CN116326685A - A saccharicterpenin analogue with carrier function, its preparation method and application in feed - Google Patents
A saccharicterpenin analogue with carrier function, its preparation method and application in feed Download PDFInfo
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- CN116326685A CN116326685A CN202310306511.5A CN202310306511A CN116326685A CN 116326685 A CN116326685 A CN 116326685A CN 202310306511 A CN202310306511 A CN 202310306511A CN 116326685 A CN116326685 A CN 116326685A
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- saccharicterpenin
- feed
- extraction
- analog
- vitamin
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23K20/10—Organic substances
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/30—Oligoelements
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/30—Feeding-stuffs specially adapted for particular animals for swines
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/70—Feeding-stuffs specially adapted for particular animals for birds
- A23K50/75—Feeding-stuffs specially adapted for particular animals for birds for poultry
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
- Y02P60/87—Re-use of by-products of food processing for fodder production
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Polymers & Plastics (AREA)
- Animal Husbandry (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Birds (AREA)
- Inorganic Chemistry (AREA)
- Fodder In General (AREA)
Abstract
The invention discloses a saccharicterpenin analogue with a carrier function, a preparation method thereof and application thereof in feed, wherein the preparation method comprises the following steps: 1) Drying and peeling oil tea fruits to obtain oil tea seeds with water content of 3-8%; 2) Shelling the camellia seeds to obtain camellia seed kernels; 3) Crushing camellia seed kernels; 4) Loading the crushed camellia seed kernel into a supercritical fluid extraction kettle for supercritical fluid extraction, wherein the extraction temperature of the supercritical fluid extraction is 30-55 ℃, the extraction pressure is 25-50MPa, and the extraction time is 45-90min; reducing the pressure to normal pressure after the extraction is finished, and obtaining a primary product; 5) Sieving the primary product with 40 mesh sieve, and collecting the undersize to obtain the saccharicterpenin analog with carrier function. The saccharicterpenin analog is white powder, has loose cellular microporous structure, and can be used for preparing feed additive, feed additive carrier, premix feed and complete compound feed, and improving stability of vitamin and trace element complex in feed.
Description
Technical Field
The invention relates to the technical field of animal feeds, in particular to a saccharicterpenin analogue with a carrier function, a preparation method thereof and application thereof in feeds.
Background
The animal feed additives include nutritional feed additives and non-nutritional feed additives, and can be made into compound premix feed by mixing with corresponding carriers and diluents, which plays an important role in satisfying balanced and effective supply of animal nutritional needs and development of feed industry.
The chemical feed additives such as antibiotics are added into the animal feed, so that the animal feed has the effects of preventing and treating diseases and promoting growth, but also has serious defects of easy residue in animal bodies, environmental pollution, drug resistance caused by pathogenic bacteria and the like, and seriously endangers the health and ecological environment of human beings and livestock and poultry. In addition, the carrier without special nutritive value is used in a large proportion in the premix, which may affect the nutrition balance of the ration, and cause the absorption and utilization of partial main nutritional ingredients and nutritional feed additives by animals to be blocked. Thus, there is an urgent need to develop novel feed additives and feed additive carriers in animal feed.
The saccharicterpenin is a natural bioactive substance composed of saccharides, glycoside and organic acid, is a feed additive approved by agricultural rural areas and is listed in the feed additive variety catalogue, has biological effects of replacing antibiotics, improving animal immunity, resisting inflammation, resisting stress, resisting oxidation and the like, and can promote the digestion and absorption of nutrient substances in feed by animals. The natural saccharicterpenin is nontoxic, and can be added into animal feed for long term use.
However, according to the current production method and process, to obtain the saccharicterpenin feed additive meeting the GB/T25247-2010 standard, a series of complicated steps such as organic solvent extraction, drying and the like are required to be carried out on the processing byproducts of the camellia oleifera (mainly camellia seed meal), a large amount of sewage, waste liquid and waste residues are generated, and the organic solvent also has potential safety hazards, for example, the patent application number CN202111429021.1 discloses a high-efficiency extraction method of the saccharicterpenin as an antibacterial growth-promoting agent, which comprises the following steps: degreasing raw materials by petroleum ether, adding 75% methanol as an extracting solution into a constant-temperature water bath kettle according to the feed liquid ratio of the raw materials to the methanol of 1:10 for heating reflux extraction, extracting at 60 ℃ for 2.5 hours, concentrating and evaporating after extraction, extracting the evaporated concentrated solution by adopting n-butanol, concentrating the extracting solution by decompression and evaporation again, recovering the n-butanol, and finally, vacuum drying the concentrated solution to obtain a saccharicterpenin finished product. CN202211233383.8 discloses a method for extracting saccharicterpenin from oil tea cake, comprising the following steps: (1) Crushing and sieving oil tea cakes, mixing the sieved materials with ethanol, and performing squeezing treatment to obtain an extracting solution a and a whey a; (2) Mixing the emulsion a with ethanol for ultrasonic treatment to obtain an extracting solution b; (3) Mixing the extracting solution a and the extracting solution b, cooling to room temperature, adding water, and adjusting the pH value to obtain a mixed solution; (4) Mixing the mixed solution with acid protease, and sequentially performing enzymolysis treatment and enzyme deactivation treatment to obtain an enzymolysis solution; (5) Mixing the enzymolysis liquid with bentonite and bovine serum albumin for clarification treatment to obtain clarified liquid; (6) Concentrating the clear solution under reduced pressure, drying at low temperature, pulverizing, and sieving to obtain saccharicterpenin.
The extraction method of the saccharicterpenin adopts the camellia seed meal as the raw material, the extraction process adopts a plurality of operation methods in the steps of squeezing, solvent leaching, petroleum ether degreasing, evaporation concentration, enzymolysis, vacuum drying and the like, the tedious operation steps are carried out, the extraction time after the pretreatment of the raw material exceeds 2 hours, the preparation efficiency of the saccharicterpenin is greatly reduced, the production cost of the saccharicterpenin is high, the price is high, the use is limited, and particularly the production process has pollution and potential safety hazard to the environment.
In order to further simplify the pretreatment step of obtaining tea seed meal in the preparation process of saccharicterpenin, there are also many researches on directly adopting tea seeds as raw materials to prepare saccharicterpenin, for example, patent application number is CN200810121708.7 which discloses an extraction method of novel feed additive saccharicterpenin, which comprises the following steps: weighing seeds of Theaceae plants, drying, peeling, pulverizing, adding ethanol, heating with microwave, and extracting for three times. And after the extraction is finished, merging the extracting solutions, concentrating the extracting solutions under reduced pressure to recover the solvent, adding water into the solvent to form a suspension, extracting the suspension by using petroleum ether and acetone in sequence, and discarding petroleum ether and acetone extracting solutions. The remaining phase was extracted with n-butanol, and the extract was concentrated under reduced pressure and weighed. The method adopts peeled camellia seeds with shells as raw materials and combines the procedures of solvent extraction, reduced pressure concentration and the like to prepare the saccharicterpenin, the operation steps are complex, and the preparation efficiency of the saccharicterpenin is greatly reduced; and the saccharicterpenin prepared by taking the peeled camellia seeds as raw materials is dark in color and cannot meet the color and luster requirements of feed additives.
