CN115349613B - Preparation method of roxburgh rose biological freeze-dried preparation - Google Patents
Preparation method of roxburgh rose biological freeze-dried preparation Download PDFInfo
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- CN115349613B CN115349613B CN202210737030.5A CN202210737030A CN115349613B CN 115349613 B CN115349613 B CN 115349613B CN 202210737030 A CN202210737030 A CN 202210737030A CN 115349613 B CN115349613 B CN 115349613B
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Abstract
The application discloses a preparation method of a roxburgh rose biological freeze-dried preparation, which comprises the following steps: non-thermal sterilization (HPP) of fructus Rosae Normalis pure juice by using ultrahigh pressure container + ) And (3) processing, namely, after the sterile roxburgh rose pure juice is frozen rapidly, sequentially performing vacuum sublimation drying and vacuum analysis drying in a low-temperature environment, processing, mixing with auxiliary materials, and further processing according to actual conditions to prepare the required preparation. The superoxide dismutase (SOD) enzyme activity content and the VC and total flavone content in the roxburgh rose biological freeze-dried preparation are high, the stability is good, the nutritional ingredients and the nutritional value of fresh roxburgh rose fruits are reserved to the greatest extent, the product is dampproof, convenient to carry and eat, and meanwhile, the content level of the SOD in the body can be maintained, so that the roxburgh rose biological freeze-dried preparation has good market prospect.
Description
Technical Field
The application belongs to the technical field of biological food processing, and particularly relates to a preparation method of a roxburgh rose biological freeze-dried preparation.
Background
The rosa roxburghii is a perennial fallen leaf bush of Rosa genus of Rosaceae family, and is commonly called as "rosa roxburghii", also called as mountain Wang Guo, chun Gui, zhi pear, wood pear, etc. Most of the fruits are oblate and spherical, and the fruits are crisp in pulp and have a thick fragrance after ripe fruits. Fructus Rosae Normalis is nutritious, and contains SOD, VC, VP, VP2, VB1, VB2, VB-sitosterol, VE, VA, VD, VK, calcium, phosphorus, ferrum, tannin, fructus Rosae Normalis triterpene, lipase, fructus Rosae Normalis flavone, dietary fiber, and microelements such as selenium and zinc. Wherein SOD, VC and flavone are the most abundant plants. Rosa roxburghii is known as "SOD king", "vitamin C king", folk name "magic pear" and "life-prolonging fruit", and is known as "nutrition warehouse".
SOD is considered as the most magic enzyme in life technology. SOD is one of substances with the functions of resisting aging, regulating immunity, regulating blood fat, resisting radiation and beautifying, and the legal numbering is ECl.15.1.1; CAS [905489]1.SOD is one of the most important enzymes in human body, and can delay aging because SOD can remove free radicals. People can age, and signs of aging are observed in a bit, such as pigmentation, physical deterioration, and oxidation in the body, and the supplement of antioxidants helps to reduce the oxidation speed and slow down the aging steps. Preventing and treating autoimmune diseases, SOD has certain curative effect on various autoimmune diseases. Medical reports indicate that the decay period of the antioxidant capacity is advanced to about 40 years old, and the light leaning on vegetables and fruits is insufficient to eliminate the oxidative pressure formed by the human body both inside and outside. The prevention of chronic diseases, free radicals are the main cause of the scientists to find that various chronic diseases and aging are caused, so that the disease is the source of thousands of diseases, is the great enemy of human health, and the damage of the free radicals to the body is accumulated in daily life. To make the body healthy, the oxidation speed is slow, and the in vivo SOD is kept sufficient; unfortunately, the in vivo SOD activity and concentration gradually decrease after 25 years of age, so we have to supplement exogenous SOD to compensate for the missing SOD in the human body, so that the human body is healthy.
The detected fresh fructus Rosae Normalis juice (without sterilization or non-heating sterilization) contains 3 SOD, and the proportion of three enzymes is as follows: the first 65.3%; the second 14.4%; the third 20.3%. The compound preparation is superior to an anti-aging and beautifying compound preparation for treating diseases such as cancers, and the like, and therefore, the roxburgh rose has the following functions: 1. enhancing organism resistance, enhancing immunity, resisting virus, and preventing diseases. SOD in fructus Rosae Normalis has obvious effects of relieving fatigue, enhancing immunity, and supplementing energy. 2. Cancer prevention and anticancer: rosa roxburghii is rich in superoxide dismutase (SOD) 10000U/ml. SOD is internationally recognized as an active substance with an anticancer effect, and in addition, has obvious effects on improving immunity, resisting radiation and the like, and is a first killer of 'hundred-disease source' active oxygen free radicals. The causes of tumors are numerous, but whatever the cause of the tumor, the tumor is ultimately caused by free radicals destroying the expression of the oncogene, while activating the protooncogene. After SOD enters human cells, DNA is protected and self-repaired, so that cancer suppressor genes and protooncogenes in the human body are stable and balanced, the hematopoietic function of bone marrow is promoted, the immunity of the human body is stimulated and promoted, the cells which tend to be mutated are destroyed before canceration, and meanwhile, the cells are prevented from dissociating to other parts of the human body, so that the purposes of preventing and resisting cancers are achieved. Vitamin E, B-sitosterol, SOD and catalase in fructus Rosae Normalis form a protective system for eliminating active oxygen such as free radical of superoxide anion, and has anticancer effect. 3. Anti-aging. SOD is an internationally recognized anti-aging drug. The fructus Rosae Normalis contains rich superoxide dismutase (SOD), and can improve SOD activity in human body, reduce Lipid Peroxide (LPO), and has obvious antiaging effect. SOD also has the effect of repairing damaged cells, so that the cell activity is greatly enhanced. SOD has the effect of scavenging free radicals of human body-! 4. Has sedative effect, and can make people fall asleep quickly. SOD can be used for clinically treating insomnia, can remove excessive free radicals in vivo, and can improve and treat tissue organ dysfunction and disorder, thereby achieving the purpose of treating sleep disorder. In addition, the roxburgh rose also contains vitamin C, vitamin B1 (thiamine acid), vitamin B2 (riboflavin) and other nutrient elements, and has the health-care effects of resisting oxidation, protecting skin, beautifying, expelling lead, treating scurvy, treating beriberi, strengthening spleen, promoting digestion, relieving pain, reducing three highs, preventing diabetes and the like.
