CN112522341A - Co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells - Google Patents
Co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells Download PDFInfo
- Publication number
- CN112522341A CN112522341A CN202011605527.9A CN202011605527A CN112522341A CN 112522341 A CN112522341 A CN 112522341A CN 202011605527 A CN202011605527 A CN 202011605527A CN 112522341 A CN112522341 A CN 112522341A
- Authority
- CN
- China
- Prior art keywords
- procyanidine
- steam
- oligosaccharide
- xylo
- extracting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 title claims abstract description 58
- 241000526900 Camellia oleifera Species 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 238000004880 explosion Methods 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 25
- 239000006188 syrup Substances 0.000 claims abstract description 25
- 235000020357 syrup Nutrition 0.000 claims abstract description 25
- 102000004190 Enzymes Human genes 0.000 claims abstract description 19
- 108090000790 Enzymes Proteins 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000012528 membrane Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000011033 desalting Methods 0.000 claims abstract description 8
- 238000001694 spray drying Methods 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 235000013399 edible fruits Nutrition 0.000 claims description 32
- 241001122767 Theaceae Species 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 21
- 238000002791 soaking Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- XFZJEEAOWLFHDH-UHFFFAOYSA-N (2R,2'R,3R,3'R,4R)-3,3',4',5,7-Pentahydroxyflavan(48)-3,3',4',5,7-pentahydroxyflavan Natural products C=12OC(C=3C=C(O)C(O)=CC=3)C(O)CC2=C(O)C=C(O)C=1C(C1=C(O)C=C(O)C=C1O1)C(O)C1C1=CC=C(O)C(O)=C1 XFZJEEAOWLFHDH-UHFFFAOYSA-N 0.000 claims description 9
- CWEZAWNPTYBADX-UHFFFAOYSA-N Procyanidin Natural products OC1C(OC2C(O)C(Oc3c2c(O)cc(O)c3C4C(O)C(Oc5cc(O)cc(O)c45)c6ccc(O)c(O)c6)c7ccc(O)c(O)c7)c8c(O)cc(O)cc8OC1c9ccc(O)c(O)c9 CWEZAWNPTYBADX-UHFFFAOYSA-N 0.000 claims description 9
- MOJZMWJRUKIQGL-FWCKPOPSSA-N Procyanidin C2 Natural products O[C@@H]1[C@@H](c2cc(O)c(O)cc2)Oc2c([C@H]3[C@H](O)[C@@H](c4cc(O)c(O)cc4)Oc4c3c(O)cc(O)c4)c(O)cc(O)c2[C@@H]1c1c(O)cc(O)c2c1O[C@@H]([C@H](O)C2)c1cc(O)c(O)cc1 MOJZMWJRUKIQGL-FWCKPOPSSA-N 0.000 claims description 9
- HGVVOUNEGQIPMS-UHFFFAOYSA-N procyanidin Chemical compound O1C2=CC(O)=CC(O)=C2C(O)C(O)C1(C=1C=C(O)C(O)=CC=1)OC1CC2=C(O)C=C(O)C=C2OC1C1=CC=C(O)C(O)=C1 HGVVOUNEGQIPMS-UHFFFAOYSA-N 0.000 claims description 9
- 229920002414 procyanidin Polymers 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 102000004533 Endonucleases Human genes 0.000 claims description 7
- 108010042407 Endonucleases Proteins 0.000 claims description 7
- 238000005422 blasting Methods 0.000 claims description 7
- 230000000415 inactivating effect Effects 0.000 claims description 7
- 229920006395 saturated elastomer Polymers 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 230000009849 deactivation Effects 0.000 claims description 4
- 230000002538 fungal effect Effects 0.000 claims description 4
- 238000004042 decolorization Methods 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- 229920001542 oligosaccharide Polymers 0.000 claims 2
- 238000010612 desalination reaction Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 10
- 235000018597 common camellia Nutrition 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 8
- 238000000605 extraction Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 3
- 241000209507 Camellia Species 0.000 abstract 2
- 240000001548 Camellia japonica Species 0.000 description 10
- 229920002488 Hemicellulose Polymers 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229920005610 lignin Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 229920001221 xylan Polymers 0.000 description 1
- 150000004823 xylans Chemical class 0.000 description 1
- 239000009270 zilongjin Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation 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
Landscapes
- Organic Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention provides a co-production method for extracting xylo-oligosaccharide and procyanidine from oil-tea camellia shells, which takes the oil-tea camellia shells as raw materials and obtains filtrate and material residues through crushing, presoaking, steam flash explosion, enzymolysis saccharification and filtering; separating the filtrate with membrane, decolorizing, desalting, concentrating to obtain xylooligosaccharide syrup, and spray drying to obtain xylooligosaccharide powder; extracting, separating, purifying, concentrating and drying the obtained material residue at low temperature to obtain procyanidine powder. The xylo-oligosaccharide and the procyanidine are extracted from the camellia oleifera shells by adopting a steam flash explosion technology and a biological enzyme technology, so that the added value of the camellia oleifera shells is improved, and the method is efficient and environment-friendly; simultaneously, the coproduction of two high-value substances of xylo-oligosaccharide and procyanidine of the camellia oleifera shells is realized for the first time, the extraction rates respectively reach more than 7 percent and 4 percent, and the economic benefit is improved.
