阅读说明：本技术 一种油茶果壳提取低聚木糖及原花青素的联产方法 (Co-production method for extracting xylo-oligosaccharide and procyanidine from camellia oleifera shells ) 是由 郝泽金 李彪 管业圣 贾石飞 董初球 朱慧芹 于 2020-12-30 设计创作，主要内容包括：本发明提供一种油茶果壳提取低聚木糖及原花青素的联产方法,该方法以油茶果壳为原料,经过破碎、预浸、蒸汽闪爆、酶解糖化、过滤得滤液和料渣；所得滤液经过膜分离、脱色、脱盐、浓缩得低聚木糖浆,该木糖浆经喷雾干燥得低聚木糖粉；所得料渣经过提取、分离、纯化、浓缩、低温干燥后得原花青素粉。本发明采用蒸汽闪爆技术和生物酶技术从油茶果壳中提取低聚木糖和原花青素,提高了油茶果壳的附加值,既高效又环保；同时首次实现了油茶果壳低聚木糖和原花青素两种高价值物质的联产,提取率分别达到7％和4％以上,提高了其经济效益。(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.)

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.

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.