There are some documents concerning the freeze-drying of roxburgh rose to prepare a convenient food, for example:
1. the application number CN202110915141.6 discloses a roxburgh rose freeze-dried powder and a processing method thereof, wherein the roxburgh rose freeze-dried powder comprises roxburgh rose stock solution and high fructose syrup, the first process step is that after the roxburgh rose fruits are washed and dried, water is removed, juice is squeezed and obtained, so as to obtain the roxburgh rose stock solution, and the roxburgh rose stock solution and the high fructose syrup are mixed in proportion to obtain mixed solution; step two, the mixed solution is placed into a quick-freezing warehouse for speed, and the freezing temperature is-40 to-35 ℃; transferring the frozen mixed solution into a vacuum freeze dryer for vacuum drying to obtain a semi-finished product, wherein the vacuum degree is less than or equal to 100pa, and heating in a vacuum environment to promote drying, and the heating temperature is 30-55 ℃. The method is characterized in that the method is frozen at the temperature of minus 40 ℃ to minus 35 ℃, all water such as free water in the mixed solution is frozen into solid state, the solid state is quickly dried under high vacuum condition, the boiling point of the water can be changed under vacuum environment, so that solid ice in the raw material can be sublimated and converted into gas state under low temperature, the water is dried, the color, shape, taste and the like of the raw material are reserved to the greatest extent, and the active ingredients of the raw material are reserved. However, the proposal does not adopt the subsequent process of humidity control and product dampproof process, and the roxburgh rose contains hydrophilic components such as sugar, starch, resin, pectin, mucilage, mashing, inorganic salt and the like, so that the freeze-dried product is extremely easy to absorb moisture and becomes soft, caking, deliquescing and even liquefying due to moisture absorption, thereby mildewing, bacteria breeding and spoiling, and is very unsafe to eat. In addition, the scheme does not adopt a sterilization process, raw materials are operated in a non-clean area, pollution is positive, the raw materials are placed for a long time, moisture absorption is added, bacteria breeding in the raw materials are positive, and quality cannot be guaranteed. Thus, shelf life is short, commercial and unsafe.
2. The application number 201610354549X discloses a gold roxburgh rose vacuum freeze-drying treatment process, wherein the vacuum degree of a vacuum drying bin is raised to 100-150 pa in the process step (4), the temperature is controlled to 70-80 ℃, and the temperature is kept for 6-10 hours. SOD has biological activity, and can easily inactivate SOD biological protease in fructus Rosae Normalis at above 60deg.C, and maintain at 70-80deg.C for 6-10 hr, wherein most SOD is inactivated, and VC and flavone are destroyed to lose their value.
3. Application number CN201510774934.5 discloses a method for producing seedless roxburgh rose freeze-dried tablets, which comprises the following steps: a. and (3) raw material treatment: cleaning fresh seedless Rosa roxburghii, slicing and airing the surface water; b. Freezing; c. vacuum drying: controlling the vacuum degree in the vacuum freeze dryer to be 20-40 Pa, the drying temperature to be-25 to-18 ℃ and the drying time to be 3-6 h; d. and (5) analysis and drying: gradually reducing the vacuum degree in the vacuum freeze dryer to 5-10 Pa, gradually increasing the drying temperature to 35-50 ℃, and drying for 5-15 min to obtain seedless roxburgh rose freeze-dried tablets; e. sterile packaging; the seedless roxburgh rose freeze-dried tablet produced by the method can keep the original flavor and shape, the nutrition and functional components are not lost, the method accords with the regulations in the edible fungus sanitation standard GB7096-2003, and the water content index is lower than 1/2 of the national standard. However, this solution has the following drawbacks: (1) whether the rosa roxburghii is seedy or seedless, the rosa roxburghii is divided into an edible part and a non-edible part, wherein the edible part is mainly pulp, the non-edible part is mainly pericarp and seed, for example, juice is squeezed, the juice yield is generally about 50%, namely, a large part of the rosa roxburghii is non-edible. (2) According to the scheme, a peeling process is not adopted before slicing, seedless roxburgh rose with the diameter of 3-8cm is selected according to the first embodiment and the second embodiment, and after slicing, the diameter of the finished seedless roxburgh rose freeze-dried slice is 0.5cm as the smallest possible, and the eating method is only chewing. Although the freeze-drying process is carried out, the freeze-dried slices are not frozen into powder, the non-edible insoluble long fibers in the pericarps are still wrapped around the freeze-dried slices, and the insoluble long fibers cannot swallow after chewing, so that the product quality is affected. (3) The technical scheme does not have a humidity control process, although in the second and third embodiments, e, packaging: the dried product is taken out in time, but the time difference is also a certain in the industrial production. The water content of the seedless roxburgh rose freeze-dried tablet is below 5%, and the roxburgh rose freeze-dried tablet contains hydrophilic components such as sugar, starch, resin, pectin, mucilage, mashing, inorganic salt and the like, has strong hygroscopicity, is easy to absorb water in the air, and is difficult to ensure the quality of the seedless roxburgh rose freeze-dried tablet under the working condition. (4) The technical scheme is that the package is sterile, but a sterilization process is not adopted, and under the working condition, the quality of the seedless roxburgh rose freeze-dried tablet is difficult to ensure.