Description
Technical Field
The invention relates to the technical field of resource utilization of agricultural and forestry wastes, in particular to a co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells.
Background
The camellia oleifera shells are byproducts of processing camellia oleifera fruit into camellia oleifera abel, and generally account for 50% -60% of the whole fresh camellia oleifera abel fruit. The camellia oleifera shells contain rich cellulose, hemicellulose, lignin, procyanidine and other substances, wherein the content of procyanidine is 4%, the content of cellulose is 15%, the content of hemicellulose is 25% and the content of lignin is 30%, wherein the hemicellulose is mainly xylan and is an ideal raw material for preparing xylo-oligosaccharide. The kernels of the oil tea are used for processing into the oil tea, and the shells are usually discarded or burned as waste, so that not only is the resource seriously wasted, but also the solid waste pollution is increased. The method for extracting the xylo-oligosaccharide by direct soaking is not few, but the method for simultaneously extracting the xylo-oligosaccharide and the procyanidine by a steam flash explosion technology and a biological enzyme technology is not reported.
Steam explosion technology has been widely used in feed production, and as a bioconversion technology, the method can effectively destroy the inner and outer layer structures of any material and endow the material with new properties.
The camellia oleifera shells are used as raw materials to prepare the functional xylo-oligosaccharide and the procyanidine, so that agricultural product resources can be comprehensively utilized, the income of farmers can be increased, the environmental pollution is reduced, and the method has a good market prospect.
Disclosure of Invention
The invention aims to provide a co-production method for extracting xylo-oligosaccharide and procyanidine from oil-tea camellia shells.
The invention is realized by the following technical scheme: a co-production method for extracting xylooligosaccharide and procyanidin from oil tea fruit shell comprises crushing oil tea fruit shell, pre-soaking, steam flashing, enzymolysis saccharifying, and filtering to obtain filtrate and residue; membrane separating the filtrate, decolorizing, desalting, concentrating to obtain xylooligosaccharide syrup, and spray drying to obtain xylooligosaccharide powder; extracting the above residue, separating, purifying, concentrating, and drying at low temperature to obtain procyanidin.
Further, the oil tea shells are crushed to 10-20 meshes.
Furthermore, the pre-soaking solution in the scheme is 0.2% dilute hydrochloric acid, the pre-soaking condition is that the material-liquid ratio is 1:8-15(W/W), and the pre-soaking time is 6-12 h.
Furthermore, the steam pressure of the steam flash explosion in the scheme is 1.8-2.5Mpa, and the pressure maintaining time is 2-4 min.
Furthermore, the amount of the added endonuclease is 3-5% in the enzymolysis saccharification, the enzymolysis temperature is 48-62 ℃, the time is 5-7h, the enzyme deactivation temperature is 100 ℃, and the enzyme deactivation time is 18-30 min.
