阅读说明：本技术 一种温和抗炎的茶皂素提取物及其应用 (Mild anti-inflammatory tea saponin extract and application thereof ) 是由 王孔江 辛亮 王颖 毛勇进 于 2021-06-19 设计创作，主要内容包括：本发明涉及植物提取技术领域,尤其涉及一种温和抗炎的茶皂素提取物及其应用。所述茶皂素提取物提取自植物榨油后的废弃渣饼；所述植物包括油茶,向日葵,橄榄,花生,油菜,玉米,核桃,芝麻,亚麻,山茶,棕榈,粟米中的至少一种。本发明提供的茶皂素提取物具有以下优点：提取自植物榨油后的废弃渣饼,实现了我国大规模农业废料的有效回收利用,提取方法简便,提取过程未使用有机溶剂即可实现高纯度、高收率的目标产物,且控制工艺条件和混凝剂、吸附剂的选择优化了目标产物的综合性能,产物的稳定性、抑菌性能优异；能够以吨为量级提炼茶皂素,为大规模茶皂素提取提供了可行性。(The invention relates to the technical field of plant extraction, and particularly relates to a mild anti-inflammatory tea saponin extract and application thereof. The tea saponin extract is extracted from waste residue cakes after oil pressing of plants; the plant comprises at least one of Camellia oleifera, sunflower, olive, peanut, rape, corn, walnut, sesame, flax, camellia, palm and millet. The tea saponin extract provided by the invention has the following advantages: the waste residue cake after oil pressing from plants is extracted, so that the effective recycling of large-scale agricultural waste in China is realized, the extraction method is simple and convenient, the target product with high purity and high yield can be realized without using an organic solvent in the extraction process, the comprehensive performance of the target product is optimized by controlling the process conditions and selecting a coagulant and an adsorbent, and the product has excellent stability and antibacterial performance; the tea saponin can be extracted by taking ton as magnitude, and feasibility is provided for large-scale extraction of the tea saponin.)

1. A mild anti-inflammatory tea saponin extract is extracted from waste residue cake after oil extraction from plant; the plant is characterized by comprising at least one of camellia oleifera, sunflower, olive, peanut, rape, corn, walnut, sesame, flax, camellia, palm and millet.

2. The mild anti-inflammatory tea saponin extract as claimed in claim 1, wherein the specific extraction method is:

the first step is as follows: collecting waste residue cake after oil pressing, adding solvent, mixing and homogenizing, stirring, filtering, and separating filtrate and residue;

the second step is that: adding a coagulant into the filtrate, uniformly stirring, adding an adsorbent, uniformly stirring, and filtering to obtain a coarse material I;

the third step: adding a decoloring agent into the coarse material I, uniformly stirring, and filtering to obtain a coarse material II;

the fourth step: and refining and removing impurities from the coarse material II to obtain a finished product.

3. The mild anti-inflammatory tea saponin extract as claimed in claim 2, wherein the first step is specifically, collecting waste residue cake after oil tea oil extraction, drying until the water content is less than or equal to 6, adding solvent, homogenizing with colloid mill, stirring at 60-75 deg.C for 1-3h, filtering with 50-300 mesh, and separating filtrate and residue.

4. The mild anti-inflammatory tea saponin extract as claimed in claim 3, wherein the solvent is a waste cake primary solution, specifically, the waste cake is mixed with water, stirred for 1-3h at 60-75 ℃, filtered, the residue is collected and added with water again, the temperature is kept and stirred for 1-3h, filtered, and the filtrate is collected, namely, the waste cake primary solution.

5. The mild anti-inflammatory tea saponin extract as claimed in any one of claims 2 to 4 wherein said coagulant comprises at least 2 of polyacrylamide, polyaluminium chloride, polyaluminium sulphate, polyaluminium chloride, polyferric sulphate, polyquaternium.

6. The mild anti-inflammatory tea saponin extract as claimed in any one of claims 2-5 wherein said adsorbent comprises at least one of silica gel, alumina, molecular sieves, calcium silicate, wheat germ powder, diatomaceous earth, bentonite, bone char, chitosan, kaolin, talc.

7. The mild anti-inflammatory tea saponin extract as claimed in claim 6 wherein the particle size of the adsorbent is 20-270 μm.

8. The mild anti-inflammatory tea saponin extract as claimed in any one of claims 2 to 7 wherein the depigmenting agent is metal hydroxide, acid salt and mineral acid; the weight ratio of the metal hydroxide, the acid salt and the inorganic acid is (3-160): (0.1-2): (3-10).