4. The patent application 201610464953.2 discloses a preparation method of a roxburgh rose freeze-dried particle, and further provides a preparation method of the roxburgh rose freeze-dried particle, which can also have the following characteristics: the method comprises the following specific steps: (a) standing the original juice of the roxburgh rose for at least 5 hours, and filtering; (b) concentrating in vacuum to 1/4-1/5 of the original volume; (c) Adding a protective agent into the concentrated solution, stirring until the protective agent is completely dissolved, and adjusting the pH value to 6-8 after filtering; (d) performing a vacuum freeze drying process; (e) And (3) carrying out sterile packaging after crushing to obtain the roxburgh rose freeze-dried particles. Wherein in step (e), both the pulverization and the aseptic packaging are carried out in an environment where the temperature is not more than 25 ℃ and the relative humidity of air is not more than 40%. And sealing by adopting an aluminum-plastic composite bag to obtain the roxburgh rose freeze-dried particles. However, the technical scheme has the defects and disadvantages that: (1) the original juice of fructus Rosae Normalis is left standing in air for 5 hr, and VC, SOD, flavone, etc. are oxidized to reduce its content. (2) In the unclean area, the original juice of the roxburgh rose is kept still in the air for 5 hours, the original juice is polluted, the sterilization process is not carried out, and the freeze-dried product is crushed and packaged in a sterile room, but the product quality can not be ensured. (3) Although the protective agent is added into the concentrated solution, glucose can avoid the caking of the solution during drying, so that the dried product is loose and fragile. However, the roxburgh rose contains hydrophilic components such as saccharides, starch, resin, pectin, mucilage, mashing, inorganic salt and the like, has strong hygroscopicity and strong viscosity, and has poor fluidity, lubricity and formability.
Because the Rosa roxburghii has shorter storage period and contains more tannin, the Rosa roxburghii has heavier bitter taste and is difficult to be accepted; rosa roxburghii contains rich bioactive protease such as superoxide dismutase (SOD), such as juicing, and needs to be sterilized for prolonging shelf life, but traditional heating sterilization can destroy the bioactivity of superoxide dismutase (SOD) and other nutrients such as VC, ketones and the like, thereby losing the value. When the pure roxburgh rose juice is prepared into a freeze-dried product, the freeze-dried product of the pure roxburgh rose juice contains hydrophilic components such as polysaccharide, pectin, mucilage and the like besides strong physiological activity and chemical components with definite pharmacological action, has strong hygroscopicity, and softens, blocks, deliquesces, mildews and bacteria breeds and even liquefies due to moisture absorption, thereby affecting the pharmacological and health-care values of the freeze-dried product. Meanwhile, the half-life period of superoxide dismutase (SOD) in the body is short, and besides a small amount of superoxide dismutase is taken or eaten for many times, the content level of superoxide dismutase (SOD) in the body is maintained for a long time.
The unique nutritional value of the fresh rosa roxburghii fruit in fruit and vegetable foods is important for health, anti-aging and beauty of people, but the prior art does not overcome the defects of high-temperature sterilization or non-sterilization and dampproof technology of the rosa roxburghii freeze-dried preparation or product, and the rosa roxburghii freeze-dried product which can furthest retain the nutritional components and the medical value of the rosa roxburghii freeze-dried preparation or product, has dampproof property, is convenient to carry and eat and can maintain the content level of SOD in the body cannot be researched.
Disclosure of Invention
Aiming at the problems and the defects of the technology, the application provides a preparation method of a roxburgh rose biological freeze-dried preparation. According to the application, after non-thermal sterilization, the pure juice of the roxburgh rose is freeze-dried and mixed with auxiliary materials, and then the mixed juice is further processed according to actual conditions to prepare the preparation required by the roxburgh rose biological freeze-dried preparation, wherein the vitamin C and flavone in the roxburgh rose biological freeze-dried preparation are less in damage, high in content and good in stability, the superoxide dismutase (SOD) enzyme activity is not damaged, even the SOD enzyme activity is improved or activated, the nutritional ingredients and the nutritional value of fresh roxburgh rose fruits are reserved to the greatest extent, and the product is dampproof, convenient to carry and eat, and meanwhile, the content level of the SOD in the body can be maintained for a long time, so that the preparation has good market prospect.
In order to achieve the above purpose, the present application adopts the following technical scheme:
a preparation method of a fructus Rosae Normalis biological lyophilized preparation comprises the following steps: non-thermal sterilization treatment is carried out on the pure juice of the roxburgh rose by adopting ultra-high pressure (HPP+), after the sterile pure juice of the roxburgh rose is frozen rapidly, vacuum sublimation drying and vacuum analysis drying are carried out in sequence in a low-temperature environment for treatment, the mixed material is mixed with auxiliary materials, and then the mixed material is further processed into required tablets, granules, powder or capsules according to actual conditions, so that the roxburgh rose biological freeze-dried preparation is obtained.
Further, the granule is prepared by granulating, microencapsulating and aseptically packaging the mixed materials; the tablet is prepared by granulating, tabletting, coating, and packaging with aluminum-plastic bubble cap or sterile bag or bottle.
The microencapsulation is to granulate the mixture material, namely the capsule core material, by using natural or synthetic polymer film-forming materials, namely capsule materials, and then to embed the mixture material into the microcapsule with the semi-permeability or sealing capsule film and the diameter of 5-250 mu m.
The processes of granulating, microencapsulating, coating, packaging and the like are mainly moisture-proof, so that the product is prevented from being deteriorated due to moisture absorption; the microcapsule is embedded or encapsulated, namely the slow release technology of the roxburgh rose biological freeze-dried preparation. The microcapsule embedding or microencapsulation capsule has dampproof and slow release effects, so as to maintain the content level of SOD in vivo.
Further, the preparation method of the roxburgh rose biological freeze-dried preparation comprises the following steps:
(1) Pretreatment: cleaning fresh fructus Rosae Normalis, and air drying to remove surface water;
(2) Juice squeezing: sending the fresh rosa roxburghii fruit processed in the step (1) into a juicer for juicing, and filtering and deslagging twice to obtain rosa roxburghii pure juice;
(3) Non-heat sterilization (hpp+) treatment: sealing the pure Rosa roxburghii juice obtained in the step (2) by using a large-package plastic bag or plastic bottle, then sending the plastic bag or plastic bottle filled with the pure Rosa roxburghii juice into a high-pressure cabin of a UHP, HHP or HPP ultrahigh-pressure container, adding a medium, then sealing the high-pressure cabin, applying pressure to the ultrahigh-pressure container and maintaining pressure for sterilization to obtain the sterile pure Rosa roxburghii juice;
(4) Cleaning and sterilizing the large package: the sterile Rosa roxburghii pure juice large package in the step (3) is conveyed to a sterile environment through a clean air curtain for cleaning, disinfection and sterilization; the large package is a plastic flexible package or a plastic bottle for filling;
(5) Quick freezing: under the aseptic environment, unpacking the large package cleaned and sterilized in the step (4), sub-packaging the sterile roxburgh rose pure juice into a bracket layered tray, and sending the bracket layered tray into a quick-freezing warehouse or a freeze dryer for quick freezing to obtain frozen roxburgh rose pure juice;
(6) Vacuum sublimation drying: the frozen roxburgh rose pure juice bracket layered tray in the step (5) is sent into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and a frozen and dried roxburgh rose pure juice freeze-dried product after sterilization, namely a vacuum sublimation dried product is obtained;
(7) Vacuum analysis and drying: collecting the vacuum sublimated and dried product, respectively loading the product and auxiliary materials into a bracket layered tray together, conveying the bracket layered tray into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimated and dried product and auxiliary materials to obtain a true quick analysis dried product and dried auxiliary materials;
(8) Mixing: according to the weight portion, the vacuum analysis dried product and the drying auxiliary materials are stirred, mixed and homogenized at a certain rotating speed, and then further processed according to the actual situation to prepare the required preparation, thus obtaining the roxburgh rose biological freeze-dried preparation.