Further, the scheme comprises the following specific steps:
s1, crushing camellia oleifera fruit shell to 10-20 meshes of granularity;
s2, adding 0.2% dilute hydrochloric acid into the oil tea fruit shell obtained in the step S1, wherein the material-liquid ratio is 1: 10(W/W), soaking for 8h, and fishing out dry residues;
s3, placing the oil tea fruit shell pre-soaked in the step S2 in a blasting cavity of steam explosion equipment, opening an air inlet valve, introducing saturated steam, keeping the steam pressure at 2Mpa, and maintaining the pressure for 3min to complete steam explosion to obtain steam explosion oil tea fruit shell;
s4, adding water into the steam exploded oil tea fruit shell obtained in the step S3, fully and uniformly mixing, adjusting the pH value to 6.0, adding 4% fungal incision enzyme, keeping the temperature of 50 ℃ for enzymolysis for 6 hours, after the enzymolysis reaction is finished, inactivating the enzyme at the temperature of 100 ℃ for 20 minutes, and then separating enzymolysis liquid and material residues;
s5, performing membrane separation, decoloring, desalting and concentrating on the enzymolysis liquid obtained in the step S4 to obtain xylooligosaccharide syrup, and continuously performing spray drying on the xylooligosaccharide syrup to obtain xylooligosaccharide powder;
s6, extracting, separating, purifying, concentrating and drying the material residue obtained in the step S4 at low temperature to obtain procyanidine powder.
The invention also provides xylo-oligosaccharide obtained by the co-production method, wherein the xylo-oligosaccharide is 70 type low-sugar wood syrup.
The invention also provides the procyanidine powder obtained by the co-production method.
The invention has the beneficial effects that: according to the invention, xylo-oligosaccharide and procyanidine are extracted from the waste oil tea fruit shells by adopting a steam flash explosion technology and a biological enzyme technology, so that the added value of the oil tea fruit shells is improved, and the method is efficient and environment-friendly; simultaneously, the coproduction of two high-value substances of xylo-oligosaccharide and procyanidine of the camellia oleifera shells is realized for the first time, the extraction rates respectively reach more than 7 percent and 4 percent, and the economic benefit is improved.
Drawings
FIG. 1 is a process flow diagram of the practice of the present invention.
Detailed Description
The invention is further explained with reference to the drawings and the embodiments.
The endonuclease used by the invention is provided by a Jinan Bailong organism; the content detection method of 70-type xylooligosaccharide syrup adopts high performance liquid chromatography; the procyanidin concentration detection method adopts a sulfuric acid-vanillin colorimetric method. The 70-type xylo-oligosaccharide syrup is 70-type syrup with physicochemical indexes meeting the national standard of GB/T35545-2017 xylo-oligosaccharide.
Example 1
The embodiment provides a co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells, as shown in fig. 1, the co-production method comprises the following steps:
s1, crushing 10kg of oil tea fruit shell to 10-mesh granularity for later use;
s2, adding 100kg of 0.2% dilute hydrochloric acid water, soaking for 8 hours, and fishing out dry residues for later use;
s3, placing the pre-soaked oil-tea camellia shells in a blasting cavity of steam explosion equipment, opening an air inlet valve, introducing saturated steam, keeping the steam pressure at 2Mpa for 3min, and completing steam explosion to obtain steam-exploded oil-tea camellia shells for later use;
s4, adding 160kg of water into 20kg of steam exploded oil tea camellia shells obtained in S3, fully and uniformly mixing, adjusting the pH value to 6.0, then adding 600g of endonuclease, and keeping the temperature of 50 ℃ for enzymolysis for 6 hours. After the enzymolysis reaction is finished, inactivating enzyme for 20min at the temperature of 100 ℃, and then separating enzymolysis liquid and material residues for later use.
And S5, performing membrane separation, decoloring, desalting and concentrating on the enzymolysis liquid obtained in the step S4 to obtain 70-type xylo-oligosaccharide syrup. Wherein the membrane separation adopts a 50nm ceramic membrane and an ultrafiltration membrane for filtration; the decolorization is carried out for one time, and the adding amount of the active carbon is 30 percent of the solid content; no. 3 resin is adopted for desalting, and the dosage of the resin is 500 g; concentrating the feed liquid in vacuum to 40%, and spraying sugar powder in a spray dryer; and then concentrated by a central circulating tube evaporator, and the product is 70 type xylo-oligosaccharide syrup after the solid content reaches 70 percent.
S6, extracting, separating, purifying, concentrating and drying the material residue obtained in the step S4 at low temperature to obtain procyanidine powder. Comprises extracting with 70% acetone at 50 deg.C for 60min, repeating for 2 times, and vacuum filtering; separating and purifying with AB-8 type macroporous adsorbent resin, eluting with 70% ethanol solution, vacuum concentrating the liquid until no flowing solution is seen, and drying at low temperature to obtain procyanidin powder.
