CN102140142A - Extraction process for high-purity polysaccharides of tricholoma matsutake - Google Patents
Extraction process for high-purity polysaccharides of tricholoma matsutake Download PDFInfo
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- CN102140142A CN102140142A CN 201110072492 CN201110072492A CN102140142A CN 102140142 A CN102140142 A CN 102140142A CN 201110072492 CN201110072492 CN 201110072492 CN 201110072492 A CN201110072492 A CN 201110072492A CN 102140142 A CN102140142 A CN 102140142A
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Abstract
The invention provides an extraction process for high-purity polysaccharides of tricholoma matsutake, which comprises the extraction steps of cleaning, crushing, degreasing, water leaching, concentrating; obtained polysaccharides of tricholoma matsutake can independently serve as a product, is further processed into products such as capsules, dissolved medicines, tablets and the like, and also can be used as principal components such as functional health foods and medicines. The extraction process combines water lifting and ultrasonic technique, greatly improves the yield of polysaccharides, reduces the production cost, effectively retains the activity of polysaccharides of tricholoma matsutake and simultaneously provides technique assurance for improving economical returns.
Description
Technical field
The present invention relates to the improvement of blazei polysaccharide extraction process, further will be to disclose a kind of high purity blazei polysaccharide extraction process, have economy, characteristics such as efficient, easy, belong to Chinese medicine extracts active ingredients field.
Background technology
Matsutake (Tricholoma Matsutake) has another name called loose bacterium, Song Qin, Trichotoma matsutake.Matsutake belongs to Basidiomycotina, Hymenomycetes, Agaricales, Tricholomataceae, Tricholoma.Matsutake is the geographic endemic species in Asia, mainly is distributed in Japan, the Korea peninsula and China northeast, southwest and Taiwan Province.Matsutake mushroom body plumpness, the pleasant aroma, meat is very delicious, and very high nutritive value and pharmaceutical use are arranged, cancer suppressing ratio up to 90 % about, the people is referred to as " king in the mushroom ".
Blazei polysaccharide exist α-, β-two kind of dextran isomer, wherein beta-glucan is the primary structure unit that cell and tissue form.Dextran has played vital role in energy storage.In recent years, the antitumour activity of beta-glucan, particularly β-1,3 dextran has obtained broad research.Relative, it is fewer that the research of alpha-glucan is in the news, and it prevents hemostasis-coagulation mainly in anti-AIDS, and the reducing blood-fat aspect plays an important role.
Blazei polysaccharide has biologic activity widely, to its deep research and development of carrying out derived product, has vast market prospect.At present, more to the Study on extraction report of blazei polysaccharide.As: adopt combined-enzyme method to extract blazei polysaccharide, but extract yield can only reach 6.5%.Because the restriction of extraction process has greatly influenced the blazei polysaccharide Products Development.
Summary of the invention
The invention provides a kind of high purity blazei polysaccharide extraction process, be a kind of new extraction process, extraction yield is greatly enhanced, and is applicable to suitability for industrialized production.
The extraction process of blazei polysaccharide of the present invention may further comprise the steps:
1), cleans: get 100～500g matsutake and clean, dry to constant weight;
2), pulverize: matsutake is crushed to 60～100 orders;
3), degreasing: add 1L 30%～80% ethanol in the matsutake after pulverizing, soak 1～4h 30～80 ℃ of backflows, perhaps soaked overnight constantly stirs 1000～8000rmp centrifugal collecting precipitation therebetween;
4), 1L water, supersound process 1～3h, 25～65 ℃ of operative temperatures, power 100～600 W will be added in the above-mentioned throw out;
5), flooding step: with the liquid material after the supersound process, carry out boiling water bath lixiviate 1～4h, remove by filter residue and insolubles, get the polysaccharide mother liquor;
6), concentrate: with the polysaccharide mother liquor 30～70 ℃, vacuum tightness-0.03～-0.09MPa under underpressure distillation be concentrated into 1/3～1/10 of original volume;
7), slowly add ethanol in the solution after will concentrating, making the solution alcohol concn is 40～95%, 4 ℃ of standing over night, and the centrifugal 5-30 of 1000～8000rpm minute, after dehydrated alcohol cleaned, vacuum-drying promptly got the matsutake water-soluble polysaccharide.