9. The mild anti-inflammatory tea saponin extract as claimed in claim 8, wherein the third step is specifically that the metal hydroxide and the acid salt are mixed, added to the crude material for decolorization, then added with phosphoric acid, stirred uniformly and filtered to obtain crude material two.

10. The use of the mild anti-inflammatory tea saponin extract according to any one of claims 1 to 9 wherein the tea saponin extract is used in the fields of daily chemicals, pesticides, farming and medicine.

Technical Field

The invention relates to the technical field of plant extraction, and particularly relates to a mild anti-inflammatory tea saponin extract and application thereof.

Background

Natural surfactants are natural substances with surface activity and derivatives thereof, compared with synthetic surfactants, the natural surfactants have the advantages of high biodegradability, low toxicity and irritation and unique property, and the natural surfactants are gradually favored by the daily chemical market along with the increasingly remarkable harm of the synthetic surfactants to the environment and human bodies. The natural surfactant is mainly derived from animals and plants, and is mostly high molecular organic matters with complex structures, such as lanolin, proteins, saccharides, lecithin, cholesterol, saponins and the like; the saponin has physiological properties of antibiosis, sedation, foamability and the like, and is a popular choice of natural surfactants in the existing daily chemical products. However, the production technology of the existing natural surfactant is not mature, the utilization rate of the natural substances by the traditional extraction method is still at a low level, and the large-scale requirement of daily chemical products on the natural surfactant cannot be met.

China is the country with the largest oil tea cultivation area and the highest yield, the scale of planting oil tea in China currently reaches 6-7 million mu, the amount of produced oil tea seeds exceeds 263 million tons, and the amount of produced camellia oil reaches 64.3 million tons; about 2 million tons of oil camellia oleifera cake are thus produced. At present, the camellia oleifera abel cake is mainly used as a pond cleaning agent, a fertilizer and a fuel, more than 100 million tons of camellia oleifera abel cake is abandoned in white every year, and the economic development and utilization value of the camellia oleifera abel cake is very low; the existing data show that the oil tea seed cake contains rich nutrient substances such as tea saponin and the like, and is limited by the problems of laggard industrialized extraction technology, high extraction cost and the like, the tea saponin in the oil tea seed cake is not fully utilized, and the market development potential is huge.

Based on the above, a natural surfactant which is green and environment-friendly, high in feasibility and excellent in comprehensive performance is researched, so that the natural surfactant can replace a chemical synthesis surfactant and is applied to daily chemical products in a large scale, and the problem to be solved in the field is formed.

Disclosure of Invention

The invention provides the mild anti-inflammatory tea saponin extract, solves the problems of low utilization rate and large resource waste of oil tea cake in the prior art, and realizes the tea saponin extract which is green, environment-friendly, high in feasibility and excellent in antibacterial stability.

The invention provides a mild anti-inflammatory tea saponin extract, wherein the tea saponin extract is extracted from waste residue cakes obtained after vegetable oil pressing; the plant comprises at least one of Camellia oleifera, sunflower, olive, peanut, rape, corn, walnut, sesame, flax, camellia, palm and millet.

In a preferred embodiment, the specific extraction method is as follows:

the first step is as follows: collecting waste residue cake after oil pressing, adding solvent, mixing and homogenizing, stirring, filtering, and separating filtrate and residue;

the second step is that: adding a coagulant into the filtrate, uniformly stirring, adding an adsorbent, uniformly stirring, and filtering to obtain a coarse material I;

the third step: adding a decoloring agent into the coarse material I, uniformly stirring, and filtering to obtain a coarse material II;

the fourth step: and refining and removing impurities from the coarse material II to obtain a finished product.

In a preferred embodiment, the first step is specifically that the waste residue cake after oil tea camellia oil extraction is collected, dried until the water content is less than or equal to 6%, a solvent is added, a colloid mill is used for homogenizing, the mixture is stirred for 1-3 hours at the temperature of 60-75 ℃, and is filtered by a 50-300 mesh sieve, and filtrate and filter residue are separated.

In a preferred embodiment, the solvent is a waste residue cake primary solution, specifically, the waste residue cake is mixed with water, stirred for 1-3h at 60-75 ℃, filtered, the filter residue is collected and added with water again, the mixture is stirred for 1-3h under heat preservation, and filtered, and the collected filtrate is the waste residue cake primary solution.