For example, patent application number CN201310044570.6 discloses a method for extracting tea oil and saccharicterpenin by using a physical wall breaking auxiliary aqueous enzymatic method, wherein after the tea seeds are shelled, dried and crushed, physical wall breaking treatment is carried out, then a certain proportion of enzyme is added for aqueous enzymatic extraction, enzymatic hydrolysate is centrifugally separated to obtain tea oil and a water layer, and the water layer is concentrated and dried to obtain saccharicterpenin. According to the method, shelled camellia seeds are used as raw materials, and the steps of a water enzyme method and concentration and drying are combined to prepare the saccharicterpenin, so that the operation steps are complicated, and the preparation efficiency of the saccharicterpenin is greatly reduced; the temperature and time during enzymolysis are strictly controlled in the extraction process by adopting the aqueous enzymatic method, so that not only is the strict requirement on the precise control of the process met, but also the enzyme deactivation operation is required at high temperature after the aqueous enzymatic method is adopted, so that Maillard reaction of nutrient substances is easy to occur, the prepared saccharicterpenin is dark in color, and the requirement of a feed additive on the color cannot be met.
In addition, none of the above-mentioned prior art extract saccharicterpenin is related to having carrier function, and it is not known that the saccharicterpenin prepared by the above-mentioned method has the function of being able to exert the carrier of vitamin, trace element complex to improve absorption and stability of various nutrients and reduce loss of nutrients.
Therefore, in view of the above, there is a need to develop a novel saccharicterpenin-like product with carrier function, so as to innovate the production process, reduce the production cost, improve the color and quality of saccharicterpenin, and promote the large-scale and effective utilization of the processing byproducts of oil tea.
Disclosure of Invention
The invention aims to solve the technical problems that: overcomes the defects of the prior art, and provides a saccharicterpenin analogue with simple production process, green and environment-friendly production process, no potential safety hazard of organic solvents, low production cost, better color quality and carrier function, a preparation method thereof and application thereof in feed.
The technical scheme adopted for solving the technical problems is as follows: a method for preparing a saccharicterpenin analogue with a carrier function, which comprises the following steps:
1) Drying and peeling the oil tea fruits to obtain oil tea seeds with the water content of 3-8%;
2) Shelling the camellia seeds to obtain camellia seed kernels;
3) Crushing camellia seed kernels;
4) Loading the crushed camellia seed kernels into a supercritical fluid extraction kettle for supercritical fluid extraction, wherein the extraction temperature of the supercritical fluid extraction is 35-55 ℃, the extraction pressure is 25-50MPa, and the extraction time is 45-90min; reducing the pressure to normal pressure after the extraction is finished, and obtaining a dry and clean primary product as raffinate;
5) Sieving the primary product with 40 mesh sieve, and collecting the undersize to obtain the saccharicterpenin analog with carrier function.
As most of functional substances such as grease, saccharicterpenin and the like exist in the nuts, in the preparation process of the saccharicterpenin analogue, the camellia fruits are firstly peeled and shelled to obtain camellia seed kernels, cellulose, surface dust and heavy metals can be removed by peeling, and non-functional or non-feedable substances such as lignin and anti-nutritional ingredients and the like contained in the shells can be removed by shelling, so that the unification of the internal substances of the product is ensured. Meanwhile, the shelling (the shell accounts for about 40% of the mass of the camellia seeds) is processed, so that under the extraction condition, supercritical fluid and pressure directly act on the seed kernel raw material to ensure that the saccharicterpenin analogue presents the formation of a honeycomb micropore structure. Therefore, the peeling and shelling treatment not only greatly improves the extraction production efficiency and the quality stability of the product, but also ensures the natural nutrition characteristic of the product as the saccharicterpenin analogue.
Extracting crushed camellia seed kernel by supercritical fluid extraction technology at specific extraction temperature, extraction pressure and extraction timeThe oil-tea camellia seed kernel is subjected to oil removal, and the obtained raffinate after the oil-tea camellia seed kernel is subjected to oil removal is the primary product; in the step, the supercritical fluid extraction technology is adopted to remove the grease substances in the camellia seed kernels, and a series of complicated operation steps such as squeezing, leaching, enzymolysis, evaporation concentration, drying and the like in the prior art are not required in the whole process of obtaining the primary product, so that the operation process for removing the grease substances in the camellia seed kernels is greatly simplified, and the cost is reduced; the raw materials in the process are always in a low-temperature environment and are not subjected to high-temperature treatment, so that the phenomena of nutrient loss and Maillard reaction caused by high temperature used in the processes of ordinary squeezing, leaching and enzymolysis enzyme deactivation are avoided, the obtained product is white powder, and the color and quality of the saccharicterpenin analogue are effectively improved. The temperature, pressure and time during supercritical fluid extraction all play an important role in the structure and function of the saccharicterpenin analogs. Under certain temperature and pressure conditions, fluid in supercritical state has fluidity in liquid state and permeability in gas state, and supercritical fluid (CO) 2 ) First, the raw material tissue is penetrated under high pressure, and then, in the process of reducing the pressure to normal pressure, the supercritical fluid (CO 2 ) Can be rapidly released from the tissue, thereby forming a cellular three-dimensional microporous structure. Meanwhile, when the extraction time is less than 45min or the pressure is less than 25MPa, the problems that the grease removal is incomplete and the honeycomb micropore structure cannot be formed are caused; when the extraction time is more than 90min or the pressure is more than 50MPa, the equipment performance requirement is higher, the energy consumption is high, the energy efficiency is high, the preparation cost of the saccharicterpenin analogues is greatly improved, and the preparation efficiency of the saccharicterpenin analogues is reduced. Therefore, the extraction conditions not only ensure the efficient removal of grease and the protection of natural components in raw materials, but also ensure the formation of cellular microporous structures of products, and effectively improve the carrier function of the stability of vitamin and trace element complexes.
Finally, the primary product is sieved by a 40-mesh sieve, so that the camellia seed kernel skin and the camellia seed shells possibly existing can be effectively removed, the unification of the components and the particle sizes of the product is further ensured, the prepared saccharicterpenin analogue has proper dispersibility and fluidity, and the better carrier function can be effectively promoted.
The preparation process of the saccharicterpenin analogue adopts the steps of peeling, shelling, supercritical fluid extraction and screening, has simple preparation process, and can obtain the saccharicterpenin analogue with the carrier function only by taking peeled and shelled camellia seed kernels as raw materials and combining a specific supercritical fluid extraction process and screening by 40 meshes. The saccharicterpenin analogue can be obtained under the combined influence of three processes of a peeling and shelling process, a supercritical fluid extraction process and a sieving particle size of the oil tea fruits, and can not be obtained by lacking or replacing any one process, so that the prepared saccharicterpenin analogue is not only white powder, but also has the characteristic of loose cellular microporous structure, can play the function of a feed additive carrier, can effectively improve the stability of vitamin and trace element complex in feed, avoid the loss of nutrient substances in the feed, and can more effectively and uniformly play the function of the carrier.
Further, the moisture content of the peeled camellia seeds in the step 1) is 4-8%.
Preferably, the particle size of the pulverization in the step 3) is 0.1 to 1.0mm.
Preferably, the extraction temperature of the supercritical fluid extraction in the step 4) is 35-45 ℃, the extraction pressure is 35-45MPa, and the extraction time is 60-90min.
The invention also provides a saccharicterpenin analogue with a carrier function, which is prepared by adopting the preparation method of the saccharicterpenin analogue, wherein the saccharicterpenin analogue is white powder and has a loose cellular micropore structure, and the pore diameter of the micropore is 0.2-1.5 mu m. According to the literature, the average particle size of the vitamin micro-emulsion is less than or equal to 45nm (Cao Jindang, nano-scale vitamin preparation and research and development of production process), the micro-element complex, such as zinc methionine complex, with the particle size of 78.8-396nm (Ms. AllaMarukhllenko et al, comparative Analysis of Physical and Chemical Properties of Differently Obtained Zn-Methionine Chelate with Proved Antibiofilm Properties (Part II), pharmacogics, 2023), is less than or within the pore size range (0.2-1.5 mu m), so that the vitamin and the micro-element complex can enter or be adsorbed into micropores of the product, the dispersion performance of the vitamin and the micro-element complex can be improved, the stability of the vitamin and the micro-element complex can be improved, the loss of the vitamin and the micro-element complex in the preparation of feed can be effectively reduced, and the terpene sugar analogues prepared by the invention have better carrier functions.
