CN111533723B - Method for extracting anthocyanin from mature fresh fruit of black fungus - Google Patents
Method for extracting anthocyanin from mature fresh fruit of black fungus Download PDFInfo
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- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
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- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method for extracting anthocyanin from mature fresh fruits of black fungus vegetables, which comprises the following steps: 1) Crushing mature fresh fruit of Auricularia auricula, adding antioxidant, pulping, performing solid-liquid separation, and cooling the separated liquid to obtain extract A; 2) Adding purified water into the solid phase separated in the step 1), homogenizing and grinding, then carrying out solid-liquid separation, and cooling the separated liquid to obtain an extracting solution B; 3) Mixing the extract A and the extract B, adding 95% ethanol, reflux-extracting for 2 times, and concentrating under reduced pressure to obtain extract C; 4) Purifying anthocyanin by macroporous resin chromatography to obtain eluent; 5) Concentrating the eluent obtained in the step 4) under reduced pressure, and freeze-drying to obtain anthocyanin powder. The anthocyanin is prepared from the mature fresh fruit of the agaricus blazei, so that the recycling of the fresh fruit of the agaricus blazei after the use of the agaricus blazei is realized, and the prepared anthocyanin has the advantages of no solvent residue, low cost, no environmental pollution, good taste, high use safety and the like.
Description
Technical Field
The invention belongs to the technical field of extraction and preparation of crop vegetables and fruits, and particularly relates to a method for extracting anthocyanin from mature fresh fruits of black fungus.
Background
The edible fungus vegetable (basella rubra) is a common vegetable in China, belongs to the plant of the genus Abelmoschus of the family Abelmoschus, and is named as the edible fungus, the rouge, the bean curd vegetable, the cabbage and the like because the leaves of the edible fungus vegetable are similar to the edible fungus, are thick and sticky and smooth, and are named as the edible fungus vegetable. The edible fungus is easy to grow, has strong capability of resisting bad environment, is planted in each of the south and north provinces in China, is mainly used as vegetables, and can also be used as medicines. The Chinese medicine shows that the black fungus vegetable has the effects of lubricating intestines, cooling blood, detoxifying, connecting tendons, promoting bones, relieving swelling and the like, is commonly used for treating symptoms such as chest and intestine heat stagnation, urine shortness, diarrhea, hematochezia, burns and scalds, rheumatic arthritis and the like, and modern pharmacological researches show that the black fungus vegetable has pharmacological activities such as antivirus, antioxidation, antibiosis, antiphlogosis and the like, is rich in nutrition, contains various chemical components, and mainly comprises saponin, volatile oil, polysaccharide, various vitamins and the like.
The edible fungus vegetable has high yield and few plant diseases and insect pests, and almost no pesticide is used in the production process, so that the edible fungus vegetable is a good organic vegetable, axillary berries can be obtained in the growth and maturity period of the edible fungus vegetable, and no report about the extraction and application of edible fungus fruits exists at present. Researches show that the fresh fruits are rich in anthocyanin, can be used for producing anthocyanin, has low production cost and wide raw material sources, and the anthocyanin extracted from the black fungus fruits is sweet in taste, has no bad mouthfeel such as sour and astringent taste, and has great economic value and application prospect.
Anthocyanin is also called as anthocyanidin, is a water-soluble natural pigment widely existing in plants in nature, and belongs to flavonoid compounds. The plant petals are main color-developing substances, most of colorful colors of fruits, vegetables, flowers and the like are related to the main color-developing substances, and anthocyanin is used as a natural pigment, so that the plant petals have no toxic or side effect, high safety and natural color tone; the anthocyanin is an effective antioxidant substance, has obvious effects of improving body immunity and scavenging free radicals, can prevent skin aging, strengthen blood circulation, can eliminate eyestrain, delay cerebral nerve aging and the like, has wide application market prospect, generally has the problems of low extraction efficiency, complex operation and high cost in the current market extraction method, has fewer sources of extraction raw materials, such as blueberries, cranberries and the like, has high cost and fewer sources, and has certain limitation on wide application.
