but this extracting method to there is extraction time long, the problems such as power consumption is high, active component extract yield is low.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of Herba Typhonii gigantei polyoses extract, the method includes pretreatment, supersound extraction or microwave extraction, concentration, precipitate with ethanol, collection, dry, packaging preservation etc., apply the Herba Typhonii gigantei polysaccharide saving extraction time that this technique is extracted, extraction ratio is high, and extract has the biological activitys such as significant anti-tyrosine kinase, antioxidation and antitumor.
It is an object of the invention to be achieved through the following technical solutions:
A kind of preparation method of Herba Typhonii gigantei polyoses extract, described method utilizes compound enzyme medical material to carry out enzymolysis under ultrasound condition, carry out supersound extraction, concentration, precipitate with ethanol, collection again, dry prepare, and specifically includes following preparation process:
1) adding the compound enzyme of 1-10% weight ratio and the water of 3-15 weight ratio in dry Herba Typhonii gigantei rhizome powder, at 30-90 DEG C, carry out enzymolysis 0.5-5h under the Ultrasonic Conditions of 25KHz-100KHz, enzymolysis terminates post-heating inactivation compound enzyme;
2) carrying out 1-4 time under the Ultrasonic Conditions of 25KHz-100KHz to extract, each 1-5h, united extraction liquid carries out sucking filtration;Again through centrifuge when 2000-4000 rev/min centrifugal 5-20 minute, process thing is carried out solid-liquid separation, after abandoning solid content, supernatant is concentrated;
3) supernatant carries out concentrating under reduced pressure, and the 1/4-1/5 being concentrated into original volume can united extraction liquid;
4) adopt the ethanol of 70-95% concentration that above-mentioned concentrated solution is stirred mixing, precipitate with ethanol 6-18 hour, be centrifuged 5-20 minute under 3000 revs/min of rotating speeds, collect polysaccharide bottom Centrifuge Cup;
5) dry, obtain Herba Typhonii gigantei polyoses extract product.
The preparation method of described a kind of Herba Typhonii gigantei polyoses extract, described compound enzyme is papain, cellulase, pectase, acid protease, at, many phthaleins dextranase and diastatic arbitrarily two or more mixture.
Advantages of the present invention and effect be:
The invention provides a kind of Herba Typhonii gigantei extraction method of polysaccharides safe and environment-friendly, efficient, the method extraction ratio is high, purity is high, ultrasound wave combined-enzyme method is used to extract Herba Typhonii gigantei polysaccharide, the processing step such as including pretreatment, supersound extraction or microwave extraction, concentration, precipitate with ethanol, collection, dry, packaging preservation, this technological operation is simple and practical, apply the Herba Typhonii gigantei polysaccharide saving extraction time that this technique is extracted, extraction ratio is high, and extract has the biological activitys such as significant anti-tyrosine kinase, antioxidation and antitumor.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
In following embodiment, agents useful for same is commercially available prod, below in conjunction with embodiment, invention is described in detail.
Embodiment 1:
Compound enzyme (0.5g papain, 0.5g cellulase and 0.5g amylase) is added in the 50g Herba Typhonii gigantei rhizome powder dried, adds water 200ml, in the supersonic generator of 25KHz, at 30 DEG C, ultrasonic enzymolysis 2h, after enzymolysis terminates, enzyme denaturing 1h at 100 DEG C.Selected frequency is the Ultrasonic Conditions of 100KHz, carries out extracting 2 times to the extraction material of above-mentioned preprocessed mistake, each 1h, united extraction liquid, by centrifuge when 3000 revs/min centrifugal 10 minutes, process thing is carried out solid-liquid separation, after abandoning solid content, supernatant is concentrated;Carry out concentrating under reduced pressure at 60 DEG C to collecting supernatant, be concentrated into the 1/5 of original volume;Above-mentioned concentrated solution is stirred mixing by the ethanol adopting 95% concentration, and concentrated solution precipitate with ethanol, after 12 hours, is centrifuged 10 minutes under 3000 revs/min of rotating speeds, collects polysaccharide bottom Centrifuge Cup;The polysaccharide of collection is put in vacuum drying oven, at 50 DEG C of vacuum dryings;Yield 3.1%, polyoses content 38.9%.
Embodiment 2:
Compound enzyme (1.0g cellulase and 0.5g pectase) is added in the 50g Herba Typhonii gigantei rhizome powder dried, adds water 250ml, in the supersonic generator of 25KHz, at 30 DEG C, ultrasonic enzymolysis 2h, after enzymolysis terminates, enzyme denaturing 1h at 100 DEG C.Selected frequency is the Ultrasonic Conditions of 80KHz, carries out extracting 2 times to the extraction material of above-mentioned preprocessed mistake, each 1h, united extraction liquid, by centrifuge when 3000 revs/min centrifugal 10 minutes, process thing is carried out solid-liquid separation, after abandoning solid content, supernatant is concentrated;Carry out concentrating under reduced pressure at 60 DEG C to collecting supernatant, be concentrated into the 1/4 of original volume;Above-mentioned concentrated solution is stirred mixing by the ethanol adopting 80% concentration, and concentrated solution precipitate with ethanol, after 10 hours, is centrifuged 10 minutes under 3000 revs/min of rotating speeds, collects polysaccharide bottom Centrifuge Cup;The polysaccharide of collection is put in vacuum drying oven, at 50 DEG C of vacuum dryings;Yield 3.5%, polyoses content 32.4%.
Embodiment 3:
Compound enzyme (1.0g cellulase and 0.5g amylase) is added in the 50g Herba Typhonii gigantei rhizome powder dried, adds water 500ml, in the supersonic generator of 25KHz, at 30 DEG C, ultrasonic enzymolysis 4h, after enzymolysis terminates, enzyme denaturing 1h at 100 DEG C.Selected frequency is the Ultrasonic Conditions of 100KHz, carries out extracting 2 times to the extraction material of above-mentioned preprocessed mistake, each 1h, united extraction liquid, by centrifuge when 3000 revs/min centrifugal 10 minutes, process thing is carried out solid-liquid separation, after abandoning solid content, supernatant is concentrated;Carry out concentrating under reduced pressure at 60 DEG C to collecting supernatant, be concentrated into the 1/4 of original volume;Above-mentioned concentrated solution is stirred mixing by the ethanol adopting 90% concentration, and concentrated solution precipitate with ethanol, after 12 hours, is centrifuged 10 minutes under 3000 revs/min of rotating speeds, collects polysaccharide bottom Centrifuge Cup;The polysaccharide of collection is put in vacuum drying oven, at 50 DEG C of vacuum dryings;Yield 3.3%, polyoses content 34.4%.
Embodiment 4:
Compound enzyme (0.5g acid protease and 0.5g many phthaleins dextranase) is added in the 50g Herba Typhonii gigantei rhizome powder dried, adds water 300ml, in the supersonic generator of 25KHz, at 30 DEG C, ultrasonic enzymolysis 1h-4h, after enzymolysis terminates, enzyme denaturing 0.5-1h at 100 DEG C.Selected frequency is the Ultrasonic Conditions of 100KHz, carries out extracting 2 times to the extraction material of above-mentioned preprocessed mistake, each 1h, united extraction liquid, by centrifuge when 3000 revs/min centrifugal 15 minutes, process thing is carried out solid-liquid separation, after abandoning solid content, supernatant is concentrated;Carry out concentrating under reduced pressure at 60 DEG C to collecting supernatant, be concentrated into the 1/4 of original volume;Adopting, above-mentioned concentrated solution is stirred mixing by the ethanol of 75% concentration, and concentrated solution precipitate with ethanol, after 12 hours, is centrifuged 10 minutes under 3000 revs/min of rotating speeds, collects polysaccharide bottom Centrifuge Cup;The polysaccharide of collection is put in vacuum drying oven, at 50 DEG C of vacuum dryings;Yield 3.1%, polyoses content 33.8%.