The invention also provides application of the saccharicterpenin analogue with the carrier function in feed, the saccharicterpenin analogue is used as a carrier of vitamin and trace element complex, and is used for preparing feed additives and premixed feeds, so that the stability of the vitamin and trace element complex in the feed can be improved, wherein the vitamin comprises vitamin A, vitamin D3, vitamin E, vitamin K3, vitamin B1, vitamin B2, vitamin B6, vitamin B12, nicotinic acid, biotin and the like, and the trace element complex comprises complex of iron (Fe), manganese (Mn), zinc (Zn), copper (Cu) and the like and amino acid.
Further, the feed additive comprises the following components in parts by mass: 25-50 parts of saccharicterpenin analogues, 10-20 parts of compound vitamins and 30-65 parts of trace element complexes.
Preferably, the feed additive comprises the following components in parts by weight: 35 parts of saccharicterpenin analogues, 10 parts of compound vitamins and 55 parts of trace element complexes.
Further, the premixed feed comprises a compound premixed feed, a vitamin premixed feed and a trace element premixed feed, and the compound premixed feed is prepared by adopting the feed additive as a raw material.
The invention also provides an application of the saccharicterpenin analog with the carrier function in feed, and an application of the premixed feed in preparation of complete compound feed.
Further, the complete compound feed is used for feeding laying hens and pigs, and can improve the production performance of the laying hens and the pigs.
The saccharicterpenin analogue with the carrier function, the preparation method thereof and the application in feed have the beneficial effects that:
(1) The preparation process of the saccharicterpenin analogue is simple, the production process is environment-friendly, the preparation method adopts the steps of peeling, shelling, supercritical fluid extraction and screening, the peeled and shelled camellia seed kernel is taken as a raw material, the supercritical fluid extraction technology is combined to extract the grease substances in the camellia seed kernel so as to remove the grease substances in the camellia seed kernel, the physical screening method is directly adopted to directly obtain the product saccharicterpenin analogue, the raw material in the whole preparation process is always in a low-temperature environment, the traditional complex steps of solvent leaching, concentrating and drying, enzymolysis, concentrating and drying and the like are not required in the extraction process, the preparation process of the saccharicterpenin analogue is greatly simplified, the time from raw material (camellia seed) to product (saccharicterpenin analogue) is controlled to be 2-3 h, the extraction time after the pretreatment of the raw material is controlled to be within 45-90min, the preparation time of the saccharicterpenin analogue is greatly shortened, the preparation cost of the saccharicterpenin analogue is reduced, and the preparation efficiency, the product quality and the controllability of the saccharicterpenin analogue are improved;
(2) The saccharicterpenin analogues prepared under the specific process of peeling, shelling, supercritical fluid extraction and screening are white powder, so that the requirements of feed additives on color and luster are met; compared with the national standard GB/T25247-2010, the oil-removed tea total saponins have the main ingredient indexes which are in accordance with or superior to the standard except the oil-removed tea total saponins, and have the function of saccharicterpenin;
(3) The structure of the saccharicterpenin analogue prepared by the invention is fluffy, has a loose cellular microporous structure with the pore diameter of 0.2-1.5 mu m (refer to figure 2) on the microstructure, has the function of a feed additive carrier, can wrap feed additives such as vitamin and trace element complex and the like by the cellular microporous structure with the pore diameter of 0.2-1.5 mu m, reduces the contact area of the vitamin and trace element complex and air, effectively prevents the vitamin and trace element complex from being oxidized and decomposed, and can uniformly disperse raw material substances in the feed additive in the cellular micropores with the pore diameter of 0.2-1.5 mu m, so that the saccharicterpenin analogue can effectively improve the stability of the vitamin and trace element complex in the feed, avoid the loss of the vitamin and trace element complex in the feed, can be used as a carrier of various different kinds of nutrients and can more effectively and uniformly perform the function of the carrier;
(4) The saccharicterpenin analogue prepared by the invention can be used as carriers of vitamin and trace element complexes for preparing feed additives, premixed feeds and complete compound feeds, so that the prepared feed additives, premixed feeds and complete compound feeds contain nutrients such as vitamins and trace elements required by animals, and the contained saccharicterpenin analogue is a natural plant component, not only contains various nutrients, but also can play the function of the carriers, has the effect of replacing antibiotics, can achieve one-material multi-purpose in the premixed feeds and the complete compound feeds, improves the value of products, not only reduces the use amount of nutrient-free functional carriers, but also improves the immunity and the production performance of animals, effectively improves the quality of meat and egg products, and has larger economic benefit and social benefit.
Drawings
FIG. 1-is a comparative diagram of the production flow of a saccharicterpenin-one (ordinary saccharicterpenin) prepared in comparative example 1 and a saccharicterpenin analogue prepared by the method of the present invention;
FIG. 2-is an external and microstructure view of the saccharicterpenin analog prepared in example 1;
FIG. 3-is an external and microscopic structural view of saccharicterpenin I prepared in comparative example 1;
FIG. 4 is a view showing the appearance and microstructure of saccharicterpenin II prepared in comparative example 2;
FIG. 5-is an external and microscopic structural view of saccharicterpenin III prepared in comparative example 3;
FIG. 6-is a view showing the appearance and microstructure of saccharicterpenin IV prepared in comparative example 4;
FIG. 7-is an external and microstructure view of saccharicterpenin five prepared in comparative example 5;
FIG. 8-is an external and microstructure view of saccharicterpenin six prepared in comparative example 6;
FIG. 9-is an external and microstructure view of saccharicterpenin seven prepared in comparative example 7;
FIG. 10-vitamin B in a vitamin premix of the saccharicterpenin analog and saccharicterpenin one to seven pairs at 30d storage 1 Influence of loss rate;
FIG. 11-vitamin B in vitamin premix feed of saccharicterpenin analogs and saccharicterpenin one to seven pairs at 45d storage 1 Influence of loss rate;
FIG. 12-vitamin B in vitamin premix feed of saccharicterpenin analogs and saccharicterpenin one to seven pairs at 60d storage 1 Influence of loss rate;
FIG. 13-effect of saccharicterpenin analogs and saccharicterpenin one to seven on vitamin E loss rate in vitamin premix feed at 30d storage;
FIG. 14-effect of saccharicterpenin analogs and saccharicterpenin one to seven on vitamin E loss rate in vitamin premix feed at 45d of storage;
FIG. 15-effect of saccharicterpenin analogs and saccharicterpenin one to seven on vitamin E loss rate in vitamin premix feed at 60d storage;
FIG. 16-effect of saccharicterpenin analogs and saccharicterpenin one to seven on iron glycinate loss rate in trace element premix feed at 30d storage;
FIG. 17-effect of saccharicterpenin analogs and saccharicterpenin one to seven on iron glycinate loss rate in trace element premix feed at 60d storage;
FIG. 18-effect of saccharicterpenin analogs and saccharicterpenin one to seven on iron glycinate loss rate in trace element premix feed at 120d of storage;
FIG. 19-effect of saccharicterpenin analogs and saccharicterpenin one to seven on zinc methionine loss rate in trace element premix feed at 30d storage;
FIG. 20-effect of saccharicterpenin analogs and saccharicterpenin one to seven on zinc methionine loss rate in trace element premix feed at 60d storage;
FIG. 21-effect of saccharicterpenin analogs and saccharicterpenin one to seven on zinc methionine loss rate in trace element premix feed at 120d of storage;
figure 22-effect of saccharicterpenin prepared in different test groups on laying rate when used in the manufacture of complete compound feed for laying hens.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings, but these embodiments do not limit the scope of the invention in any way.