The anthocyanin is extracted by utilizing the mature effect of the agaricus blazei, the recycling problem of the fruits of the agaricus blazei can be solved, meanwhile, the quality of the produced anthocyanin is superior to that of the anthocyanin extracted by other ways such as grape skin, blueberries and the like, the production cost of the anthocyanin is reduced, and a new plant source is provided for anthocyanin production.
Disclosure of Invention
The invention aims to provide a method for extracting anthocyanin from mature fresh fruit of black fungus, which solves the problems of insufficient anthocyanin sources and high raw material cost by recycling the mature fresh fruit of the black fungus, and the extracted anthocyanin has good taste and no bitter taste, and is simple in extraction method and suitable for industrial production.
The purpose of the invention is realized in the following way:
A method for extracting anthocyanin from mature fresh fruit of black fungus comprises the following steps:
1) Crushing mature fresh agaric fruits, adding an antioxidant into the crushed fresh agaric fruits to prepare pulp, centrifuging the pulp for 5 to 15 minutes at the rotating speed of 2000 to 4000rpm to perform solid-liquid separation, and then cooling the separated liquid to 10 to 15 ℃ to obtain an extracting solution A;
the antioxidant is one or more of sodium bisulphite, sodium metabisulfite, sodium thiosulfate and vitamin C, and the mass fraction of the antioxidant in the mature fresh fruit of the black fungus vegetable is 0.001-0.05%;
2) Adding 1-3 times of purified water into the solid phase separated in the step 1), grinding the mixture by a refiner to obtain homogenate, centrifuging the homogenate for 5-15 min at the rotating speed of 2000-4000 rpm for solid-liquid separation, and cooling the separated liquid to 10-15 ℃ to obtain extract B;
3) Mixing the extracting solution A and the extracting solution B, adding 95% ethanol until the total concentration of the ethanol is 20-80%, reflux-extracting for 2 times at 60-70 ℃ for 20-40 min each time, and concentrating under reduced pressure to obtain extracting solution C;
4) Purifying anthocyanin by macroporous resin chromatography: activating a chromatographic column, pouring 95% ethanol by volume into the chromatographic column filled with macroporous resin, soaking the macroporous resin for 15-30 min, repeatedly washing the macroporous resin with distilled water until the filtrate becomes transparent, respectively soaking the macroporous resin with 2% hydrochloric acid by volume and 2% sodium hydroxide by volume for 2-5 h, washing the macroporous resin with distilled water until the macroporous resin is neutral, loading the extract C onto the chromatographic column, and eluting anthocyanin with 60% ethanol by mass to obtain eluent after the loading of the extract C onto the chromatographic column is completed;
The macroporous resin is one of XDA-7 and LX-10G, LX-68G, LSA-10 macroporous resin;
5) Concentrating the eluent obtained in the step 4) under reduced pressure, and freeze-drying to obtain anthocyanin powder.
In the step 1), the antioxidant is sodium bisulphite, and the mass fraction of the sodium bisulphite in the mature fresh fruits of the black fungus vegetables is 0.01%.
In the step 1), the solid-liquid separation is carried out by centrifugation for 10min at a rotation speed of 3000rpm, and then the separated liquid is cooled to 12 ℃ to obtain an extract A.
In the step 2), the purified water is added in an amount 3 times the amount of the solid phase separated in the step 1).
In the step 2), the solid-liquid separation is carried out by centrifugation for 10min at a rotating speed of 3000rpm, and then the separated liquid is cooled to 12 ℃ to obtain an extracting solution B.
In the step 3), 95% ethanol is added until the total concentration of the ethanol is 75%, the extraction temperature is 65 ℃, and the extraction time is 30min each time.
In the step 4), the macroporous resin is LX-10G macroporous resin.
In the step 4), ethanol with the volume fraction of 95% is poured into a chromatographic column filled with macroporous resin, and the macroporous resin is soaked for 30min.
In the step 4), hydrochloric acid with the volume fraction of 2% and sodium hydroxide with the volume fraction of 2% are used for soaking the macroporous resin for 2 hours respectively.