In a preferred embodiment, the coagulant comprises at least 2 of polyacrylamide, polyaluminium chloride, polyaluminium sulfate, polyferric chloride, polyferric sulfate and polyquaternium.

In a preferred embodiment, the adsorbent comprises at least one of silica gel, alumina, molecular sieve, calcium silicate, wheat germ powder, diatomaceous earth, bentonite, bone char, chitosan, kaolin, and talc.

In a preferred embodiment, the particle size of the adsorbent is 20 to 270 μm.

In a preferred embodiment, the decolorizing agents are metal hydroxides, acid salts and mineral acids; the weight ratio of the metal hydroxide, the acid salt and the inorganic acid is (3-160): (0.1-2): (3-10).

In a preferred embodiment, the third step is specifically to mix the metal hydroxide and the acid salt, add the mixture into the coarse material for decolorization, add the phosphoric acid, stir the mixture evenly, and filter the mixture to obtain the coarse material two.

The invention provides an application of a mild anti-inflammatory tea saponin extract, and the tea saponin extract is applied to the fields of daily chemical products, pesticides, breeding industry and medicines.

Has the advantages that:

the tea saponin extract provided by the invention has the following advantages:

(1) the tea saponin extract is extracted from waste residue cakes after vegetable oil pressing, so that the effective recycling of large-scale agricultural waste in China is realized, and the great market economic value is exerted under the advantage of environmental protection;

(2) the extraction method of the tea saponin extract is simple and convenient, the high-purity and high-yield target product can be realized without using an organic solvent in the extraction process, the comprehensive performance of the target product is optimized by controlling the process conditions and selecting the coagulant and the adsorbent, and the stability and the bacteriostatic performance of the product are excellent; especially the liquid extract can maintain clear and transparent state for a long time;

(3) the tea saponin extract can be produced in the ton order, provides feasibility for large-scale tea saponin extraction, can powerfully promote the development of daily chemical products, pesticides, breeding industry and medicine field, and has wide application prospect.

Drawings

FIG. 1 example of saponin extract prepared in example 1.

Detailed Description

The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.

The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.

The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.

When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.

The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.

Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.

In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.

"Polymer" means a polymeric compound prepared by polymerizing monomers of the same or different types. The generic term "polymer" embraces the terms "homopolymer", "copolymer", "terpolymer" and "interpolymer". "interpolymer" means a polymer prepared by polymerizing at least two different monomers. The generic term "interpolymer" includes the term "copolymer" (which is generally used to refer to polymers prepared from two different monomers) and the term "terpolymer" (which is generally used to refer to polymers prepared from three different monomers). It also includes polymers made by polymerizing more monomers. "blend" means a polymer formed by two or more polymers being mixed together by physical or chemical means.

In order to solve the above problems, the present invention provides in a first aspect a mild anti-inflammatory tea saponin extract extracted from waste cake after oil pressing from plants; the plant comprises at least one of Camellia oleifera, sunflower, olive, peanut, rape, corn, walnut, sesame, flax, camellia, palm and millet.

Further preferably, the plant is at least one of camellia oleifera, olive and corn.

Still more preferably, the plant is camellia oleifera.

In some preferred embodiments, the tea saponin extract is extracted by a specific extraction method comprising:

the first step is as follows: collecting waste residue cake after oil pressing, adding solvent, mixing and homogenizing, stirring, filtering, and separating filtrate and residue;

the second step is that: adding a coagulant into the filtrate, uniformly stirring, adding an adsorbent, uniformly stirring, and filtering to obtain a coarse material I;

the third step: adding a decoloring agent into the coarse material I, uniformly stirring, and filtering to obtain a coarse material II;

the fourth step: and refining and removing impurities from the coarse material II to obtain a finished product.

In some preferred embodiments, the first step is specifically, collecting the waste residue cake after oil tea camellia oil extraction, drying until the water content is less than or equal to 6%, adding a solvent, homogenizing by using a colloid mill, stirring for 1-3h at the temperature of 60-75 ℃, filtering by a 50-300 mesh sieve, and separating filtrate and filter residue.

In some preferred embodiments, the solvent is a waste residue cake primary solution, specifically, the waste residue cake is mixed with water, stirred for 1-3h at 60-75 ℃, filtered, the filter residue is collected and added with water again, stirred for 1-3h under heat preservation, filtered, and the filtrate is collected, namely the waste residue cake primary solution.