Example 1
A preparation method of a saccharicterpenin analogue with a carrier function is shown in a process flow chart in figure 1, and comprises the following steps:
1) Drying and peeling the oil tea fruits to obtain oil tea seeds with water content of 5%;
2) The camellia seeds are put into a sheller for shelling, and camellia seed kernels are obtained;
3) Crushing camellia seed kernels, wherein the particle size of the crushed camellia seed kernels is 0.25-1.0mm;
4) Loading crushed camellia seed kernels into a supercritical fluid extraction kettle for supercritical fluid extraction, wherein the extraction medium in the supercritical fluid extraction is supercritical CO 2 The extraction temperature is 40 ℃, the extraction pressure is 35MPa, and the extraction time is 90min; reducing the pressure to normal pressure after the extraction is finished, and obtaining a dry and clean primary product as raffinate;
5) Sieving the primary product with a 40 mesh sieve, and taking the undersize to obtain the saccharicterpenin analog with a carrier function, wherein the saccharicterpenin analog is white powder and has a loose cellular microporous structure, and the pore diameter of the micropores is 0.5-1.4 mu m.
Example 2
A method for preparing a saccharicterpenin analogue with a carrier function, which comprises the following steps:
1) Drying and peeling the oil tea fruits to obtain oil tea seeds with water content of 4%;
2) The camellia seeds are put into a sheller for shelling, and camellia seed kernels are obtained;
3) Crushing camellia seed kernels, wherein the particle size of the crushed camellia seed kernels is 0.2-1.0mm;
4) Loading crushed camellia seed kernels into a supercritical fluid extraction kettle for supercritical fluid extraction, wherein the extraction medium in the supercritical fluid extraction is supercritical CO 2 The extraction temperature is 35 ℃, the extraction pressure is 35MPa, and the extraction time is 60min; reducing the pressure to normal pressure after the extraction is finished, and obtaining a dry and clean primary product as raffinate;
5) Sieving the primary product with a 40 mesh sieve, and taking the undersize to obtain the saccharicterpenin analog with a carrier function, wherein the saccharicterpenin analog is white powder and has a loose cellular microporous structure, and the pore diameter of the micropores is 0.4-1.2 mu m.
Example 3
A method for preparing a saccharicterpenin analogue with a carrier function, which comprises the following steps:
1) Drying and peeling the oil tea fruits to obtain oil tea seeds with the water content of 3%;
2) The camellia seeds are put into a sheller for shelling, and camellia seed kernels are obtained;
3) Crushing camellia seed kernels, wherein the particle size of the crushed camellia seed kernels is 0.1-0.8mm;
4) Loading crushed camellia seed kernels into a supercritical fluid extraction kettle for supercritical fluid extraction, wherein the extraction medium in the supercritical fluid extraction is supercritical CO 2 The extraction temperature is 40 ℃, the extraction pressure is 40MPa, and the extraction time is 90min; reducing the pressure to normal pressure after the extraction is finished, and obtaining a dry and clean primary product as raffinate;
5) Sieving the primary product with a 40 mesh sieve, and taking the undersize to obtain the saccharicterpenin analog with a carrier function, wherein the saccharicterpenin analog is white powder and has a loose cellular microporous structure, and the pore diameter of the micropores is 0.2-1.2 mu m.
The invention refers to national standard GB/T25247-2010 for detecting various technical indexes contained in the saccharicterpenin analogues prepared in examples 1-3 and comparing various indexes with the national standard, and the results are shown in Table 1:
table 1 table of comparison of technical indices of the saccharicterpenin analogs prepared in examples 1-3 corresponding to the national standards
From the above table, it can be seen that, among the ingredient indexes contained in the saccharicterpenin analogues prepared by the methods of examples 1-3, the other main ingredient indexes are all in line with or superior to the national standard GB/T25247-2010 except for the total saponins of tea, and at present, the total saponins of various saccharicterpenins in the market are 15% -20%, and the feeding effect is equivalent to that of 30% of the total saponins. Therefore, the product of the invention is named as a saccharicterpenin analogue and has the function of saccharicterpenin.
Example 4
The application of the saccharicterpenin analog with the carrier function in the feed adopts the saccharicterpenin analog prepared in the embodiment 1 as a carrier of a vitamin and trace element complex to prepare a feed additive, so that the stability of the vitamin and trace element complex in the feed can be improved, and the feed additive comprises the following components in parts by weight: 35 parts of saccharicterpenin analogue, 10 parts of compound vitamin (respectively comprising 0.37 part of vitamin A and 0.37 part of vitamin D) 3 0.15 part, 1.85 parts of tocopheryl acetate, 3.75 parts of nicotinic acid, 1.85 parts of calcium pantothenate and vitamin K 3 0.55 part of vitamin B 2 0.92 part of vitamin B 6 0.55 part of vitamin B 12 0.01 parts), trace element complex (complex of trace element and amino acid) 55 parts (each comprising 6 parts of copper glycinate complex, 20 parts of iron glycinate complex, 14 parts of zinc methionine complex, and 15 parts of manganese methionine complex).
The preparation method of the feed additive comprises the following steps: placing the saccharicterpenin analog into a clean turnover mixer, proportionally adding the complex vitamin and the trace element complex, sealing the mixer, and stirring at normal temperature (20 ℃) for 20r/min for 12min to obtain the feed additive with carrier function and containing the saccharicterpenin analog.
Example 5
The use of a saccharicterpenin analog with carrier function in feed, the feed additive prepared in example 4 was used for preparing premixed feed (specific formula table 8) and complete formula feed (specific formula table 9) of laying hen.
Example 6
The use of the saccharicterpenin analogues with carrier function in feed adopts the feed additive prepared in the example 4 to prepare premixed feed (specific formula table 12) and complete formula feed (specific formula table 13) of pigs, and the specific formula table is experimental example.
Example 7
The application of the saccharicterpenin analog with the carrier function in the feed adopts the saccharicterpenin analog prepared in the example 1 as a carrier of vitamins for preparing vitamin premix feed, and the specific formula is shown in Table 6.
Example 8
The application of the saccharicterpenin analog with the carrier function in the feed adopts the saccharicterpenin analog prepared in the example 1 as a carrier of a trace element complex for preparing trace element premix feed, and the specific formula table is shown in Table 7.
Comparative example 1
The preparation method of the saccharicterpenin adopts a traditional method, and comprises the following specific operation steps:
1) Drying and peeling the oil tea fruits to obtain oil tea seeds with water content of 5%;
2) The camellia seeds are sent into a squeezer for physical squeezing, most of grease is removed, and camellia seed cakes are obtained;
3) Removing grease substances in the camellia seed cake by adopting an organic solvent leaching method: crushing the camellia seed cake, sieving with a 0.5mm sieve, adding No. 6 solvent oil (the main component is alkane compound) according to the solvent-to-material ratio of 4 (V/W), leaching for 45min at 50 ℃, and removing most of grease after solid-liquid separation to obtain camellia seed meal;
4) Treating the camellia seed meal by adopting a solvent countercurrent extraction method, separating and drying, and sieving with a 40-mesh sieve: extracting soluble substances by adopting an organic solvent (75% ethanol) according to a constant temperature dynamic countercurrent extraction ratio of 1:5, extracting at 50 ℃ for 150min, concentrating and evaporating leaching liquor at 80 ℃ by a rotary evaporator after leaching, and vacuum drying or spray drying the evaporated concentrated liquor, and adding zeolite powder to obtain common saccharicterpenin, namely saccharicterpenin I, which is the most common saccharicterpenin in the market at present, and can be directly purchased from Hangzhou Tang-Tian technology Co.