In the step 5), the freeze drying temperature is-10 to-70 ℃ and the vacuum degree is 5 to 15Pa.
The invention has the beneficial effects that:
The invention utilizes the mature fresh fruit of the black fungus to extract anthocyanin, can solve the recycling problem of the black fungus, realizes the recycling of the fresh fruit of the black fungus after the use of the black fungus, solves the problems of insufficient anthocyanin sources and high raw material cost, and provides a new plant source for anthocyanin production.
The quality of the anthocyanin extracted by the method is superior to that of the anthocyanin extracted by other ways such as grape skin, blueberries and the like, the extracted anthocyanin has good taste, no bitter taste, the quality of the agaricus auriculata is improved, and the extracted anthocyanin has the advantages of no solvent residue, low cost, no environmental pollution, good taste, high use safety and the like.
The invention utilizes the mature purple fresh fruit of the black fungus to extract anthocyanin, has simple process, is easy for industrial production, and has the advantages of high yield, soft extraction and purification conditions, environment friendliness, simple process, suitability for industrialization and the like.
Detailed Description
The invention is further illustrated below with reference to examples.
The detection method of the anthocyanin content in the embodiments 1-3 is a method for measuring the anthocyanin content in the W/T-2013 annex A.2 of the plant extract cowberry extract.
The starting materials or chemical reagents used in examples 1 to 3 according to the invention, unless otherwise specified, were all obtained by conventional means.
Example 1
A method for extracting anthocyanin from mature fresh fruit of black fungus comprises the following steps:
1) Crushing 2kg of mature fresh agaric fruits, adding sodium bisulphite according to the mass percentage of 0.01% to prepare fruit pulp, centrifuging for 10min at the rotating speed of 3000rpm to perform solid-liquid separation, and cooling the separated liquid to 12 ℃ to obtain 500ml of extracting solution A;
2) Adding 3 times of purified water into the solid phase separated in the step 1), grinding the solid phase into homogenate by a refiner, centrifuging the homogenate for 10min at a rotating speed of 3000rpm, and cooling the separated liquid to 12 ℃ to obtain 3000ml of extract B;
3) Mixing the extract A and the extract B, adding 95% ethanol until the total concentration of ethanol is 75%, reflux-extracting for 2 times at 65deg.C for 30min, and concentrating under reduced pressure to obtain 2000ml extract C;
4) Purifying anthocyanin by macroporous resin chromatography: activating a chromatographic column, pouring 95% ethanol by volume into the chromatographic column filled with LX-10G macroporous resin, soaking the LX-10G macroporous resin for 30min, repeatedly flushing the LX-10G macroporous resin with distilled water until the effluent becomes transparent, respectively soaking the LX-10G macroporous resin for 2h with 2% hydrochloric acid by volume and 2% sodium hydroxide by volume, flushing the extract C to neutrality, loading the extract C onto the chromatographic column, and eluting anthocyanin with 60% ethanol by mass to obtain 1000ml eluent;
5) Concentrating the eluent obtained in the step 4) under reduced pressure, and freeze-drying to obtain 12g of anthocyanin powder.
Through detection, the purity of the anthocyanin in the obtained anthocyanin powder is 21.6%.
Example 2
A method for extracting anthocyanin from mature fresh fruit of black fungus comprises the following steps:
1) Crushing 3kg of mature fresh agaric fruits, adding sodium bisulphite into the crushed fresh agaric fruits according to the mass percentage of 0.01% to prepare fruit pulp, centrifuging the fruit pulp for 10min at the rotating speed of 3000rpm to perform solid-liquid separation, and cooling the separated liquid to 12 ℃ to obtain 700ml of extracting solution A;
2) Adding 3 times of purified water into the solid phase separated in the step 1), grinding the solid phase into homogenate by a refiner, centrifuging the homogenate for 10min at a rotating speed of 3000rpm, and cooling the separated liquid to 12 ℃ to obtain 4000ml of extract B;
3) Mixing the extract A and the extract B, adding 95% ethanol until the total concentration of ethanol is 75%, reflux-extracting for 2 times at 65deg.C for 30min each time, and concentrating under reduced pressure to obtain 3000ml extract C;
4) Purifying anthocyanin by macroporous resin chromatography: activating a chromatographic column, pouring 95% ethanol by volume into the chromatographic column filled with LX-10G macroporous resin, soaking the LX-10G macroporous resin for 30min, repeatedly flushing the LX-10G macroporous resin with distilled water until the effluent becomes transparent, respectively soaking the LX-10G macroporous resin for 2h with 2% hydrochloric acid by volume and 2% sodium hydroxide by volume, flushing the extract C to neutrality, loading the extract C onto the chromatographic column, and eluting anthocyanin with 60% ethanol by mass to obtain 1500ml eluent;
5) Concentrating the eluent obtained in the step 4) under reduced pressure, and freeze-drying to obtain 17g of anthocyanin powder.