Further, in the step (2), the filter screen for the first filtration is 200-300 meshes, and the filter screen for the second filtration is 400-800 meshes.
The filtering purpose is to remove the cellulose, pectin and other invalid components in the juice, reduce the yield of the freeze-dried roxburgh rose juice, and the yield of the freeze-dried powder with the water content of 10 percent is less than or equal to 5 percent, thereby improving the content of the effective components of the freeze-dried powder, overcoming the defect of large dosage and reducing the hygroscopicity of the freeze-dried product.
Further, in step (3), the medium is water or higher hydraulic oil; when the medium in the ultrahigh pressure container is water, applying 400-600 MPa pressure to the pure Rosa roxburghii juice packaged in the plastic flexible package or the plastic bottle, and keeping the pressure for 5-15 min; when the medium in the ultrahigh pressure container is high-grade hydraulic oil, applying 100-1000 MPa to the pure Rosa roxburghii juice packaged in the plastic flexible package or the plastic bottle; the dwell time is 1-30 min.
The application adopts ultra-high pressure sterilization technology (UHP for short) or high static pressure technology (high hydrostatic pressure for short) or high pressure sterilization technology (high pressure processing for short) for non-thermal sterilization (HPP+) to kill bacteria, mold and saccharomycetes in the pure juice of the Rosa roxburghii in plastic flexible package or plastic bottle package, and the application can not cause the inactivation of active ingredients such as SOD and the like in the pure juice of the Rosa roxburghii in plastic flexible package or plastic bottle package and the destruction of nutritional ingredients such as VC, VP and the like in a large amount like the high temperature sterilization.
Further, in the step (5), the rapid freezing temperature is-30 to-40 ℃.
Further, in the step (6), the vacuum degree of vacuum sublimation drying is 30-150 pa, the temperature is 30-40 ℃, and the water content of the vacuum sublimation dried product is 10+/-2%.
Further, in the step (7), the vacuum degree of the vacuum analysis drying is 5-30 pa, the temperature is 40-60 ℃, the relative humidity of air is 20-40%, and the water content of the true quick analysis drying product is 5+/-2%; the auxiliary materials are mixed auxiliary materials prepared by mixing microcrystalline cellulose, micro powder silica gel and dextrin according to the mass ratio of = (0.3-0.4): (0.2-0.4), and the mass ratio of the three auxiliary materials is added to be 1.
The auxiliary materials have the functions of moisture absorption prevention, lubrication, slow release and the like, the auxiliary materials are added to ensure that the process of the biological freeze-dried preparation of the roxburgh rose is carried out smoothly and the safety and the effectiveness of finished products are ensured, the auxiliary materials have good fluidity, hygroscopicity, formability and lubricity, the auxiliary materials can be single auxiliary materials or combined auxiliary materials, and the drug loading rate of the auxiliary materials is not lower than the self weight.
The door of the sublimation drying chamber is communicated with the sterile or clean area of the non-controlled wet area, and the rest is isolated from the sterile area of the non-controlled wet area; the sterilized pure roxburgh rose juice is quickly frozen at the temperature of minus 30 to minus 40 ℃, and then frozen water molecules are directly sublimated into water vapor at the temperature of 30 to 40 ℃ in a vacuum environment of 30 to 150pa so as to be removed, thus obtaining a freeze-dried product of the sterilized pure roxburgh rose juice with the water content of 10+/-2 percent.
Further, in the step (8), the mass ratio of the vacuum analysis dried product to the drying auxiliary material is=1:x, and x is less than or equal to 1.
And (3) in the vacuum analysis and drying process, the sublimated and freeze-dried product and auxiliary materials are placed in a vacuum environment of 5-30 pa, and part of water remained in the sublimated and freeze-dried product is evaporated at the temperature of 40-60 ℃ so that the water content reaches the requirement of 5+/-2%. The vacuum analysis drying chamber and the communicating chamber thereof are subjected to humidity control treatment, the relative air humidity is controlled to be 20-40%, the door of the vacuum analysis drying chamber is communicated with the aseptic space of the humidity control area, and the rest is isolated from the aseptic space of the humidity control area; the air pressure between the sterile rooms of the humidity control area is more than 5pa greater than the air pressure between the sterile rooms of the non-humidity control area.
Further, when the roxburgh rose biological freeze-dried preparation is a granule, the mixed material is prepared by granulating, microencapsulating and aseptically packaging; when the roxburgh rose biological freeze-dried preparation is a tablet, the mixed material is prepared by granulating, tabletting, coating, aluminum-plastic bubble cap or aseptic bagging or bottling packaging; the rotating speed is 500-600 r/min. When the coating is carried out by adopting a fluidization coating method, the fluidization temperature is less than or equal to 60 ℃.
The granulation adopts dry granulation: the freeze-dried product and auxiliary materials are uniformly mixed, pressed into slices with certain hardness and diameter by a tablet press, and crushed into freeze-dried preparations with certain size particles by a particle crusher, wherein the freeze-dried preparations comprise rolling, granulating and other methods. The steps of mixing the vacuum-resolved dry product with the auxiliary material and dry granulation can be performed in one apparatus.