The production flow charts of the saccharicterpenin I prepared by the comparative example and the saccharicterpenin analogue prepared by the method are shown in figure 1, and as can be seen from figure 1, the traditional saccharicterpenin preparation method (namely, comparative example 1) is prepared by adopting peeled camellia seeds as raw materials, squeezing the peeled camellia seeds by a physical squeezing method to obtain camellia seed cakes, and then combining the steps of organic solvent leaching, solvent countercurrent extraction, separation and drying; however, the saccharicterpenin analogue is prepared by taking peeled and dehulled camellia seed kernels as raw materials, extracting the camellia seed kernels by combining a high-pressure low-temperature supercritical fluid extraction technology, and directly screening the raffinate by adopting a physical screening method.
Compared with the traditional preparation method of the saccharicterpenin, the preparation method does not need to use an organic solvent and a drying step, reduces the risk of solvent residue, and simplifies the preparation process; the raw materials do not need to be treated at high temperature, so that the risk of adverse influence of nutrient substances on the color of the product due to Maillard reaction is reduced. The invention adopts peeled and dehulled camellia seed kernels as raw materials and combines a supercritical fluid extraction and physical sieving method to enable the appearance of the finally prepared saccharicterpenin analogue to be white powder (shown in figure 2-A), and the saccharicterpenin analogue is more in accordance with the requirements of feed on color and luster because the saccharicterpenin analogue adopts the camellia seed which is not dehulled as raw materials and combines the processes of solvent extraction, drying and the like, so that the appearance of the prepared product is grey brown (shown in figure 3-A), and the requirements of feed on color and luster cannot be met.
The product of the present invention (the analogue of saccharicterpenin prepared in example 1) differs from saccharicterpenin one not only in color, but also in microstructure (as shown in fig. 2 and 3) and nutrient composition (as shown in table 2) index.
From fig. 2 and 3, it is clear that the product of the present invention is clearly distinguished in microstructure from saccharicterpenin one, which has a loose cellular microporous structure (fig. 2-B), whereas saccharicterpenin one does not have the cellular microporous structure (fig. 3-B). The honeycomb microporous structure enables the saccharicterpenin analogue prepared by the invention to have special physical properties better than that of the saccharicterpenin-feed additive carrier, can effectively improve the stability of vitamin and trace element complex, and reduces the loss of vitamin and trace element complex in feed.
TABLE 2 saccharicterpenin analogs and saccharicterpenin a main nutritional index (air drying basis)
As can be seen from table 2, the contents of moisture (dry matter), crude protein, crude fat, total saponins in the saccharicterpenin analogs were not greatly different from that of saccharicterpenin; crude fiber, tannin, especially crude ash, is lower than saccharicterpenin one, and total sugar content is higher than saccharicterpenin one; it is known that the saccharicterpenin analogs prepared by the invention have better nutritive value than saccharicterpenin.
Comparative example 2
This comparative example differs from comparative example 1 in that: and (2) carrying out shelling treatment before the step (2), and then carrying out subsequent operation steps, wherein the prepared product is named as saccharicterpenin II.
Comparative example 3
The present comparative example used the aqueous enzymatic process to prepare saccharicterpenin, which also used dehulled camellia seed kernels as the starting material, and then prepared by the method of example 1 in CN201310044570.6, and the prepared product was designated as saccharicterpenin three.
Comparative example 4
This comparative example differs from example 1 in that: crushing and subsequent supercritical fluid extraction steps are directly carried out on peeled camellia seeds without shelling, wherein the technological parameters of supercritical fluid extraction and the final screening particle size are the same as those of the embodiment, and the prepared product is named as saccharicterpenin IV.
The process flow for preparing saccharicterpenin in example 1 of the present invention is shown in Table 3 as follows:
TABLE 3 Table 1 shows the differences between the process flows for preparing saccharicterpenin from comparative examples 1-4
| Treatment group | Raw materials | Extraction process |
| Example 1 | Peeled and shelled camellia seed kernel | Supercritical fluid extraction |
| Comparative example 1 | Tea seed with shell | Squeezing and solvent leaching |
| Comparative example 2 | Peeled and shelled camellia seed kernel | Squeezing and solvent leaching |
| Comparative example 3 | Peeled and shelled camellia seed kernel | Aqueous enzymatic process |
| Comparative example 4 | Tea seed with shell | Supercritical fluid extraction |
The first, second, third and fourth saccharicterpenins prepared in comparative examples 1-4 are shown in FIGS. 3-6.
Comparing example 1 with comparative examples 2 and 3, respectively, it was found that the saccharicterpenin analogs prepared by the supercritical fluid extraction process of the present invention exhibited white appearance, had a loose cellular microporous structure on the microstructure (as shown in fig. 2), whereas the saccharicterpenin di-and saccharicterpenin tri-obtained by the extraction methods of the comparative examples 2 and 3, respectively, using the squeezing + solvent extraction and the aqueous enzymatic method, exhibited dark yellow appearance, and had no loose cellular microporous structure on the microstructure (as shown in fig. 4 and 5). The saccharicterpenin analogue prepared by the invention not only has better color and luster than saccharicterpenin II and saccharicterpenin III, but also has a honeycomb micropore structure capable of playing a carrier function. Thus, when the same raw materials are used for preparing saccharicterpenin, only the product prepared by combining the specific supercritical fluid extraction process in the invention can prepare white powder with loose cellular micropore structure capable of exerting the function of a carrier.
Comparing example 1 with comparative example 4, it was found that the appearance of the saccharicterpenin analogue prepared by using peeled and dehulled camellia seed kernel as raw material in the invention is white, the microstructure is provided with a loose cellular microporous structure (shown in figure 2), however, the four appearance of the saccharicterpenin prepared by using shelled camellia seed in comparative example 4 is dark yellow, and the microstructure is not provided with a loose cellular microporous structure (shown in figure 6). The saccharicterpenin analogue prepared by the invention not only has better color and luster than the saccharicterpenin IV, but also has a honeycomb micropore structure capable of playing a carrier function. Therefore, when the same supercritical fluid extraction process is used for preparing the saccharicterpenin, white powder with appearance and loose cellular microporous structure capable of playing a carrier function can be prepared only by using peeled and dehulled rapeseed kernels as raw materials.
Comparative example 5
This comparative example differs from example 1 in that: the extraction pressure during supercritical fluid extraction is 20MPa, and the prepared product is named as saccharicterpenin.
Comparative example 6
This comparative example differs from example 1 in that: the extraction time of supercritical fluid extraction is 30min, and the prepared product is named as saccharicterpenin six.
Comparative example 7
This comparative example differs from example 1 in that: the extraction temperature during supercritical fluid extraction is 60 ℃, and the prepared product is named as saccharicterpenin seven.