Through detection, the purity of the anthocyanin in the obtained anthocyanin powder is 22.3 percent.
Example 3
A method for extracting anthocyanin from mature fresh fruit of black fungus comprises the following steps:
1) Crushing 5kg of mature fresh agaric fruits, adding sodium bisulphite according to the mass percentage of 0.01% to prepare fruit pulp, centrifuging for 10min at the rotating speed of 3000rpm to perform solid-liquid separation, and cooling the separated liquid to 12 ℃ to obtain 1200ml of extracting solution A;
2) Adding 3 times of purified water into the solid phase separated in the step 1), grinding the solid phase into homogenate by a refiner, centrifuging the homogenate for 10min at a rotating speed of 3000rpm, and cooling the separated liquid to 12 ℃ to obtain 5000ml of extract B;
3) Mixing the extract A and the extract B, adding 95% ethanol until the total concentration of ethanol is 75%, reflux-extracting for 2 times at 65deg.C for 30min each time, and concentrating under reduced pressure to obtain 4000ml extract C;
4) Purifying anthocyanin by macroporous resin chromatography: activating a chromatographic column, pouring 95% ethanol by volume into the chromatographic column filled with LX-10G macroporous resin, soaking the macroporous resin for 30min, repeatedly washing the LX-10G macroporous resin with distilled water until the filtrate becomes transparent, respectively soaking the LX-10G macroporous resin with 2% hydrochloric acid by volume and 2% sodium hydroxide by volume for 2h, washing the filtrate with distilled water to be neutral, loading the extract C onto the chromatographic column, and eluting anthocyanin with 60% ethanol by mass fraction to obtain 2400ml eluent;
5) Concentrating the eluent obtained in the step 4) under reduced pressure, and freeze-drying to obtain 27g of anthocyanin powder.
Through detection, the purity of the anthocyanin in the obtained anthocyanin powder is 20.9%.
Claims (6)
1. A method for extracting anthocyanin from mature fresh fruits of black fungus vegetables (basella rubra), which is characterized by comprising the following steps:
1) Crushing mature fresh agaric fruits, adding an antioxidant into the crushed fresh agaric fruits to prepare pulp, centrifuging the pulp for 5 to 15 minutes at a rotating speed of 2000 to 4000rpm to perform solid-liquid separation, and cooling the separated liquid to 10 to 15 ℃ to obtain an extract A;
2) Adding 1-3 times of purified water into the solid phase separated in the step 1), grinding the solid phase by a refiner to obtain homogenate, centrifuging the homogenate for 5-15 min at the rotating speed of 2000-4000 rpm for solid-liquid separation, and cooling the separated liquid to 10-15 ℃ to obtain an extracting solution B;
3) Mixing the extract A and the extract B, adding 95% ethanol until the total concentration of ethanol is 75%, reflux-extracting for 2 times at 65deg.C for 30min, and concentrating under reduced pressure to obtain extract C;
4) Purifying anthocyanin by macroporous resin chromatography:
Activating a chromatographic column, pouring 95% ethanol by volume into the chromatographic column filled with macroporous resin, soaking the macroporous resin for 15-30 min, repeatedly washing the macroporous resin with distilled water until the filtrate becomes transparent, respectively soaking the macroporous resin with 2% hydrochloric acid by volume and 2% sodium hydroxide by volume for 2-5 h, washing with distilled water until the macroporous resin is neutral, loading the extract C into the chromatographic column, and eluting anthocyanin with 60% ethanol by mass after loading to obtain eluent;
5) Concentrating the eluent obtained in the step 4) under reduced pressure, and freeze-drying to obtain anthocyanin powder;
the temperature of freeze drying is-10 to-70 ℃ and the vacuum degree is 5-15 Pa;
In the step 4), the macroporous resin is LX-10G macroporous resin;
In the step 1), the antioxidant is sodium bisulphite, and the mass fraction of the sodium bisulphite in the mature fresh fruits of the black fungus vegetables is 0.01%.