The camellia oleifera is used as a unique woody oil crop in China and is an important source of tea saponin, and waste residue cakes (oil tea cakes) of the camellia oleifera after oil pressing contain up to 15 percent of tea saponin, so that the resource has huge development and utilization value potential. The traditional extraction method of tea saponin in the camellia oleifera mainly comprises a water extraction method and an organic solvent extraction method, and in recent years, supercritical fluid extraction, microwave-assisted extraction and ultrasonic technology are also applied to the extraction process attempt of active ingredients in plants; compared with the traditional process, the updating of equipment obviously improves the yield and purity of the extracted product, but based on the mass storage of the camellia oleifera abel cake in China, the emerging process is difficult to extract the tea saponin in the camellia oleifera abel cake in large scale; the traditional extraction method is simple and convenient in process, but the obtained product is low in purity and poor in stability, and effective development and utilization of resources are difficult to realize. The invention focuses on a green and environment-friendly water extraction process, and further adopts the waste cake primary solution to dissolve and extract the oil-tea camellia dregs, and assists a colloid mill to fully dissolve the tea bran in the solvent, so that the extraction efficiency can be improved. Meanwhile, the process method realizes the recycling of solid waste residues in the extraction process, each extraction provides raw materials for the next operation, the production efficiency of the process is optimized, the cost resources are effectively saved, and the actual production operation is facilitated.

In some preferred embodiments, the coagulant comprises at least 2 of polyacrylamide, polyaluminum chloride, polyaluminum sulfate, polyferric chloride, polyferric sulfate, and polyquaterniums.

Further preferably, the coagulant is polyacrylamide, polyaluminium chloride and polyquaternium.

In some preferred embodiments, the weight ratio of the polyacrylamide, the polyaluminum chloride and the polyquaternium is (1-45): (0.5-50): (3-26).

More preferably, the weight ratio of the polyacrylamide to the polyaluminium chloride to the polyquaternium is (2-30): (1-40): (5-20).

In some preferred embodiments, the adsorbent comprises at least one of silica gel, alumina, molecular sieves, calcium silicate, wheat germ powder, diatomaceous earth, bentonite, bone char, chitosan, kaolin, and talc.

Further preferably, the adsorbent is diatomite, bentonite and bone char.

More preferably, the weight ratio of the diatomite, the porphyry and the bone charcoal is (3-8): (1.5-3): (0.2-2.4).

In some preferred embodiments, the particle size of the adsorbent is 20 to 270 μm.

The polymer coagulant with charge ion activity can effectively adsorb impurity components such as protein, tannin and the like in filtrate after extraction, but the improvement of the impurity adsorption capacity of a polymer molecular chain is accompanied by the increase of solution viscosity, the solid-liquid separation needs longer time after adsorption, and the problems of poor separation effect and product purity reduction are caused by pressurizing and accelerating the separation of coarse materials and impurities. According to the invention, by the research and discovery, the inorganic adsorbent and the organic polymer coagulant are used together, so that the separation of the precipitate in the clarification process can be enhanced, and the treatment efficiency is improved; further, the organic polymer coagulant is added firstly, so that the potential of the organic colloid carrying negative charges in the filtrate is reduced, the organic colloid is separated from a tea saponin composition system, an inorganic adsorbent is further added, and impurity particles are rapidly gathered and deposited in a bridging net catching structure formed by the inorganic adsorbent and the organic coagulant. According to the invention, surprisingly, when the adsorbent is diatomite, porphyry and bone charcoal, the antibacterial performance of the tea saponin composition is improved, and the diatomite, the porphyry and the bone charcoal are supposed to have strong specific adsorption effect on impurities in the filtrate, so that the product purity of the tea saponin composition is effectively improved, the tea saponin extract is more easily adsorbed on the surface of thalli after contacting with microorganisms, the normal physiological function of a cell tissue structure is damaged, the cytoplasm content of bacteria is promoted to be dissolved out, and the antibacterial effect is achieved.

In some preferred embodiments, the weight ratio of the filtrate, coagulant and adsorbent is (2500-: (0.8-10): (50-200).

The invention breaks through the complex process of traditional plant extraction, does not need to add organic solvent, can achieve high-purity products only by water extraction, and can obtain the tea saponin composition with bacteriostasis and strong decontamination capability under the safe and mild process conditions through the processes of extraction, clarification, decoloration and refining. Through a large amount of experimental researches, the intermediate product is filtered by selecting a 50-300 mesh (especially 200 mesh) filter cloth in the extraction and clarification processes, and the weight ratio of the filtrate, the coagulant and the adsorbent is (2500-: (0.8-10): (50-200), the tea saponin extract and impurities show a strong separation trend, non-target compounds in the system are aggregated and separated out under the multiple actions of chemical bonding and intermolecular force, and the obtained tea saponin composition can effectively and fully exert the bacteriostatic and decontamination capabilities.