The microcapsule is microcapsule embedding, namely microcapsule, which is to granulate a freeze-dried product of roxburgh rose by using natural or synthetic polymer film-forming materials, namely capsule cores, and then embed the freeze-dried product of roxburgh rose into a semi-permeable or sealed capsule film, and the diameter of the microcapsule is 5-250 mu m by using a certain method and equipment; the microcapsule embedding or microencapsulation capsule has dampproof and slow release effects, so as to maintain the content level of SOD in vivo.
Tabletting refers to granulating fructus Rosae Normalis lyophilized product and its mixture or granulating and microencapsulating, and tabletting by rotary multi-punch tabletting technology. The tablets are packed by adopting aluminum plastic bubble caps, namely, the freeze-dried preparation of the roxburgh rose after being coated is packed by adopting a bubble cap packing machine, and the tablet has the printing function.
The coating refers to the freeze-dried preparation of the roxburgh rose after tabletting, and the coating is carried out by adopting a rolling or fluidization coating method. When the fluidized coating method is adopted for coating, the hot air temperature is less than or equal to 60 ℃, and the activity of superoxide dismutase SOD can be destroyed when the hot air temperature is higher than 60 ℃. The fluidization temperature is less than or equal to 60 ℃ during coating.
Adopts dry granulation technology: because the roxburgh rose freeze-dried powder is micro-fine powder, the specific surface area is large, and the moisture absorption capability is strong; after dry granulation, larger particles are formed, the specific surface area is reduced, and the hygroscopicity is reduced. The microcapsule embedding or microencapsulation technology is adopted, and the freeze-dried preparation, namely the capsule core material, is coated by natural or synthetic capsule materials to form a semi-permeable or totally-enclosed film, so that the moisture absorption of the freeze-dried preparation of the roxburgh rose can be effectively blocked. The compression-molded roxburgh rose freeze-dried preparation adopts a coating technology to coat the molded roxburgh rose freeze-dried preparation, thereby effectively preventing the roxburgh rose freeze-dried preparation from absorbing moisture. The coated freeze-dried roxburgh rose preparation is subjected to blister packaging or vacuum packaging, so that moisture absorption caused by contact with air due to complete opening can be avoided when the freeze-dried roxburgh rose preparation is eaten or taken.
Further, the VC content in the roxburgh rose biological freeze-dried preparation is more than or equal to 30mg/g, the SOD (superoxide dismutase) biological activity content is more than or equal to 20000-50000 u/g, and the flavone content is more than or equal to 4mg/g. Pathogenic bacteria, namely salmonella, shigella and staphylococcus aureus, are not detected in the roxburgh rose biological freeze-dried preparation; the critical relative humidity of the roxburgh rose biological freeze-dried preparation is more than or equal to 70 percent. The quality is ensured to be kept for 18 months under the environment with the relative humidity of 60-75 percent. The prepared roxburgh rose biological freeze-dried preparation meets the requirements.
Further, the clean level of the sterile environment is not lower than 30 ten thousand.
The large package cleaning and sterilizing, quick freezing and vacuum sublimation drying processes are all carried out in a sterile or clean area non-humidity control area, the clean level is not lower than 30 ten thousand, the relative humidity is 40-65%, the unclean area and the clean area are separated by a clean air curtain, and the air pressure of the clean area is more than 5pa of the air pressure of the unclean area; vacuum analysis drying, mixing vacuum analysis dried product with auxiliary materials, granulating, micro-capsule embedding or micro-encapsulation, tabletting, coating, tablet aluminum-plastic bubble cap or aseptic bagging or bottling packaging and aseptic granule packaging processes are all carried out in a humidity control area, the relative humidity is 20-40%, the humidity control area and a non-humidity control area are separated by a clean air curtain, and the air pressure of the humidity control area is more than 5pa higher than that of the non-humidity control area; the unclean area and the outdoor are separated by an air curtain, and the air pressure of the unclean area is more than 10pa of the air pressure of the outdoor; the relative humidity of air in a humidity control area of a sterile room or clean area is 20-40%.
Of course, the preparation process also comprises boxing, labeling and warehousing, namely boxing, labeling and warehousing the packaged freeze-dried roxburgh rose preparation.
During the whole production process, the air pressure of the sterile clean area is 5pa greater than that of the unclean area; the unclean section air pressure is 105pa greater than the outdoor ambient air pressure.
In the application, the cleaning, air drying, juice squeezing, nonthermal (HPP+) sterilization, boxing, labeling and packaging of the fresh rosa roxburghii fruits are all carried out in a non-clean area; the large package cleaning and disinfecting, the freezing in the quick freezing warehouse and the vacuum sublimating and drying are carried out in a non-humidity control area of a sterile or clean area, the clean level is not lower than 30 ten thousand, and the relative humidity of the non-humidity control area is 40-65%; vacuum resolving and drying with auxiliary materials, mixing with auxiliary materials, dry granulating, micro-capsule embedding or micro-encapsulation, tabletting, coating, tablet aluminum-plastic bubble cap or aseptic bag or bottle packaging and granule aseptic packaging are all carried out in an aseptic or clean area humidity control area, and the air relative humidity is 20-40%.
The quick freezing, vacuum sublimation drying and vacuum desorption drying can be carried out in a freeze dryer. Vacuum sublimation drying and vacuum desorption drying can be performed in one freeze dryer. The door of the quick freezing warehouse is communicated with the sterile room or clean area, and the rest is isolated from the sterile room. The quick freezing can be performed in a freeze-drying box in the freeze dryer or in a special quick-freezing warehouse; the mixing with the auxiliary material and the dry granulation step can be carried out in one apparatus.
The door of the sublimation drying chamber is communicated with the sterile or clean area of the non-controlled wet area, and the rest is isolated from the sterile area of the non-controlled wet area; the door of the analysis drying chamber is communicated with the aseptic room of the humidity control area, and the rest is isolated from the aseptic room of the humidity control area; the sterile room of the humidity control area and the sterile room of the non-humidity control area are separated by a clean air curtain; the air pressure between the sterile rooms of the humidity control area is more than 5pa greater than the air pressure between the sterile rooms of the non-humidity control area; the air pressure between the sterility is more than 10pa than the air pressure of the non-sterility environment; the unclean area is isolated from the outside by an air curtain. When the fluidized coating method is adopted for coating, the temperature of hot air is less than or equal to 60 ℃, and the activity of superoxide dismutase SOD can be destroyed when the temperature is higher than 60 ℃, so that the temperature is controlled.