The comparative table of supercritical fluid extraction process parameters for the preparation of saccharicterpenin in example 1 and comparative examples 5-7 of the present invention is shown in table 4:
table 4 comparison of supercritical fluid extraction process parameters corresponding to the preparation of saccharicterpenin from example 1 and comparative examples 5-7
| Treatment group | Extraction temperature/. Degree.C | Extraction pressure/MPa | Extraction time/min |
| Example 1 | 40 | 35 | 90 |
| Comparative example 5 | 40 | 20 | 90 |
| Comparative example 6 | 40 | 35 | 30 |
| Comparative example 7 | 60 | 35 | 90 |
The saccharicterpenin five, the saccharicterpenin six and the saccharicterpenin seven respectively prepared by the methods of comparative examples 5-7 are shown in fig. 7-9, which respectively change the extraction pressure, the extraction time and the extraction temperature in the supercritical fluid extraction process on the basis of example 1. When the extraction pressure (20 MPa) and the extraction time (30 min) are reduced, the residual grease in the extracted product is increased, so that the appearance forms of the saccharicterpenin five and the saccharicterpenin six do not accord with the product standard, the fluidity is poor, and meanwhile, a honeycomb micropore structure (shown in figures 7-8) is not seen on the microstructure, so that the result is more obvious in the product with reduced extraction pressure; when the extraction temperature is changed, the product becomes dark in appearance color, there may be loss or change of nutrients, and at the same time, the honeycomb structure becomes weak in characterization and the pore structure becomes significantly smaller in microstructure, so that the carrier function and stability as a feed additive of vitamins, trace elements and the like are insufficient (as shown in fig. 9). Therefore, when any one of the parameters of the extraction pressure, the extraction time and the extraction temperature in the supercritical fluid extraction process is changed, the saccharicterpenin analog of the invention cannot be obtained, and only under the supercritical fluid extraction process conditions set by the invention, the saccharicterpenin analog with good product color and luster and honeycomb micropore structure which plays a carrier function can be prepared.
Experimental example 1 parameter comparison of saccharicterpenin analog with commonly used organic Carrier and inorganic Carrier
The experimental example examined the parameter comparison of the saccharicterpenin analog prepared in the example 1 of the present invention with the commonly used organic carrier (rice hull powder) and the non-agent carrier (medical stone), and the results are shown in table 5:
TABLE 5 basic parameter comparison Table of saccharicterpenin analogs as functional vectors and commonly used vectors
Through the parameter comparison analysis of the saccharicterpenin analogues in the table and common organic and inorganic carriers in the market, the saccharicterpenin analogues prepared by the invention are slightly superior to the conventional organic carrier-rice hull powder in the aspects of surface characteristics, particle size, repose angle (fluidity), moisture content, pH, microorganism content, heavy metal content, chemical stability, nutritional ingredients, production process and the like; has great difference with the inorganic carrier-medical stone; the saccharicterpenin analogue prepared by the invention belongs to a functional organic carrier, meets the requirements of the carrier, and has special advantages in the nutrition components and the production process of the product compared with the common carrier.
Experimental example 2 study of the stability of saccharicterpenin analogs to vitamins with commonly used organic carriers, inorganic carriers and saccharicterpenin prepared in comparative examples 1 to 7
The experimental example examines the determination of vitamin stability when the saccharicterpenin analog prepared in the embodiment 1 of the invention plays a role of a carrier with rice hull powder, medical rice Dan Yi and carriers prepared in the comparative examples 1-7 (namely saccharicterpenin one to saccharicterpenin seven), and the specific determination method comprises the following steps:
vitamin premix feed containing ten different carriers of saccharicterpenin analogues, rice hull powder, medical stone and saccharicterpenin-to-saccharicterpenin seven is prepared according to the formula of Table 6, and is utilizedThe small mixer mixes the corresponding carriers with vitamins in a tumbling manner, 10 Kg/group, 3 replicates per carrier 3 groups, and the mixing time and corresponding parameters are the same. Sealing and packaging in dark place, storing in constant temperature and humidity (20deg.C, relative humidity 60%) environment, sampling at 30d,45d and 60d, and respectively processing vitamin B according to GB/T14700-2018 and GB/T17812-2008 1 And detecting the content of vitamin E, wherein the vitamin loss rate is calculated according to the following formula: loss rate = (recipe set point-measurement value) ×100%/recipe set point.
TABLE 6 Carrier function test formulas (kg) of different carriers versus vitamins
Note that: the saccharicterpenin (one-seven) in the table refers to the saccharicterpenin prepared by respectively adding the methods corresponding to the comparative examples 1-7, wherein the product prepared in the comparative example 1 is the saccharicterpenin I, the product prepared in the comparative example 2 is the saccharicterpenin II, the product prepared in the comparative example 3 is the saccharicterpenin III, and the products prepared in the comparative example 7 are the saccharicterpenin seven. The following is the same.
Vitamin B in vitamin premix feed by different carriers 1 (abbreviated as VB) 1 ) The results of the loss rate of (2) are shown in FIGS. 10-12. As can be seen from FIGS. 10 to 12, the saccharicterpenin analogs prepared according to the present invention are directed against VB 1 The loss rate of (2) is the lowest, the effect is the best, VB of 30d, 45d and 60d 1 Loss rates were 5.9%, 6.8% and 7.8%, respectively; rice hull powder as organic carrier, VB 1 VB with lower loss rate of 60d 1 The loss rate is 8.4%; medical stone as inorganic carrier, VB 1 Higher VB at 60d 1 The loss rate reaches 15.2%; compared with saccharicterpenin analogues and rice hull powder, saccharicterpenin-to saccharicterpenin seven is used as vitamin VB 1 The vector has poor properties, VB 60d 1 The loss rate is above 15%, sugarThe oil exists in the terpene five and six, VB 1 The loss rate is larger, wherein VB of saccharicterpenin five 60d 1 The loss rate was 38.3%.
The results of the loss rate of vitamin E (VE for short) from the different carriers in the vitamin premix feed are shown in FIGS. 13-15. 13-15, the loss rate of VE of the saccharicterpenin analog prepared by the invention is equivalent to that of the rice hull powder of the organic carrier, the effect is optimal, and the VE loss rate of 60d is 8.6% and 8.2% respectively; medical stone and saccharicterpenin are poor in property as vitamin carriers, the VE loss rate of 60d is between 17.0% and 41.9%, and the loss rate of the saccharicterpenin is maximum due to the existence of polyunsaturated grease.
Experimental example 3 study of the stability of the saccharicterpenin analogs with the commonly used organic carriers, inorganic carriers and the saccharicterpenin complexes prepared in comparative examples 1 to 7 against microelements
The experimental example examines the stability of the microelement complex when the saccharicterpenin analog prepared in the embodiment 1 of the invention plays a role of a carrier with rice hull powder, medical rice Dan Yi and carriers prepared in the comparative examples 1-7 (namely saccharicterpenin one to saccharicterpenin seven), and the specific measuring method comprises the following steps:
microelement premix feed containing the saccharicterpenin analogues, rice hull powder, medical stone and the eleven different carriers of saccharicterpenin one to saccharicterpenin seven is prepared according to the formula of the table 7, the corresponding carriers and microelement complex are subjected to overturn mixing by using a small mixer, 10 Kg/group is carried out, 3 groups of each carrier are repeated, and the mixing time and the corresponding parameters are the same. After being sealed and packaged in a light-proof way, the packaging material is placed in a constant temperature and humidity (20 ℃ and relative humidity of 60%) environment for storage, sampling is carried out at 30d,60d and 120d, the contents of the iron glycine complex and the zinc methionine complex are detected according to the methods of GB/T21996-2008 and GB 21694-2017 respectively, and the loss rate is calculated according to the following formula: loss rate = (recipe set point-measurement value) ×100%/recipe set point.