As a result: 0.72kg of type 70 xylo-oligosaccharide syrup and 0.43kg of procyanidin powder with purity of 88.6% were obtained.
Example 2
The embodiment provides a co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells, as shown in fig. 1, the co-production method comprises the following steps:
s1, crushing 20kg of oil tea fruit shells to 15-mesh granularity for later use;
s2, adding 160kg of 0.2% dilute hydrochloric acid water, soaking for 7 hours, and fishing out dry residues for later use;
s3, placing the pre-soaked oil-tea camellia shells in a blasting cavity of steam explosion equipment, opening an air inlet valve, introducing saturated steam, keeping the steam pressure at 2.5Mpa for 3.5min, and completing steam explosion to obtain steam explosion oil-tea camellia shells for later use;
s4, adding 40kg of steam exploded oil tea camellia shells obtained in S3 into 300kg of water, fully mixing uniformly, adjusting the pH value to 6.0, then adding 1000g of endonuclease, and keeping the temperature of 55 ℃ for enzymolysis for 6.5 h. After the enzymolysis reaction is finished, inactivating enzyme for 25min at the temperature of 100 ℃, and then separating enzymolysis liquid and material residues for later use.
S5, refer to example 1.
S6, refer to example 1.
As a result: 1.4kg of type 70 xylo-oligosaccharide syrup and 0.82kg of procyanidin powder with purity of 86.9% were obtained.
Example 3
The embodiment provides a co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells, as shown in fig. 1, the co-production method comprises the following steps:
s1, crushing 30kg of oil tea fruit shell to 18-mesh granularity for later use;
s2, adding 360kg of 0.2% dilute hydrochloric acid water, soaking for 10 hours, and fishing out dry residues for later use;
s3, placing the pre-soaked oil-tea camellia shells in a blasting cavity of steam explosion equipment, opening an air inlet valve, introducing saturated steam, keeping the steam pressure at 2.2Mpa for 4min, and completing steam explosion to obtain steam explosion oil-tea camellia shells for later use;
s4, adding 400kg of water into 60kg of steam exploded oil tea camellia shells obtained in S3, fully and uniformly mixing, adjusting the pH value to 6.0, then adding 1500g of endonuclease, and keeping the temperature of 60 ℃ for enzymolysis for 7 h. After the enzymolysis reaction is finished, enzyme is deactivated for 30min at the temperature of 100 ℃, and then enzymolysis liquid and material residues are separated for later use.
S5, refer to example 1.
S6, refer to example 1.
As a result: 2.2kg of type 70 xylo-oligosaccharide syrup and 1.2kg of procyanidin powder with purity 87.8% were obtained.
Comparative example 1
The method for extracting xylo-oligosaccharide and procyanidine in the comparative example is as follows:
s1, crushing 10kg of oil tea fruit shell to 10-mesh granularity for later use;
s2, adding 100kg of 0.2% dilute hydrochloric acid water, soaking for 8 hours, and fishing out dry residues for later use;
s3, adding 160kg of water into the dry residue obtained in the step S2, fully and uniformly mixing, adjusting the pH value to 6.0, then adding 600g of endonuclease, and keeping the temperature of 50 ℃ for enzymolysis for 6 hours. After the enzymolysis reaction is finished, inactivating enzyme for 20min at the temperature of 100 ℃, and then separating enzymolysis liquid and material residues for later use.
S4, refer to example 1.
S5, refer to example 1.
As a result: 0.5kg of type 70 xylo-oligosaccharide syrup and 0.2kg of procyanidin powder with purity of 68.7% were obtained.
Table 1 extraction ratio of each example
From table 1, it can be seen that the extraction rate of the 70-type xylo-oligosaccharide syrup extracted by the scheme of the invention is up to more than 7%, the extraction rate of the procyanidine powder is up to more than 4%, the purity of the procyanidine powder is more than 86%, and the extraction rates of the 70-type xylo-oligosaccharide syrup and the procyanidine powder are relatively low because the steam flash explosion technology and the enzymolysis technology are not combined in the comparative example.
Finally, it should be emphasized that the above-described preferred embodiments of the present invention are merely examples of implementations, rather than limitations, and that many variations and modifications of the invention are possible to those skilled in the art, without departing from the spirit and scope of the invention.