Because the application adopts the technical proposal, the application has the following beneficial effects:
(1) The application adopts a filter with 400-800 meshes to carry out secondary filtration after freshly squeezed juice of the roxburgh rose, removes cellulose, pectin, mucilage, mashing substances and other ineffective components in the juice, reduces the yield of the roxburgh rose juice after freeze-drying, ensures that the yield of freeze-dried powder with the water content of 10 percent is less than or equal to 5 percent, improves the content of effective components of the freeze-dried powder, overcomes the defect of large dosage and reduces the hygroscopicity of freeze-dried products.
(2) The application adopts a non-thermal (HPP+) sterilization and vacuum freeze-drying mode, can keep the activity of SOD biological protease in the frozen products of the roxburgh rose, ensures that the damage of VC, flavone and the like in the frozen preparations of the roxburgh rose is small, thereby keeping the nutrition value of the roxburgh rose; meanwhile, the fructus Rosae Normalis is convenient to carry and eat, and plays a role in preventing and treating diseases, protecting health, resisting aging, beautifying and the like.
(3) Because the roxburgh rose freeze-dried preparation contains hydrophilic components such as polysaccharide, pectin, mucilage and the like, has strong hygroscopicity, and softens, blocks, deliquesces, mildews and breeds bacteria and even liquefies due to moisture absorption, the pharmacological and health-care values of the roxburgh rose freeze-dried preparation are affected, and therefore the moisture prevention of the roxburgh rose freeze-dried preparation is very important. In the preparation process, relevant key steps are carried out in an environment with the relative humidity of 20-40%, and the preparation type is combined, and the moisture absorption prevention technology is adopted in the preparation process, so that the influence on the product quality due to the excessive humidity of the process environment and the moisture absorption of the freeze-dried roxburgh rose preparation is avoided. In addition, the microcapsule embedding or microencapsulation and coating technology can not only effectively prevent moisture absorption, but also have a slow release effect, and as the half-life period of superoxide dismutase SOD in the body is short, the freeze-dried preparation of the roxburgh rose is continuously and slowly released through microencapsulation and coating, so that the SOD with a high content is maintained at a certain content level in the body, thereby achieving the purposes of treatment and health care.
(4) The quick freezing, sublimation drying and analytical drying of the application are generally completed by an integrated machine. The yield of the freeze-dried pure roxburgh rose juice is generally less than 5%, if an integrated machine is adopted, quick freezing needs 8-12 hours, sublimation drying needs 6-10 hours, and if mass production is adopted, the production efficiency is affected; sublimation drying and analytical drying are generally completed by an integrated machine, but the yield of the freeze-dried pure roxburgh rose juice is generally less than 5%, the consumption of the pure roxburgh rose juice is large, the time for loading and unloading dishes is long, the contact time of the freeze-dried preparation and air is long, and moisture absorption is unavoidable, so that the product quality is affected. Therefore, the three procedures of quick freezing, sublimation drying and analysis drying are separated in the process flow, and the analysis drying procedure is carried out in the humidity control area, so that the influence on the product quality due to long time consumption for loading and unloading the tray and long moisture absorption time is avoided, and meanwhile, the production efficiency is improved.
(5) The existing production process flow of the solid traditional Chinese medicine preparation such as tablets, capsules, particles and the like does not have the processes of sterilizing and disinfecting raw materials, and the processes of extracting, purifying, concentrating, drying and the like of components can be performed in a clean area, but the raw materials of the traditional Chinese medicine can be bacteria, so that the safety risk is brought to the finished product drug administration. The biological freeze-dried preparation of the roxburgh rose adopts HPP+ non-thermal sterilization pretreatment, so that pathogenic bacteria (salmonella, shigella and staphylococcus aureus) cannot be detected, and the risk is avoided.
Drawings
For a clearer description of an example of the application or of a technical solution in the prior art, the drawings required in the description of the embodiment or of the prior art will be briefly described, it being obvious that the drawings in the description below are only some examples of the application, from which, without the inventive development, other drawings can be obtained for a person skilled in the art:
FIG. 1 is a process flow diagram of a biological lyophilized formulation of Rosa roxburghii according to the application;
FIG. 2 is a graph showing the Critical Relative Humidity (CRH) measured on coated tablets of the biological lyophilized formulation of Rosa roxburghii of the application;
FIG. 3 is a graph of Critical Relative Humidity (CRH) measured on non-coated tablets of a biologically lyophilized formulation of Rosa roxburghii according to the application;
FIG. 4 is a graph showing the Critical Relative Humidity (CRH) of the granule assay of the biological lyophilized preparation of Rosa roxburghii of the application.
Detailed Description
The following detailed description of the application is provided in further detail, but the application is not limited to these embodiments, any modifications or substitutions in the basic spirit of the present examples, which still fall within the scope of the application as claimed.