The blazei polysaccharide that the present invention extracts both can further be processed into product forms such as capsule, electuary, tablet separately as a kind of product, can also be as the main component of functional health care food, medicine.
Positively effect of the present invention is: utilize water to mention that ultrasonic technique combines, greatly improve the polysaccharide yield and reach more than 7.3%, reduced production cost, effectively kept the activity of blazei polysaccharide, technical guarantee is provided for increasing economic efficiency simultaneously.
Description of drawings
Fig. 1 is the blazei polysaccharide infrared spectrogram that the embodiment of the invention 1 is extracted;
Fig. 2 is the blazei polysaccharide infrared spectrogram that the embodiment of the invention 2 is extracted;
Fig. 3 is the blazei polysaccharide infrared spectrogram that the embodiment of the invention 3 is extracted;
Fig. 4 is blazei polysaccharide anti-oxidant activity experiment of the present invention.
Embodiment
For the ease of understanding the present invention, especially exemplified by following examples.Its effect is understood that it is to explaination of the present invention but not to any type of restriction of the present invention.
1), clean: get the 100g matsutake respectively, tap water is cleaned, and removes residual dirt, dries then to constant weight;
2), pulverize: matsutake is crushed to 60 orders;
3), degreasing: add 1L 40% ethanol in the matsutake after pulverizing, soak 2h 40 ℃ of backflows, perhaps soaked overnight constantly stirs the 4000rmp centrifugal collecting precipitation therebetween;
4), above-mentioned materials is added 1L water, supersound process 1h, 30 ℃ of operative temperatures, power 200 W;
5), flooding step: with the liquid material after the supersound process, carry out boiling water bath lixiviate 1h, remove by filter residue and insolubles;
6), concentrate: the polysaccharide mother liquor that boiling water extraction is obtained underpressure distillation under 40 ℃, vacuum tightness-0.06MPa is concentrated into 1/5 of original volume;
7), slowly add ethanol in the solution after will concentrating, making the solution alcohol concn is 60%, 4 ℃ of standing over night, centrifugal 10 minutes of 4000rpm, and after dehydrated alcohol cleaned, vacuum-drying promptly obtained the matsutake water-soluble polysaccharide, and yield is 7.3%;
8), infrared spectra (IR) analysis revealed, 3400,2930 and 1630cm
-1Absorption peak is a polysaccharide characteristic absorption peak (referring to Fig. 1).
1), clean: get the 200g matsutake respectively, tap water is cleaned, and removes residual dirt, dries then to constant weight;
2), pulverize: matsutake is crushed to 80 orders;
3), degreasing: add 1L 60% ethanol in the matsutake after pulverizing, soak 2h 60 ℃ of backflows, perhaps soaked overnight constantly stirs the 4000rmp centrifugal collecting precipitation therebetween;
4), above-mentioned materials is added 1L water, supersound process 1.5h, 45 ℃ of operative temperatures, power 350 W;
5), flooding step: with the liquid material after the supersound process, carry out boiling water bath lixiviate 2h, remove by filter residue and insolubles;
6), concentrate: the polysaccharide mother liquor that boiling water extraction is obtained underpressure distillation under 55 ℃, vacuum tightness-0.06MPa is concentrated into 1/8 of original volume;
7), slowly add ethanol in the solution after will concentrating, making the solution alcohol concn is 80%, 4 ℃ of standing over night, centrifugal 10 minutes of 4000rpm, and after dehydrated alcohol cleaned, vacuum-drying promptly obtained the matsutake water-soluble polysaccharide, and yield is 7.5%;
8), infrared spectra (IR) analysis revealed, 3400,2930 and 1630cm
-1Absorption peak is a polysaccharide characteristic absorption peak (referring to Fig. 2).