TABLE 7 Carrier function test formulas (kg) of different carriers for microelement complexes
The results of the loss rate of trace element complex iron glycine in trace element premix feed by different carriers are shown in fig. 16-18. 16-18, it can be seen that the saccharicterpenin analogs prepared by the invention have better protection effect on iron glycinate as carriers, and the iron glycinate loss rates of 30d, 60d and 120d are respectively 6.6%, 7.8% and 9.0%; conventionally, for trace element complexes, inorganic carriers have better effects than organic carriers. The product is used as an organic carrier, and the carrier effect of the product on the iron glycinate is between rice hull powder (organic carrier) and medical stone (inorganic carrier). The carrier properties of saccharicterpenin one to saccharicterpenin seven produced by other processes are poorer than those of the saccharicterpenin analogues, wherein the loss rate of the glycine iron of 120d is the highest and reaches 25.8% because of the fact that the saccharicterpenin five contains polyunsaturated fatty acids; the loss rate of the glycine iron of the other 6 carriers is 13.1-23.7%.
The results of the loss rate of trace element complex zinc methionine in trace element premix feed by different carriers are shown in fig. 19-21. As shown in FIGS. 19-21, compared with the ten other carriers, the sugar terpene extract analogue prepared by the invention has the lowest loss rate of zinc methionine and the best protection effect, and the loss rates of zinc methionine of 30d, 60d and 120d are respectively 5.6%, 6.9% and 7.9%, which are superior to those of rice hull powder and medical stone which are conventional carriers; the protection effect of saccharicterpenin-to saccharicterpenin-seven on zinc methionine produced by other processes is 13.1% -24.4% than that of the saccharicterpenin analogue, rice hull powder and medical rice Dan Cha, 120 d.
Experimental examples 1-3 show that the saccharicterpenin analogue prepared by the invention can play a role of a carrier, can effectively reduce the loss of vitamin and trace element complex in feed, and improve the stability of the vitamin and trace element; the saccharicterpenin analogues prepared only by the specific process of peeling, shelling, supercritical fluid extraction and screening adopted by the invention have obvious carrier functions, and when any one step or process parameter is changed or replaced, a product with poor carrier properties can be obtained, so that the function of maintaining the stability of vitamins and trace elements in the feed by the carrier cannot be effectively exerted.
Experimental example 4 Effect of feed additive on laying hen production performance and egg quality
The experimental example examined the effect of the feed additive prepared in example 4 on the productivity and egg quality of the laying hens, and the specific operation procedure was as follows:
(1) The premix feed for laying hens is prepared by using the feed additive prepared in the embodiment 4, rice hull powder and saccharicterpenin I are adopted to replace saccharicterpenin analogues respectively as a control group, and firstly rice hull powder, saccharicterpenin analogues or saccharicterpenin I, and complex vitamin, trace elements and amino acid are added to obtain the feed additive; and adding defatted corn germ powder, choline chloride, calcium hydrophosphate, stone powder and medical stone in sequence, and mixing to obtain 3 premixed feeds for laying hens, wherein the formulation table of the premixed feeds is shown in table 8.
Table 8 4% table of mixed premix feed for laying hens
Note that: 1) The vitamin complex comprises, by weight, 0.37 part of vitamin A, 0.15 part of vitamin D, 1.85 parts of tocopheryl acetate, 3.75 parts of niacin, 1.85 parts of calcium pantothenate, 0.55 part of vitamin K, 0.92 part of vitamin B2, 0.55 part of vitamin B6 and 0.01 part of vitamin B12;
2) The trace element complex comprises 6 parts of copper glycinate complex, 20 parts of iron glycinate complex, 14 parts of zinc methionine complex and 15 parts of manganese methionine complex in parts by weight.
(2) The 3 kinds of premixed feed for the laying hens are adopted to prepare basic feed (complete compound feed) for the laying hens. The formulation shown in Table 9 was followed.
Table 9 table of formulas of complete compound feeds for laying hens
(3) Animal test
Healthy, middle-late-period sea blue brown commodity laying hens with close laying rate are selected to be 450, randomly divided into 3 groups, and 6 repeats are selected from each group, and 25 repeats are selected from each group. The control group was fed with rice hull meal basal diet, the saccharicterpenin analog group and the saccharicterpenin analog group were fed with saccharicterpenin analog basal diet and saccharicterpenin-basal diet, respectively, for 1 week in the pre-test period and 7 weeks in the positive test period. The laying hens adopt a 3-layer laminated cage raising mode, are fed at fixed time for 4 times per day, drink water freely, have the illumination intensity of 15Lx, have the illumination time of 16 hours per day, and have the temperature of the henhouse controlled at 16-22 ℃. The productivity and egg quality were examined.
Measurement of production performance: the number of healthy survival, egg production and egg weight of chickens were recorded in duplicate units at 14:00 per day under the same management conditions. The correlation calculation formula is as follows: egg yield = average total number of eggs per day/chicken number; average egg weight (g) =average total daily egg weight/average total daily egg number.
Egg quality index determination: on the 5 th and 7 th weekends of the pilot period, 2 eggs were randomly collected from each repetition for egg quality determination. The egg weight was measured using an electronic balance, the egg longitudinal and transverse diameter lengths were measured using a vernier caliper, and the egg shape index was calculated. Breaking eggs and pouring the eggs on a glass plate which is adjusted to be in a horizontal position, selecting 3 egg white positions which are 1cm away from the periphery of yolk as egg white height measurement points, respectively measuring by using an egg white height measuring instrument, taking an average value of the 3 egg white positions as the egg white height, and calculating Hash units according to the egg white height and egg weight. Eggshell thickness was calculated by measuring eggshell thickness at the tip, blunt end and intermediate position of eggshell using eggshell thickness measuring instrument. Yolk color was measured under fluorescent lamp using a rogowski color fan. And (5) separating yolk, and weighing by an electronic balance to obtain yolk weight. The correlation calculation formula is as follows: egg shape index = egg longitudinal length/egg transverse length; egg yolk rate = (egg yolk weight/egg weight) ×100%; eggshell thickness= (tip eggshell thickness + blunt eggshell thickness + intermediate eggshell thickness)/3; haet unit=100×lg (high protein +7.57- 1.7 times egg weight 0.37 ). The results are shown in tables 10-11 and FIG. 22.
TABLE 10 Effect of feed additives on the performance of laying hens
Note that: the same row of data shoulder marks are the same or no letters indicate that the difference is not significant (P > 0.05), different lowercase letters indicate that the difference is significant (P < 0.05), and different uppercase letters indicate that the difference is extremely significant (P < 0.01). The table below is the same.
TABLE 11 influence of feed additives on the quality of egg laying eggs
As can be seen from tables 10-11 and fig. 22, when the feed additive prepared by adopting the saccharicterpenin analogs prepared by the invention is used for preparing the complete compound feed for the laying hens to feed the laying hens, the corresponding laying rate is improved to 87.11% from 84.46% of the control group, and is obviously higher than the average laying rate of one group of saccharicterpenin, so that the production performance of the laying hens can be obviously improved; in addition, the egg quality and the Ha's unit of the egg can be obviously improved, so that the freshness of the egg is improved, and the egg quality improving device have the function of improving the quality of animal products.
Experimental example 5 Effect of feed additive on pig productivity and serum Biochemical
The experimental example examines the influence of the feed additive prepared from the saccharicterpenin analogue of the invention on the production performance and serum biochemistry of weaned pigs, and the specific operation process is as follows:
(1) The pre-mixed feed for weaned pigs containing the saccharicterpenin analog is prepared. Adopting rice hull powder and saccharicterpenin I to replace the saccharicterpenin analogue prepared in the embodiment 1 as a control group, firstly adding the rice hull powder, the saccharicterpenin analogue or the saccharicterpenin I, and mixing with a complex vitamin and trace element complex to obtain a feed additive; and adding zeolite powder, and finally sequentially adding phytase, an acidulant, an antioxidant and a diluent to mix to obtain 3 pre-mixed feeds for weaned pigs, wherein the formula of the specific pre-mixed feeds is shown in table 12.