In some preferred embodiments, the decolorizing agents are metal hydroxides, acid salts, and inorganic acids; the weight ratio of the metal hydroxide, the acid salt and the inorganic acid is (3-160): (0.1-2): (3-10).

In some preferred embodiments, the third step is specifically to mix the metal hydroxide and the acid salt, add the mixture into the first coarse material for decolorization, add the phosphoric acid, stir the mixture uniformly, and filter the mixture to obtain the second coarse material.

Further preferably, the metal hydroxide is calcium hydroxide and sodium hydroxide, and the acid salt is sodium bisulfite.

Further preferably, the inorganic acid is selected from dibasic acid and/or tribasic acid; more preferably, the inorganic acid is a tribasic acid, specifically phosphoric acid.

In some preferred embodiments, the weight ratio of calcium hydroxide, sodium bisulfite and phosphoric acid is (1-5): (2-150): (0.1-2): (2-8).

The existing extraction process of the plant extract is difficult to realize that the color of the product is clear and transparent, the product obtained by conventionally crushing the plant raw material and dissolving the crushed plant raw material in small molecular alcohol is dark brown, and although the antioxidant is added in the extraction process, the product with high color degree can not be obtained, and the subsequent application of the product can be influenced. According to the invention, the calcium hydroxide, the sodium hydroxide and the sodium bisulfite are adopted to act on the crude material after the oil tea cake is extracted and clarified, so that the liquid transparency can be obviously improved, and the combined action of the phosphoric acid and the metal hydroxide is further found to improve the stability of the tea saponin composition and inhibit the defects of discoloration, precipitation and the like easily occurring in the extracting solution under the conditions of long term and high temperature; the reason may be that the addition of the phosphoric acid can form a flocculent cavity cross-linked structure with metal ions, further sweep impurities such as pigments, colloids and the like in the adsorption liquid, and inhibit the impurities in the tea saponin composition from interacting to form precipitates or chromophoric groups in the storage process, so that the storage stability of the tea saponin composition is fundamentally improved, and the product is kept in a clear and transparent state for a long time.

The invention provides an application of a mild anti-inflammatory tea saponin extract, and the tea saponin extract is applied to the fields of daily chemical products, pesticides, breeding industry and medicines.

Further preferably, the tea saponin extract is especially suitable for the field of daily chemical products, and as an example of the daily chemical products, the tea saponin extract comprises but is not limited to a surfactant.

Examples

In order to better understand the above technical solutions, the following detailed descriptions will be provided with reference to specific embodiments. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention. In addition, the raw materials are commercially available and the extraction methods of the extract are all conventional extraction methods, if not otherwise specified.

Example 1.

The embodiment provides a mild anti-inflammatory tea saponin extract, which is extracted from waste cake after oil pressing; the plant is oil tea.

The specific extraction method of the tea saponin extract comprises the following steps:

the first step is as follows: collecting 1000kg of waste residue cake after oil extraction of camellia oleifera, drying until the water content is less than or equal to 6%, adding 3000kg of solvent, homogenizing by using a colloid mill, stirring for 2 hours at 70 ℃, filtering by using a 200-mesh filter cloth, and separating filtrate I and filter residue I;

the second step is that: adding a coagulant into the filtrate I, uniformly stirring at 50 ℃, adding an adsorbent, uniformly stirring at 50 ℃, filtering by using 200-mesh filter cloth, collecting filtrate II and filter residue II, adding water into the filter residue II, stirring for 2 hours at 60 ℃, filtering by using 200-mesh filter cloth again, collecting filtrate III, and combining the filtrate II and the filtrate III to obtain a crude material I; the weight ratio of the filtrate I, coagulant, adsorbent and water is 2800: 4.5: 72: 500.

the third step: mixing 3kg of calcium hydroxide, 80kg of sodium hydroxide and 1kg of sodium bisulfite, adding 3000kg of coarse material I, stirring at 70 ℃ for 2h for decolorization, then adding 7kg of phosphoric acid, stirring uniformly, filtering with 200-mesh filter cloth, collecting filtrate IV and residue IV, adding 1000kg of water into residue IV, stirring at 90 ℃ for 1h, filtering with 200-mesh filter cloth, collecting filtrate V, and combining filtrate IV and filtrate V to obtain coarse material II.