Example 1
A preparation method of a roxburgh rose biological freeze-dried preparation comprises the following steps:
(1) Pretreatment: cleaning fresh fructus Rosae Normalis, and air drying to remove surface water;
(2) Juice squeezing: sending the fresh rosa roxburghii fruit processed in the step (1) into a juicer for juicing, and filtering and deslagging twice to obtain rosa roxburghii pure juice; the filter screen for the first filtering is 300 meshes, the filter screen for the second filtering is 600 meshes, and the yield of the freeze-dried powder with the water content of 10% is about 5%;
(3) Non-heat sterilization (hpp+): filling and sealing the pure Rosa roxburghii juice obtained in the step (2) by using a large-package plastic bag or a plastic bottle, then sending the plastic bag or the plastic bottle filled with the pure Rosa roxburghii juice into a high-pressure chamber of an HPP ultrahigh-pressure container, adding medium water, sealing the high-pressure chamber, applying pressure to the ultrahigh-pressure container, maintaining pressure and sterilizing to obtain the sterile pure Rosa roxburghii juice; applying 600MPa pressure to the pure juice of fructus Rosae Normalis packaged in plastic soft package or plastic bottle, and maintaining for 5min;
(4) Cleaning and sterilizing the large package: the sterile Rosa roxburghii pure juice large package in the step (3) is conveyed to a sterile environment through a clean air curtain for cleaning, disinfection and sterilization;
(5) Quick freezing: under the aseptic environment, unpacking the large package cleaned and sterilized in the step (4), sub-packaging the sterile roxburgh rose pure juice into a bracket layered tray, and sending the bracket layered tray into a quick-freezing warehouse or a freeze dryer for quick freezing to obtain frozen roxburgh rose pure juice; the temperature of the rapid freezing is-35 ℃;
(6) Vacuum sublimation drying: the frozen roxburgh rose pure juice bracket layered tray in the step (5) is sent into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and a frozen and dried roxburgh rose pure juice freeze-dried product after sterilization, namely a vacuum sublimation dried product is obtained; the vacuum degree of the vacuum sublimation drying is 50pa, the temperature is 35 ℃, and the water content of the vacuum sublimation drying product is 10+/-2%;
(7) Vacuum analysis and drying: collecting the vacuum sublimated and dried product, respectively loading the product and auxiliary materials into a bracket layered tray together, conveying the bracket layered tray into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimated and dried product and auxiliary materials to obtain a true quick analysis dried product and dried auxiliary materials; the vacuum degree of the vacuum analysis drying is 10pa, the temperature is 50 ℃, the relative humidity of air is 20%, and the water content of the true quick analysis drying product is 5+/-2%; the auxiliary materials are mixed auxiliary materials prepared by mixing microcrystalline cellulose, micro-powder silica gel and dextrin according to the mass ratio of (0.3:0.3:0.4).
(8) Mixing: stirring, mixing and homogenizing the vacuum analysis dried product and the drying auxiliary materials at a certain rotating speed according to the weight part ratio, and granulating, tabletting, coating and aluminum-plastic blister packaging to obtain the biological freeze-dried preparation of the roxburgh rose, wherein the biological freeze-dried preparation is an aluminum-plastic blister packaging coated tablet; the mass ratio of the vacuum analysis dried product to the drying auxiliary material is 1:1; the roxburgh rose biological freeze-dried preparation is a coated tablet; the rotating speed is 600r/min; the content of VC in the roxburgh rose biological freeze-dried preparation is more than or equal to 30mg/g, the content of SOD (superoxide dismutase) biological activity is more than or equal to 20000-50000 u/g, and the content of flavone is more than or equal to 4mg/g; pathogenic bacteria (salmonella, shigella, staphylococcus aureus) are not detected; the critical relative humidity of the obtained roxburgh rose biological freeze-dried preparation is more than or equal to 70%, and the quality guarantee period is 18 months under the environment with the relative humidity of 60-75%.
Further, the clean level of the sterile environment is not lower than 30 ten thousand; the fluidization temperature is less than or equal to 60 ℃ during coating; the relative humidity of air in a humidity control area of a sterile room or clean area is 20-40%.
Example 2
A preparation method of a roxburgh rose biological freeze-dried preparation comprises the following steps:
(1) Pretreatment: cleaning fresh fructus Rosae Normalis, and air drying to remove surface water;
(2) Juice squeezing: sending the fresh rosa roxburghii fruit processed in the step (1) into a juicer for juicing, and filtering and deslagging twice to obtain rosa roxburghii pure juice; the filter screen for the first filtering is 300 meshes, and the filter screen for the second filtering is 800 meshes;
(3) Non-heat sterilization (hpp+): filling and sealing the pure Rosa roxburghii juice obtained in the step (2) by using a large-package plastic bag or a plastic bottle, then conveying the plastic bag or the plastic bottle filled with the pure Rosa roxburghii juice into a high-pressure cabin of an HPP ultrahigh-pressure container, adding medium high-grade hydraulic oil, sealing the high-pressure cabin, applying pressure to the ultrahigh-pressure container, maintaining pressure and sterilizing to obtain the sterile pure Rosa roxburghii juice; applying 500MPa pressure to the pure juice of fructus Rosae Normalis packaged in plastic soft package or plastic bottle, and maintaining for 20min;
(4) Cleaning and sterilizing the large package: the sterile Rosa roxburghii pure juice large package in the step (3) is conveyed to a sterile environment through a clean air curtain for cleaning, disinfection and sterilization;
(5) Quick freezing: under the aseptic environment, unpacking the large package cleaned and sterilized in the step (4), sub-packaging the sterile roxburgh rose pure juice into a bracket layered tray, and sending the bracket layered tray into a quick-freezing warehouse or a freeze dryer for quick freezing to obtain frozen roxburgh rose pure juice; the temperature of the rapid freezing is-40 ℃;
(6) Vacuum sublimation drying: the frozen roxburgh rose pure juice bracket layered tray in the step (5) is sent into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and a frozen and dried roxburgh rose pure juice freeze-dried product after sterilization, namely a vacuum sublimation dried product is obtained; the vacuum degree of the vacuum sublimation drying is 100pa, the temperature is 40 ℃, and the water content of the vacuum sublimation drying product is 10+/-2%;
(7) Vacuum analysis and drying: collecting the vacuum sublimated and dried product, respectively loading the product and auxiliary materials into a bracket layered tray together, conveying the bracket layered tray into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimated and dried product and auxiliary materials to obtain a true quick analysis dried product and dried auxiliary materials; the vacuum degree of the vacuum analysis drying is 20pa, the temperature is 45 ℃, the relative humidity of air is 40%, and the water content of the true quick analysis drying product is 5+/-2%; the auxiliary materials are mixed auxiliary materials prepared by mixing microcrystalline cellulose, micro-powder silica gel and dextrin according to the mass ratio of (0.4:0.4:0.2).
(8) Mixing: stirring, mixing and homogenizing the vacuum analysis dried product and the drying auxiliary materials at a certain rotating speed according to the weight part ratio, and granulating, tabletting and asepsis bagging packaging to obtain the roxburgh rose biological freeze-dried preparation which is an asepsis bagging packaging non-coating tablet; the mass ratio of the vacuum analysis dried product to the drying auxiliary material is=1:0.8; the roxburgh rose biological freeze-dried preparation is a non-coated tablet; the rotating speed is 520r/min; the content of VC in the roxburgh rose biological freeze-dried preparation is more than or equal to 33mg/g, the content of SOD (superoxide dismutase) biological activity is more than or equal to 22000-55000 u/g, and the content of flavone is more than or equal to 4.4mg/g.