Embodiment 3
1), clean: get the 400g matsutake respectively, tap water is cleaned, and removes residual dirt, dries then to constant weight;
2), pulverize: matsutake is crushed to 100 orders;
3), degreasing: add 1L 80% ethanol in the matsutake after pulverizing, soak 2h 80 ℃ of backflows, perhaps soaked overnight constantly stirs the 4000rmp centrifugal collecting precipitation therebetween;
4), above-mentioned materials is added 1L water, supersound process 2h, 60 ℃ of operative temperatures, power 500 W;
5), water logging: with the liquid material after the supersound process, carry out boiling water bath lixiviate 4h, remove by filter residue and insolubles;
6), concentrate: the polysaccharide mother liquor that boiling water extraction is obtained underpressure distillation under 70 ℃, vacuum tightness-0.06MPa is concentrated into 1/10 of original volume;
7), slowly add ethanol in the solution after will concentrating, making the solution alcohol concn is 95%, 4 ℃ of standing over night, centrifugal 10 minutes of 4000rpm, and after dehydrated alcohol cleaned, vacuum-drying promptly obtained the matsutake water-soluble polysaccharide, and yield is 7.6%;
8), infrared spectra (IR) analysis revealed, 3400,2930 and 1630cm
-1Absorption peak is a polysaccharide characteristic absorption peak (referring to Fig. 3).
Test example 1
Blazei polysaccharide is to the mensuration of DPPH radical scavenging activity
Utilize the charateristic avsorption band of DPPH solution,, represent its elimination ability free radical with the decline of absorbance A behind the spectrophotometry adding blazei polysaccharide solution.
The DPPH method: accurately take by weighing DPPH standard substance 25mg, be settled to 500mL with ethanol, it is to be measured that this mother liquor is diluted to several different concentration; Get the polysaccharide testing sample solution 0.2mL of different concns, add 2.8mL DPPH ethanolic soln, mixing immediately, with spectrophotometer in the 515nm place, at certain time intervals in mensuration absorbance A i, up to stable reading.
The absorbancy of sample blank (sample 0.2mL+2.8mL 95% ethanol) is Aj.
DPPH(2.8mL DPPH+0.2mL 95% ethanol of application of sample not) absorbancy is Ac.
Then polysaccharide can be expressed as the clearance rate (SA) of DPPH:
SA（%）=[1-（Ai-Aj）/Ac]×100%。
Anti-oxidant result (DPPH model)
| ? | 0.05 | 0.1 | 0.2 | 0.4 | 1 | 2 | 4 | 8 |
| Blazei polysaccharide a | ? | ? | ? | 6.30% | 17.40% | 28.70% | 41.90% | 68.60% |
| Blazei polysaccharide b | ? | ? | ? | 7.90% | 18.60% | 30.40% | 38.30% | 65.30% |
| Blazei polysaccharide c | ? | ? | ? | 6.50% | 16.10% | 31.70% | 42.50% | 66.40% |
| Xitix | 38.80% | 59.20% | 77.20% | 91.20% | 94.10% | 95.80% | 97.20% | 98.20% |
Claims (1)
1. the extraction process of a high purity blazei polysaccharide may further comprise the steps:
(1), cleans: get 100～500g matsutake and clean, dry to constant weight;
(2), pulverize: matsutake is crushed to 60～100 orders;
(3), degreasing: add 30%～80% ethanol 1L in the matsutake after pulverizing, 1～4h is soaked in 30～80 ℃ of backflows, and perhaps soaked overnight constantly stirs 1000～8000rmp centrifugal collecting precipitation therebetween;
(4), supersound extraction: will add 1L water, supersound process 1～3h, 25～65 ℃ of operative temperatures, power 100～600 W in the above-mentioned throw out;
(5), water logging: with the liquid material after the supersound process, carry out boiling water bath lixiviate 1～4h, remove by filter residue and insolubles, get the polysaccharide mother liquor;
(6), concentrate: with the polysaccharide mother liquor 30～70 ℃, vacuum tightness-0.03～-0.09MPa under underpressure distillation be concentrated into 1/3～1/10 of original volume;