The fourth step: and refining and removing impurities from the coarse material II by using an electrodialysis device, and concentrating an extracting solution by using a plate-type falling film evaporator to obtain a finished product of the tea saponin extract.

The ion exchange membranes of the electrodialysis equipment are 20 pairs, and the membrane area is 288cm²The total area of the equipment is 0.612m²The working voltage is 50V; the evaporation capacity of the plate-type falling-film evaporator is 3000kg/h, and the evaporation area is 60m²)。

The solvent is a waste residue cake primary solution, and specifically comprises the steps of mixing 1000kg of waste residue cake with 2800kg of water, stirring for 2 hours at 70 ℃, filtering, collecting filter residues, adding 2800kg of 70 ℃ hot water, stirring for 2 hours at a heat preservation temperature, filtering with 200-mesh filter cloth, and collecting filtrate, namely the waste residue cake primary solution.

The coagulant is polyacrylamide, polyaluminium chloride and polyquaternary ammonium salt; the weight ratio of polyacrylamide, polyaluminium chloride and polyquaternium is 20: 18: 13.

the ionicity of the polyacrylamide is 40%, and the polyacrylamide is purchased from blue water purification materials, Inc. in Hiroshi; the polyaluminium chloride is purchased from chemical industry Co., Ltd in the Minam, and the polyquaternium is purchased from the Minam remote chemical industry Co., Ltd with the model number of M550.

The adsorbent is diatomite, porphyry and bone charcoal; the weight ratio of the diatomite, the porphyry and the bone charcoal is 6: 1.7: 1.2.

the particle size of the diatomite is 38 mu m, and the diatomite is purchased from a Yuanbo mineral product processing factory in Lingshou county; the particle size of the porphyry is 23 μm, and the porphyry is purchased from Shijiazhuanglin mineral products, Inc.; the bone charcoal is bovine bone charcoal, has a particle size of 45 μm, and is purchased from Feilong bone charcoal Co., Ltd.

Example 2.

The embodiment provides a mild anti-inflammatory tea saponin extract, which is extracted from waste cake after oil pressing; the plant is oil tea.

The specific extraction method of the tea saponin extract comprises the following steps:

the first step is as follows: collecting 1000kg of waste residue cake after oil extraction of camellia oleifera, drying until the water content is less than or equal to 6%, adding 3000kg of solvent, homogenizing by using a colloid mill, stirring for 2 hours at 70 ℃, filtering by using a 200-mesh filter cloth, and separating filtrate I and filter residue I;

the second step is that: adding a coagulant into the filtrate I, uniformly stirring at 50 ℃, adding an adsorbent, uniformly stirring at 50 ℃, filtering by using 200-mesh filter cloth, collecting filtrate II and filter residue II, adding water into the filter residue II, stirring for 2 hours at 60 ℃, filtering by using 200-mesh filter cloth again, collecting filtrate III, and combining the filtrate II and the filtrate III to obtain a crude material I; the weight ratio of the filtrate I, coagulant, adsorbent and water is 2800: 4.5: 72: 500.

the third step: mixing 3kg of calcium hydroxide, 80kg of sodium hydroxide and 1kg of sodium bisulfite, adding 3000kg of coarse material I, stirring at 70 ℃ for 2h for decolorization, then adding 7kg of phosphoric acid, stirring uniformly, filtering with 200-mesh filter cloth, collecting filtrate IV and residue IV, adding 1000kg of water into residue IV, stirring at 90 ℃ for 1h, filtering with 200-mesh filter cloth, collecting filtrate V, and combining filtrate IV and filtrate V to obtain coarse material II;

the fourth step: and refining and removing impurities from the coarse material II by using an electrodialysis device, and concentrating an extracting solution by using a plate-type falling film evaporator to obtain a finished product of the tea saponin extract.

The ion exchange membranes of the electrodialysis equipment are 20 pairs, and the membrane area is 288cm²The total area of the equipment is 0.612m²The working voltage is 50V; the evaporation capacity of the plate-type falling-film evaporator is 3000kg/h, and the evaporation area is 60m²)。

The solvent is a waste residue cake primary solution, and specifically comprises the steps of mixing 1000kg of waste residue cake with 2800kg of water, stirring for 2 hours at 70 ℃, filtering, collecting filter residues, adding 2800kg of 70 ℃ hot water, stirring for 2 hours at a heat preservation temperature, filtering with 200-mesh filter cloth, and collecting filtrate, namely the waste residue cake primary solution.