2. The method for extracting anthocyanin from mature fresh fruits of black fungus (basella rubra) according to claim 1, wherein in the step 1), solid-liquid separation is performed by centrifugation for 10min at 3000rpm, and then the separated liquid is cooled to 12 ℃ to obtain extract a.
3. The method for extracting anthocyanin from the mature fresh fruit of agaricus blazei (basella rubra) as claimed in claim 1, wherein the purified water is added in an amount 3 times the amount of the solid phase separated in the step 1) in the step 2).
4. The method for extracting anthocyanin from mature fresh fruits of black fungus (basella rubra) according to claim 1, wherein in the step 2), solid-liquid separation is performed by centrifugation for 10min at 3000rpm, and then the separated liquid is cooled to 12 ℃ to obtain extract B.
5. The method for extracting anthocyanin from mature fresh fruits of black fungus (basella rubra) according to claim 1, wherein in the step 4), 95% ethanol by volume is poured into a chromatographic column filled with macroporous resin, and the macroporous resin is soaked for 30min.
6. The method for extracting anthocyanin from the mature fresh fruit of agaricus blazei (basella rubra) as claimed in claim 1, wherein in the step 4), the macroporous resin is soaked with 2% hydrochloric acid and 2% sodium hydroxide for 2 hours respectively.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914304A (en) * | 2010-07-30 | 2010-12-15 | 合肥工业大学 | Method for extracting blueberry anthocyanin |
| CN103664855A (en) * | 2012-09-20 | 2014-03-26 | 浙江大学苏州工业技术研究院 | Preparation method of high-purity oligomer lotus seedpod procyanidin |
| WO2015032212A1 (en) * | 2013-09-04 | 2015-03-12 | 四川圣湖生物科技有限公司 | Method for extracting chlorogenic acid from green coffee beans |
| CN110272405A (en) * | 2019-07-18 | 2019-09-24 | 长春市紫秘笈文化传播有限公司 | A kind of extracting method of anthocyanidin |
| CN110305097A (en) * | 2019-07-04 | 2019-10-08 | 湖南华诚生物资源股份有限公司 | A method of extracting anthocyanidin from mossberry |
-
2020
- 2020-05-29 CN CN202010478091.5A patent/CN111533723B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914304A (en) * | 2010-07-30 | 2010-12-15 | 合肥工业大学 | Method for extracting blueberry anthocyanin |
| CN103664855A (en) * | 2012-09-20 | 2014-03-26 | 浙江大学苏州工业技术研究院 | Preparation method of high-purity oligomer lotus seedpod procyanidin |
| WO2015032212A1 (en) * | 2013-09-04 | 2015-03-12 | 四川圣湖生物科技有限公司 | Method for extracting chlorogenic acid from green coffee beans |
| CN110305097A (en) * | 2019-07-04 | 2019-10-08 | 湖南华诚生物资源股份有限公司 | A method of extracting anthocyanidin from mossberry |
| CN110272405A (en) * | 2019-07-18 | 2019-09-24 | 长春市紫秘笈文化传播有限公司 | A kind of extracting method of anthocyanidin |
Non-Patent Citations (2)
| Title |
|---|
| 木耳菜果实红色素的提取、纯化、稳定性及其在肉制品中的应用研究;张孔海;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》(第1期);13-27 * |
| 黑布林皮中原花青素提取工艺的优化;龚玉石 等;《食品研究与开发》;第36卷(第20期);47-51 * |
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