Claims (2)

1. the preparation method of a Herba Typhonii gigantei polyoses extract, it is characterised in that described method utilizes compound enzyme medical material to carry out enzymolysis under ultrasound condition, carry out supersound extraction, concentration, precipitate with ethanol, collection again, dry prepare, and specifically includes following preparation process:
1) adding the compound enzyme of 1-10% weight ratio and the water of 3-15 weight ratio in dry Herba Typhonii gigantei rhizome powder, at 30-90 DEG C, carry out enzymolysis 0.5-5h under the Ultrasonic Conditions of 25KHz-100KHz, enzymolysis terminates post-heating inactivation compound enzyme;
2) carrying out 1-4 time under the Ultrasonic Conditions of 25KHz-100KHz to extract, each 1-5h, united extraction liquid carries out sucking filtration;Again through centrifuge when 2000-4000 rev/min centrifugal 5-20 minute, process thing is carried out solid-liquid separation, after abandoning solid content, supernatant is concentrated;
3) supernatant carries out concentrating under reduced pressure, is concentrated into the 1/4-1/5 of original volume;
4) adopt the ethanol of 70-95% concentration that above-mentioned concentrated solution is stirred mixing, precipitate with ethanol 6-18 hour, be centrifuged 5-20 minute under 3000 revs/min of rotating speeds, collect polysaccharide bottom Centrifuge Cup;
5) dry, obtain Herba Typhonii gigantei polyoses extract product.
2. the preparation method of a kind of Herba Typhonii gigantei polyoses extract according to claim 1, it is characterized in that, described compound enzyme is papain, cellulase, pectase, acid protease, at, polypeptide dextranase and diastatic arbitrarily two or more mixture.
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CN106606616B (en) * 2015-10-27 2021-01-29 鲁南制药集团股份有限公司 Typhonium giganteum antitumor active part and preparation method and application thereof
CN105669295A (en) * 2015-12-31 2016-06-15 广西扬桂生物科技有限公司 Additive for black fungus liquid culture medium
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CN109400730B (en) * 2017-08-18 2021-08-31 中国科学院上海药物研究所 Lycium barbarum polysaccharide, and preparation method and application thereof
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CN108892733B (en) * 2018-05-25 2021-04-30 兰州大学 Radix hedysari polysaccharide modification method and application of modified radix hedysari polysaccharide

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