The coagulant is polyacrylamide, polyaluminium chloride and polyquaternary ammonium salt; the weight ratio of polyacrylamide, polyaluminium chloride and polyquaternium is 20: 18: 13.

the ionicity of the polyacrylamide is 40%, and the polyacrylamide is purchased from blue water purification materials, Inc. in Hiroshi; the polyaluminium chloride is purchased from chemical industry Co., Ltd in the Minam, and the polyquaternium is purchased from the Minam remote chemical industry Co., Ltd with the model number of M550.

The adsorbent is diatomite, porphyry and bone charcoal; the weight ratio of the diatomite, the porphyry and the bone charcoal is 4.5: 1.4: 1.5.

the particle size of the diatomite is 38 mu m, and the diatomite is purchased from a Yuanbo mineral product processing factory in Lingshou county; the particle size of the porphyry is 23 μm, and the porphyry is purchased from Shijiazhuanglin mineral products, Inc.; the bone charcoal is bovine bone charcoal, has a particle size of 45 μm, and is purchased from Feilong bone charcoal Co., Ltd.

Example 3.

The embodiment provides a mild anti-inflammatory tea saponin extract, which is extracted from waste cake after oil pressing; the plant is oil tea.

The specific extraction method of the tea saponin extract comprises the following steps:

the first step is as follows: collecting 1000kg of waste residue cake after oil extraction of camellia oleifera, drying until the water content is less than or equal to 6%, adding 3000kg of solvent, homogenizing by using a colloid mill, stirring for 2 hours at 70 ℃, filtering by using a 200-mesh filter cloth, and separating filtrate I and filter residue I;

the second step is that: adding a coagulant into the filtrate I, uniformly stirring at 50 ℃, adding an adsorbent, uniformly stirring at 50 ℃, filtering by using 200-mesh filter cloth, collecting filtrate II and filter residue II, adding water into the filter residue II, stirring for 2 hours at 60 ℃, filtering by using 200-mesh filter cloth again, collecting filtrate III, and combining the filtrate II and the filtrate III to obtain a crude material I; the weight ratio of the filtrate I, coagulant, adsorbent and water is 2800: 4.5: 72: 500.

the third step: mixing 5kg of calcium hydroxide, 120kg of sodium hydroxide and 1.5kg of sodium bisulfite, adding 3100kg of the crude material I, stirring at 70 ℃ for 2h for decolorization, then adding 8kg of phosphoric acid, stirring uniformly, filtering with 200-mesh filter cloth, collecting filtrate IV and filter residue IV, adding 1000kg of water into the filter residue IV, stirring at 90 ℃ for 1h, filtering with 200-mesh filter cloth, collecting filtrate V, and combining the filtrate IV and the filtrate V to obtain the crude material II;

the fourth step: and refining and removing impurities from the coarse material II by using an electrodialysis device, and concentrating an extracting solution by using a plate-type falling film evaporator to obtain a finished product of the tea saponin extract.

The ion exchange membranes of the electrodialysis equipment are 20 pairs, and the membrane area is 288cm²The total area of the equipment is 0.612m²The working voltage is 50V; the evaporation capacity of the plate-type falling-film evaporator is 3000kg/h, and the evaporation area is 60m²)。

The solvent is a waste residue cake primary solution, and specifically comprises the steps of mixing 1000kg of waste residue cake with 2800kg of water, stirring for 2 hours at 70 ℃, filtering, collecting filter residues, adding 2800kg of 70 ℃ hot water, stirring for 2 hours at a heat preservation temperature, filtering with 200-mesh filter cloth, and collecting filtrate, namely the waste residue cake primary solution.

The coagulant is polyacrylamide, polyaluminium chloride and polyquaternary ammonium salt; the weight ratio of polyacrylamide, polyaluminium chloride and polyquaternium is 20: 18: 13.

the ionicity of the polyacrylamide is 40%, and the polyacrylamide is purchased from blue water purification materials, Inc. in Hiroshi; the polyaluminium chloride is purchased from chemical industry Co., Ltd in the Minam, and the polyquaternium is purchased from the Minam remote chemical industry Co., Ltd with the model number of M550.