Claims (10)
1. A co-production method for extracting xylo-oligosaccharide and procyanidine from oil tea fruit shells is characterized in that the oil tea fruit shells are used as raw materials, and filtrate and material residues are obtained through crushing, presoaking, steam flash explosion, enzymolysis saccharification and filtering;
membrane separation, decolorization, desalination and concentration are carried out on the filtrate to obtain xylooligosaccharide syrup, and xylooligosaccharide powder is obtained by spray drying of the xylooligosaccharide syrup;
and extracting, separating, purifying, concentrating and drying the material residues at low temperature to obtain procyanidine powder.
2. The co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells according to claim 1, wherein the camellia oleifera shells are crushed to a particle size of 10-20 meshes.
3. The co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells as claimed in claim 1, wherein the pre-soaking solution is 0.2% dilute hydrochloric acid, the pre-soaking condition is that the material-liquid ratio is 1:8-15(W/W), and the pre-soaking time is 6-12 h.
4. The co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells according to claim 1, wherein steam pressure of steam flash explosion is 1.8-2.5Mpa, and pressure holding time is 2-4 min.
5. The co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells as claimed in claim 1, wherein the amount of endonuclease added in the enzymolysis saccharification is 3-5%, the enzymolysis temperature is 48-62 ℃, the time is 5-7h, the enzyme deactivation temperature is 100 ℃, and the enzyme deactivation time is 18-30 min.
6. The co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells as claimed in claims 1 to 5, which is characterized by comprising the following specific steps:
s1, crushing camellia oleifera fruit shell to 10-mesh granularity;
s2, adding 0.2% dilute hydrochloric acid into the oil tea fruit shell obtained in the step S1, wherein the material-liquid ratio is 1: 10(W/W), soaking for 8h, and fishing out dry residues;
s3, placing the oil tea fruit shell pre-soaked in the step S2 in a blasting cavity of steam explosion equipment, opening an air inlet valve, introducing saturated steam, keeping the steam pressure at 2Mpa, and maintaining the pressure for 3min to complete steam explosion to obtain steam explosion oil tea fruit shell;
s4, adding water into the steam exploded oil tea fruit shell obtained in the step S3, fully and uniformly mixing, adjusting the pH value to 6.0, adding 4% fungal incision enzyme, keeping the temperature of 50 ℃ for enzymolysis for 6 hours, after the enzymolysis reaction is finished, inactivating the enzyme at the temperature of 100 ℃ for 20 minutes, and then separating enzymolysis liquid and material residues;
s5, performing membrane separation, decoloring, desalting and concentrating on the enzymolysis liquid obtained in the step S4 to obtain xylooligosaccharide syrup, and performing spray drying on the xylooligosaccharide syrup to obtain xylooligosaccharide powder;
s6, extracting, separating, purifying, concentrating and drying the material residue obtained in the step S4 at low temperature to obtain procyanidine powder.
7. The co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells as claimed in claims 1 to 5, which is characterized by comprising the following specific steps:
s1, crushing camellia oleifera fruit shell to 15-mesh granularity;
s2, adding 0.2% dilute hydrochloric acid into the oil tea fruit shell obtained in the step S1, wherein the material-liquid ratio is 1: 8(W/W), soaking for 7h, and fishing out dry residues;
s3, placing the oil tea fruit shell pre-soaked in the step S2 in a blasting cavity of steam explosion equipment, opening an air inlet valve, introducing saturated steam, keeping the steam pressure at 2.5Mpa, and maintaining the pressure for 3.5min to complete steam explosion to obtain the steam exploded oil tea fruit shell;
s4, adding water into the steam exploded oil tea fruit shell obtained in the step S3, fully and uniformly mixing, adjusting the pH value to 6.0, adding 4% fungal incision enzyme, carrying out enzymolysis for 6.5 hours at 55 ℃, inactivating the enzyme for 25min at 100 ℃ after the enzymolysis reaction is finished, and then separating enzymolysis liquid and material residues;
s5, performing membrane separation, decoloring, desalting and concentrating on the enzymolysis liquid obtained in the step S4 to obtain xylooligosaccharide syrup, and performing spray drying on the xylooligosaccharide syrup to obtain xylooligosaccharide powder;
s6, extracting, separating, purifying, concentrating and drying the material residue obtained in the step S4 at low temperature to obtain procyanidine powder.