TABLE 12 premixed feed for weaned pigs 1%
Note that: 1) The vitamin complex comprises, by weight, 0.37 part of vitamin A, 0.15 part of vitamin D, 1.85 parts of tocopheryl acetate, 3.75 parts of niacin, 1.85 parts of calcium pantothenate, 0.55 part of vitamin K, 0.92 part of vitamin B2, 0.55 part of vitamin B6 and 0.01 part of vitamin B12;
2) The trace element complex comprises 6 parts of copper glycinate complex, 20 parts of iron glycinate complex, 14 parts of zinc methionine complex and 15 parts of manganese methionine complex in parts by weight.
(2) The 3 kinds of weaned pig premix feed are adopted to prepare basic feed (complete compound feed) for weaned pigs. The formulation shown in Table 13 was followed.
Table 13 formula table of complete compound feed for weaned pigs
(3) Animal test
The experiment selects 48 healthy (ternary hetero) Du X long X big piglets weaned at 21 days, randomly groups 3, 8 repeats each group, and 2 piglets each repeat; the control group is fed with rice husk powder basic diet, the saccharicterpenin analog group and the saccharicterpenin analog group are respectively fed with saccharicterpenin analog diet and saccharicterpenin one diet, and the diet does not contain zinc oxide and drug feed additives. The pre-feeding period was 3 days and the positive trial period was 28 days.
The test pigs are fed by single columns and eat and drink water freely. The pigsty is cleaned and disinfected at regular time according to a conventional pigsty cleaning and disinfecting system, the pigsty is cleaned and dried in the pigsty, the temperature of the pigsty is controlled to be 22-26 ℃, immunization and feeding management are carried out according to a conventional pigsty immunization program, the feed intake is recorded every day, and the health and mental condition of the pigsty are observed.
Measurement of production performance: all pigs were weighed on an empty stomach at the beginning of the formal trial and at 28d, and Average Daily Feed Intake (ADFI), average Daily Gain (ADG), and feed-to-weight ratio (F/G) were calculated from the recorded feed intake. The method comprises the following steps: average Daily Gain (ADG) = (end-initial average weight) per day of test; average Daily Feed Intake (ADFI) =total feed consumption/number of pigs tested/number of days tested; feed weight ratio (F/G) =average daily feed intake/average daily gain.
Fecal scoring: the stool morphology and stool contamination at the anus of the pigs were observed at 09:00 and 16:00 daily. The stool scores were graded as: 0 minutes-normal; 1 min-soft stool; 2 minutes-mild diarrhea; 3 minutes-severe diarrhea.
Serum was used and tested: on day 28 of the formal test, 1 piglet per group was randomly selected, 10mL of vena cava blood before collection was allowed to stand at 4℃for 1 hour, and after centrifugation at 3000rpm for 10min, serum was prepared and isolated and stored at-80℃for biochemical and immunological index detection. The total protein, albumin, globulin, alanine aminotransferase, aspartic acid aminotransferase, urea, total cholesterol, triglyceride, immunoglobulin A, immunoglobulin G and immunoglobulin M content in the serum samples were determined using a full-automatic biochemical analyzer and a kit (Shanghai enzyme-linked biotechnology Co., ltd.). Statistical analysis was performed on the test data and the results are shown in tables 14-16.
TABLE 14 Effect of feed additives on weaned piglet production Performance
TABLE 15 Effect of feed additives on piglet faecal scoring (diarrhea)
Table 16 Effect of saccharicterpenin analog feed additive with Carrier function on serum Biochemical and immune index of piglets
As can be seen from the tables 14-16, compared with a control group, when the feed additive prepared by adopting the saccharicterpenin analogue prepared by the invention is used for preparing the complete compound feed for weaned pigs to feed the weaned pigs, the average daily gain and daily feed intake of the weaned pigs can be obviously improved, the feed-to-feed ratio can be reduced, and the growth performance of the weaned pigs can be effectively improved; the method can also remarkably reduce the fecal score of the piglets, can effectively improve the intestinal health of the piglets, prevent diarrhea, and can also remarkably improve the content of serum immunoglobulin G of the piglets, thereby effectively improving the immune level of the piglets.
The experimental summary of experimental examples 4-5 shows that when the feed additive prepared from the saccharicterpenin analogue is used for preparing complete compound feeds for laying hens and weaned pigs, the animal production performance can be effectively improved, the animal product quality can be improved, and the animal immunity can be improved.
The present invention is not limited to the above-mentioned embodiments, but is intended to be limited to the following embodiments, and any modifications, equivalent changes and variations in the above-mentioned embodiments can be made by those skilled in the art without departing from the scope of the present invention.
Claims (10)
1. A preparation method of a saccharicterpenin analogue with a carrier function is characterized by comprising the following steps of: the method comprises the following steps:
1) Drying and peeling the oil tea fruits to obtain oil tea seeds with the water content of 3-8%;
2) Shelling the camellia seeds to obtain camellia seed kernels;
3) Crushing camellia seed kernels;
4) Loading the crushed camellia seed kernels into a supercritical fluid extraction kettle for supercritical fluid extraction, wherein the extraction temperature of the supercritical fluid extraction is 30-55 ℃, the extraction pressure is 25-50MPa, and the extraction time is 45-90min; reducing the pressure to normal pressure after the extraction is finished, and obtaining a dry and clean primary product as raffinate;
5) Sieving the primary product with 40 mesh sieve, and collecting the undersize to obtain the saccharicterpenin analog with carrier function.
2. A process for the preparation of a saccharicterpenin analog with carrier function as claimed in claim 1, wherein: the moisture content of the camellia seeds peeled in the step 1) is 4-8%.
3. A process for the preparation of a saccharicterpenin analog with carrier function as claimed in claim 2, wherein: the particle size of the crushed particles in the step 3) is 0.1-1.0mm.
4. A process for the preparation of a saccharicterpenin analog with carrier function as claimed in claim 1, wherein: the extraction temperature of the supercritical fluid extraction in the step 4) is 35-45 ℃, the extraction pressure is 35-45MPa, and the extraction time is 60-90min.
5. A saccharicterpenin analog with carrier function, characterized in that: the process for the preparation of a saccharicterpenin analog according to any one of claims 1-4, wherein the saccharicterpenin analog is a white powder and has a loose cellular microporous structure, and the pore diameter of the micropores is 0.2-1.5 μm.
6. Use of a saccharicterpenin analog with carrier function according to claim 5 in feed, characterized in that: the saccharicterpenin analogue is used as a carrier of vitamin and trace element complex for preparing feed additives and premixed feeds, and can improve the stability of the vitamin and trace element complex in the feeds.
7. Use of a saccharicterpenin analog with carrier function according to claim 6 in feed, characterized in that: the feed additive comprises the following components in parts by weight: 25-50 parts of saccharicterpenin analogues, 10-20 parts of compound vitamins and 30-65 parts of trace element complexes.
8. Use of a saccharicterpenin analog with carrier function according to claim 6 in feed, characterized in that: the premixed feed comprises a compound premixed feed, a vitamin premixed feed and a trace element premixed feed, and the compound premixed feed is prepared by adopting the feed additive as a raw material.
9. Use of a saccharicterpenin analog with carrier function according to claim 6 in feed, characterized in that: the application of the premixed feed in preparing complete compound feed.
10. Use of a saccharicterpenin analog with carrier function according to claim 9 in feed, wherein: the complete compound feed is used for feeding laying hens and pigs, and can improve the production performance of the laying hens and the pigs.
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| CN115521943A (en) * | 2022-10-10 | 2022-12-27 | 湖南文理学院 | Method for extracting saccharicterpenin from oil tea cake |
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