The adsorbent is diatomite, porphyry and bone charcoal; the weight ratio of the diatomite, the porphyry and the bone charcoal is 6: 1.7: 1.2.

the particle size of the diatomite is 38 mu m, and the diatomite is purchased from a Yuanbo mineral product processing factory in Lingshou county; the particle size of the porphyry is 23 μm, and the porphyry is purchased from Shijiazhuanglin mineral products, Inc.; the bone charcoal is bovine bone charcoal, has a particle size of 45 μm, and is purchased from Feilong bone charcoal Co., Ltd.

Example 4.

The embodiment provides a mild anti-inflammatory tea saponin extract, and the specific implementation mode is the same as that of embodiment 1; except that the solvent is water.

Example 5.

The embodiment provides a mild anti-inflammatory tea saponin extract, and the specific implementation mode is the same as that of embodiment 1; the difference is that the polyaluminium chloride is replaced by polyferric sulfate, which is purchased from Shandong Haoyao New Material Co.

Example 6.

The embodiment provides a mild anti-inflammatory tea saponin extract, and the specific implementation mode is the same as that of embodiment 1; the difference lies in that the weight ratio of the diatomite, the porphyry and the bone charcoal is 1: 1: 3.

example 7.

The embodiment provides a mild anti-inflammatory tea saponin extract, and the specific implementation mode is the same as that of embodiment 1; except that the diatomaceous earth was replaced with zeolite, which was purchased from a distant mica factory in lingshou county and had a particle size of 38 μm.

Example 8.

The embodiment provides a mild anti-inflammatory tea saponin extract, and the specific implementation mode is the same as that of embodiment 1; the difference is that the ion degree of the polyacrylamide is 20 percent, and the polyacrylamide is purchased from blue water purification materials, Inc. in the department of Credit.

Example 9.

The embodiment provides a mild anti-inflammatory tea saponin extract, and the specific implementation mode is the same as that of embodiment 1; the difference is that the third step is as follows: mixing 45kg of calcium hydroxide and 1kg of sodium bisulfite, adding 3000kg of coarse material I, stirring at 70 ℃ for 2h for decolorization, then adding 7kg of phosphoric acid, stirring uniformly, filtering with 200-mesh filter cloth, collecting filtrate IV and residue IV, adding 1000kg of water into residue IV, stirring at 90 ℃ for 1h, filtering with 200-mesh filter cloth, collecting filtrate V, and combining filtrate IV and filtrate V to obtain coarse material II;

example 10.

The embodiment provides a mild anti-inflammatory tea saponin extract, and the specific implementation mode is the same as that of embodiment 1; the difference lies in that the third step: mixing 3kg of calcium hydroxide, 80kg of sodium hydroxide and 1kg of sodium bisulfite, adding 3000kg of the crude material I, stirring at 70 ℃ for 2h for decolorization, filtering with 200-mesh filter cloth, collecting filtrate IV and residue IV, adding 1000kg of water into the residue IV, stirring at 90 ℃ for 1h, filtering with 200-mesh filter cloth, collecting filtrate V, and combining the filtrate IV and the filtrate V to obtain the crude material II.

Performance test method

1. The purity of the tea saponin extract is as follows:

the purity of saponin in the tea saponin extracts prepared in examples 1-10 (g/g dry matter x 100%) was tested using HPLC.

2. And (3) stability testing:

the tea saponin extracts obtained in examples 1 to 10 were allowed to stand at 50 ℃ for 7 days, 10 parallel samples were set for each set of example samples, the state of the parallel samples was observed after 7 days, the number n of samples showing turbidity or precipitation was recorded, and the stability index k was (10-n)/10 × 100%.

3. And (3) testing the bacteriostatic activity:

preparing the tea saponin extracts prepared in examples 1-10 into 0.1% water solution by bacteriostatic zone determination method, and collecting the water solution with concentration of 1.5 × 10⁸And (3) coating a staphylococcus aureus suspension per mL on a flat plate, placing a round filter paper sheet soaked with a tea saponin extract aqueous solution on the flat plate, carrying out inverted cultivation for 20 hours at 36.5 ℃, taking out, recording the diameter of a bacteriostatic circle, and carrying out parallel determination for 10 times on each sample to obtain an average value. The diameter of the inhibition zone is defined to be more than 20mm, the inhibition is excellent, and the diameter of the inhibition zone is 15-20mm is good antibacterial activity, and the diameter of the antibacterial ring is less than 15 mm.

Performance test data

TABLE 1 Performance test results

Finally, it is pointed out that the foregoing examples are illustrative only, serving to explain some of the characteristics of the process according to the invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.