8. The co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells as claimed in claims 1 to 5, which is characterized by comprising the following specific steps:
s1, crushing camellia oleifera fruit shell to 18-mesh granularity;
s2, adding 0.2% dilute hydrochloric acid into the oil tea fruit shell obtained in the step S1, wherein the material-liquid ratio is 1: 12(W/W), soaking for 10h, and fishing out dry residues;
s3, placing the oil tea fruit shell pre-soaked in the step S2 in a blasting cavity of steam explosion equipment, opening an air inlet valve, introducing saturated steam, keeping the steam pressure at 2.2Mpa, and maintaining the pressure for 4min to complete steam explosion to obtain steam explosion oil tea fruit shell;
s4, adding water into the steam exploded oil tea fruit shell obtained in the step S3, fully and uniformly mixing, adjusting the pH value to 6.0, adding 4% fungal incision enzyme, performing enzymolysis for 7 hours at the temperature of 60 ℃, inactivating the enzyme for 30 minutes at the temperature of 100 ℃ after the enzymolysis reaction is finished, and then separating enzymolysis liquid and material residues;
s5, performing membrane separation, decoloring, desalting and concentrating on the enzymolysis liquid obtained in the step S4 to obtain xylooligosaccharide syrup, and performing spray drying on the xylooligosaccharide syrup to obtain xylooligosaccharide powder;
s6, extracting, separating, purifying, concentrating and drying the material residue obtained in the step S4 at low temperature to obtain procyanidine powder.
9. Xylo-oligosaccharides obtainable by the co-production process according to any one of claims 1 to 8, characterized in that said xylo-oligosaccharides are type 70 low sugar wood syrups.
10. A procyanidin powder obtained by the co-production process of any one of claims 1 to 8.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011605527.9A CN112522341A (en) | 2020-12-30 | 2020-12-30 | Co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011605527.9A CN112522341A (en) | 2020-12-30 | 2020-12-30 | Co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells |
Publications (1)
Publication Number | Publication Date |
---|---|
CN112522341A true CN112522341A (en) | 2021-03-19 |
Family
ID=74977465
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202011605527.9A Pending CN112522341A (en) | 2020-12-30 | 2020-12-30 | Co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112522341A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112877482A (en) * | 2020-12-30 | 2021-06-01 | 江西神州通油茶科技有限公司 | Method for extracting xylooligosaccharide from camellia oleifera shells |
Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102210786A (en) * | 2011-06-08 | 2011-10-12 | 中国林业科学研究院林产化学工业研究所 | Method for extracting natural antioxidant from shells of camellia oleifera |
CN104072468A (en) * | 2013-03-26 | 2014-10-01 | 宜春元博山茶油科技农业开发有限公司 | Proanthocyanidin extraction process from camellia seed hull |
CN104083534A (en) * | 2014-07-21 | 2014-10-08 | 湖南农业大学 | Method for preparing procyanidine of camellia seed shell |
CN104447941A (en) * | 2014-12-19 | 2015-03-25 | 江西省科学院应用化学研究所 | Method for simultaneous extraction of oligomeric proanthocyanidins and tea saponin from camellia oleifera shells |
CN104591173A (en) * | 2015-01-24 | 2015-05-06 | 南昌航空大学 | Method for preparing graphene by reducing graphene oxide based on camellia oleifera extract |
CN105639397A (en) * | 2016-01-04 | 2016-06-08 | 江西省科学院应用化学研究所 | Natural mixed bacteriostatic agent and preparation method thereof |
US20170042783A1 (en) * | 2014-05-15 | 2017-02-16 | Nissan Chemical Industries, Ltd. | Thickened composition containing lipid peptide-type compound |
CN108997294A (en) * | 2018-08-28 | 2018-12-14 | 湖南大三湘茶油股份有限公司 | High-quality glucosidase procyanidins and preparation method thereof |
CN110616237A (en) * | 2019-10-22 | 2019-12-27 | 天津科技大学 | Method for preparing xylo-oligosaccharide from steam-exploded plant fiber raw material |
CN111470505A (en) * | 2020-03-02 | 2020-07-31 | 北京林业大学 | Co-production method of camellia oleifera xylo-oligosaccharide, lignin and active carbon |
-
2020