(7), alcohol precipitation: slowly add ethanol in the solution after will concentrating, making the solution alcohol concn is 40～95%, 4 ℃ of standing over night, the centrifugal 5-30 of 1000～8000rpm minute, after dehydrated alcohol cleans, vacuum-drying, promptly.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102885291A (en) * | 2012-11-01 | 2013-01-23 | 黑龙江省麒麟工贸公司 | Tricholoma-matsutake chewing tablet and preparation method thereof |
| CN103040060A (en) * | 2012-11-09 | 2013-04-17 | 吉林博大农林生物科技有限公司 | Matsutake-ginseng drink for assisting in radiation resistance |
| CN103461572A (en) * | 2013-09-18 | 2013-12-25 | 么宏伟 | Tricholoma matsutake instant drink and processing method thereof |
| CN104593441A (en) * | 2014-12-31 | 2015-05-06 | 广东东阳光药业有限公司 | Method for simultaneously extracting volatile oil, polysaccharides and amino acids from tricholoma matsutake |
| CN105273098A (en) * | 2015-11-03 | 2016-01-27 | 广西南宁胜祺安科技开发有限公司 | Method for extracting tricholoma matsutake polysaccharide from tricholoma matsutake |
| CN105646729A (en) * | 2016-03-30 | 2016-06-08 | 聊城大学 | Method for safely and efficiently preparing polysaccharides of tricholoma matsutake |
| CN105732839A (en) * | 2016-05-04 | 2016-07-06 | 聊城大学 | Preparation method of high-activity tricholoma matsutake polysaccharide |
| CN107188987A (en) * | 2017-07-25 | 2017-09-22 | 长江师范学院 | A kind of extracting method of QINGKANGJUN polysaccharide and its application |
| CN109836508A (en) * | 2019-03-05 | 2019-06-04 | 江南大学 | A kind of preparation method and applications of blazei polysaccharide extract |
| JP2022024959A (en) * | 2020-07-16 | 2022-02-09 | オクスロ株式会社 | Bifidobacteria bz25 fermented milk having cholesterol reducing effect |
| CN116102668A (en) * | 2023-04-14 | 2023-05-12 | 广东美宝化妆品有限公司 | Anti-aging and antioxidant polysaccharide extract in tricholoma matsutake, and extraction device and process thereof |
-
2011
- 2011-03-25 CN CN 201110072492 patent/CN102140142B/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
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| 《中兽医医药杂志》 20070610 霍俊凤等 超声波技术优化姬松茸水溶性粗多糖提取工艺的研究 27-28 1 , 第03期 * |
| 《广东药学》 20020630 黄翔宇等 姬松茸菌丝体与子实体多糖的提取及含量的比较 2-4 1 , 第03期 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102885291A (en) * | 2012-11-01 | 2013-01-23 | 黑龙江省麒麟工贸公司 | Tricholoma-matsutake chewing tablet and preparation method thereof |
| CN103040060A (en) * | 2012-11-09 | 2013-04-17 | 吉林博大农林生物科技有限公司 | Matsutake-ginseng drink for assisting in radiation resistance |
| CN103461572A (en) * | 2013-09-18 | 2013-12-25 | 么宏伟 | Tricholoma matsutake instant drink and processing method thereof |
| CN103461572B (en) * | 2013-09-18 | 2014-10-15 | 么宏伟 | Tricholoma matsutake instant drink and processing method thereof |
| CN104593441A (en) * | 2014-12-31 | 2015-05-06 | 广东东阳光药业有限公司 | Method for simultaneously extracting volatile oil, polysaccharides and amino acids from tricholoma matsutake |
| CN105273098A (en) * | 2015-11-03 | 2016-01-27 | 广西南宁胜祺安科技开发有限公司 | Method for extracting tricholoma matsutake polysaccharide from tricholoma matsutake |
| CN105646729A (en) * | 2016-03-30 | 2016-06-08 | 聊城大学 | Method for safely and efficiently preparing polysaccharides of tricholoma matsutake |
| CN105732839A (en) * | 2016-05-04 | 2016-07-06 | 聊城大学 | Preparation method of high-activity tricholoma matsutake polysaccharide |
| CN107188987A (en) * | 2017-07-25 | 2017-09-22 | 长江师范学院 | A kind of extracting method of QINGKANGJUN polysaccharide and its application |
| CN109836508A (en) * | 2019-03-05 | 2019-06-04 | 江南大学 | A kind of preparation method and applications of blazei polysaccharide extract |
| JP2022024959A (en) * | 2020-07-16 | 2022-02-09 | オクスロ株式会社 | Bifidobacteria bz25 fermented milk having cholesterol reducing effect |
| JP7090144B2 (en) | 2020-07-16 | 2022-06-23 | オクスロ株式会社 | Bifidobacterium BZ25 fermented milk with cholesterol lowering effect |
| CN116102668A (en) * | 2023-04-14 | 2023-05-12 | 广东美宝化妆品有限公司 | Anti-aging and antioxidant polysaccharide extract in tricholoma matsutake, and extraction device and process thereof |
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