- 2020-12-30 CN CN202011605527.9A patent/CN112522341A/en active Pending
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102210786A (en) * | 2011-06-08 | 2011-10-12 | 中国林业科学研究院林产化学工业研究所 | Method for extracting natural antioxidant from shells of camellia oleifera |
CN104072468A (en) * | 2013-03-26 | 2014-10-01 | 宜春元博山茶油科技农业开发有限公司 | Proanthocyanidin extraction process from camellia seed hull |
US20170042783A1 (en) * | 2014-05-15 | 2017-02-16 | Nissan Chemical Industries, Ltd. | Thickened composition containing lipid peptide-type compound |
CN104083534A (en) * | 2014-07-21 | 2014-10-08 | 湖南农业大学 | Method for preparing procyanidine of camellia seed shell |
CN104447941A (en) * | 2014-12-19 | 2015-03-25 | 江西省科学院应用化学研究所 | Method for simultaneous extraction of oligomeric proanthocyanidins and tea saponin from camellia oleifera shells |
CN104591173A (en) * | 2015-01-24 | 2015-05-06 | 南昌航空大学 | Method for preparing graphene by reducing graphene oxide based on camellia oleifera extract |
CN105639397A (en) * | 2016-01-04 | 2016-06-08 | 江西省科学院应用化学研究所 | Natural mixed bacteriostatic agent and preparation method thereof |
CN108997294A (en) * | 2018-08-28 | 2018-12-14 | 湖南大三湘茶油股份有限公司 | High-quality glucosidase procyanidins and preparation method thereof |
CN110616237A (en) * | 2019-10-22 | 2019-12-27 | 天津科技大学 | Method for preparing xylo-oligosaccharide from steam-exploded plant fiber raw material |
CN111470505A (en) * | 2020-03-02 | 2020-07-31 | 北京林业大学 | Co-production method of camellia oleifera xylo-oligosaccharide, lignin and active carbon |
Non-Patent Citations (2)
Title |
---|
尤新主编: "《功能性低聚糖生产与应用》", 31 January 2004, 中国轻工业出版社 * |
张立钊等: "酶法处理油茶籽壳制备低聚木糖工艺的优化", 《食品工业》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112877482A (en) * | 2020-12-30 | 2021-06-01 | 江西神州通油茶科技有限公司 | Method for extracting xylooligosaccharide from camellia oleifera shells |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN100497647C (en) | Method for adsorbing and decomposing stalk cellulose using cellulase | |
CN102162199B (en) | Method for extracting lignin from raw grass | |
CN104099431A (en) | Method for extracting xylose from viscoce chemical fiber squeezed alkali liquor | |
CN108251472B (en) | Preparation method of xylo-oligosaccharide | |
CN111004827B (en) | Preparation method of xylo-oligosaccharide | |
CN106191328A (en) | A kind of xylose production process | |
CN110171818B (en) | Method for extracting graphene from corn straws | |
CN109826044B (en) | Method for separating cellulose, hemicellulose and lignin from cotton stalk | |
CN111019011B (en) | Method for extracting rice bran polysaccharide | |
CN108993424B (en) | Preparation and regeneration method of porous lignin adsorbent | |
CN106519066A (en) | Method for production of dietary fiber and combined production of pectin by utilizing fruit branches and fruit peels (residues) | |
CN105754015A (en) | Method for extracting chitin from oyster shell | |
CN108179646A (en) | With the method for plant fiber material production xylose, high-boiling alcohol lignin and fiber | |
WO2019196165A1 (en) | Method for continuously separating lignocellulose component | |
CN111269171A (en) | Preparation method of high-purity 1-deoxynojirimycin | |
CN112522341A (en) | Co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells | |
CN109136293B (en) | Rape straw recycling full-utilization method | |
CN105463040A (en) | Method for raising yield of xylooligosaccharide | |
CN100432095C (en) | Waste-water-free production method for diosgenin | |
CN102925516A (en) | Xylo-oligosaccharide preparation method | |
CN110669035A (en) | Method for preparing anthocyanin from indigo fruit | |
CN107495392A (en) | The preparation method and corn dietary fiber of a kind of corn dietary fiber | |
CN116375030B (en) | Method for preparing high-quality activated carbon from waste residue generated in production of secondary ethanol | |
CN112877482A (en) | Method for extracting xylooligosaccharide from camellia oleifera shells | |
CN103819514B (en) | Cotton dregs dephenolize technology and utilize this technology to prepare the method for raffinose from cotton dregs |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210319 |