Further, the clean level of the sterile environment is not lower than 30 ten thousand; a humidity control area of an aseptic or clean area, and the relative humidity of air is 20-40%; the critical relative humidity of the obtained roxburgh rose biological freeze-dried preparation is more than or equal to 70%, and the quality guarantee period is 18 months under the environment with the relative humidity of 60-75%.
Example 3
A preparation method of a roxburgh rose biological freeze-dried preparation comprises the following steps:
(1) Pretreatment: cleaning fresh fructus Rosae Normalis, and air drying to remove surface water;
(2) Juice squeezing: sending the fresh rosa roxburghii fruit processed in the step (1) into a juicer for juicing, and filtering and deslagging twice to obtain rosa roxburghii pure juice; the filter screen for the first filtering is 200 meshes, and the filter screen for the second filtering is 800 meshes;
(3) Non-heat sterilization (hpp+): filling and sealing the pure Rosa roxburghii juice obtained in the step (2) by using a large-package plastic bag or plastic bottle, then sending the plastic bag or plastic bottle filled with the pure Rosa roxburghii juice into a high-pressure cabin of a UHP, HHP or HPP ultrahigh-pressure container, adding medium high-grade hydraulic oil, sealing the high-pressure cabin, applying pressure to the ultrahigh-pressure container, maintaining pressure and sterilizing to obtain sterile pure Rosa roxburghii juice; when the medium in the ultrahigh pressure container is high-grade hydraulic oil, applying 100MPa pressure to the pure Rosa roxburghii juice packaged in the plastic flexible package or the plastic bottle; the dwell time is 30min;
(4) Cleaning and sterilizing the large package: the sterile Rosa roxburghii pure juice large package in the step (3) is conveyed to a sterile environment through a clean air curtain for cleaning, disinfection and sterilization;
(5) Quick freezing: under the aseptic environment, unpacking the large package cleaned and sterilized in the step (4), sub-packaging the sterile roxburgh rose pure juice into a bracket layered tray, and sending the bracket layered tray into a quick-freezing warehouse or a freeze dryer for quick freezing to obtain frozen roxburgh rose pure juice; the temperature of the rapid freezing is-30 ℃;
(6) Vacuum sublimation drying: the frozen roxburgh rose pure juice bracket layered tray in the step (5) is sent into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and a frozen and dried roxburgh rose pure juice freeze-dried product after sterilization, namely a vacuum sublimation dried product is obtained; the vacuum degree of the vacuum sublimation drying is 150pa, the temperature is 30 ℃, and the water content of the vacuum sublimation drying product is 10+/-2%;
(7) Vacuum analysis and drying: collecting the vacuum sublimated and dried product, respectively loading the product and auxiliary materials into a bracket layered tray together, conveying the bracket layered tray into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimated and dried product and auxiliary materials to obtain a true quick analysis dried product and dried auxiliary materials; the vacuum degree of the vacuum analysis drying is 30pa, the temperature is 40 ℃, the relative humidity of air is 30%, and the water content of the true quick analysis drying product is 5+/-2%; the auxiliary materials are mixed auxiliary materials prepared by mixing microcrystalline cellulose, micro-powder silica gel and dextrin according to the mass ratio of (0.35:0.35:0.3).
(8) Mixing: stirring, mixing and homogenizing the vacuum analysis dried product and the drying auxiliary materials at a certain rotating speed according to the weight part ratio, and granulating, microencapsulating and aseptically packaging to obtain the biological freeze-dried preparation of the roxburgh rose, wherein the biological freeze-dried preparation is aseptically packaged granules; the mass ratio of the vacuum analysis dried product to the drying auxiliary material is=1:0.9; the roxburgh rose biological freeze-dried preparation is sterile packaged granules; the rotating speed is 500r/min; the VC content in the roxburgh rose biological freeze-dried preparation granules is more than or equal to 31.5mg/g, the SOD (superoxide dismutase) biological activity content is more than or equal to 21000-52000 u/g, and the flavone content is more than or equal to 4.2mg/g; the critical relative humidity of the obtained roxburgh rose biological freeze-dried preparation is more than or equal to 70%, and the quality guarantee period is 18 months under the environment with the relative humidity of 60-75%.
Further, the clean level of the sterile environment is not lower than 30 ten thousand; the relative humidity of air in a humidity control area of a sterile room or clean area is 20-40%.
Example 4
A preparation method of a roxburgh rose biological freeze-dried preparation comprises the following steps:
(1) Pretreatment: cleaning fresh fructus Rosae Normalis, and air drying to remove surface water;
(2) Juice squeezing: sending the fresh rosa roxburghii fruit processed in the step (1) into a juicer for juicing, and filtering and deslagging twice to obtain rosa roxburghii pure juice; the filter screen for the first filtering is 300 meshes, and the filter screen for the second filtering is 400 meshes;
(3) Non-heat sterilization (hpp+): filling and sealing the pure Rosa roxburghii juice obtained in the step (2) by using a large-package plastic bag or plastic bottle, then sending the plastic bag or plastic bottle filled with the pure Rosa roxburghii juice into a high-pressure cabin of a UHP, HHP or HPP ultrahigh-pressure container, adding medium high-grade hydraulic oil, sealing the high-pressure cabin, applying pressure to the ultrahigh-pressure container, maintaining pressure and sterilizing to obtain sterile pure Rosa roxburghii juice; when the medium in the ultrahigh pressure container is high-grade hydraulic oil, applying 1000MPa to the pure Rosa roxburghii juice packaged in the plastic flexible package or the plastic bottle; the dwell time is 1min;
(4) Cleaning and sterilizing the large package: the sterile Rosa roxburghii pure juice large package in the step (3) is conveyed to a sterile environment through a clean air curtain for cleaning, disinfection and sterilization;
(5) Quick freezing: under the aseptic environment, unpacking the large package cleaned and sterilized in the step (4), sub-packaging the sterile roxburgh rose pure juice into a bracket layered tray, and sending the bracket layered tray into a quick-freezing warehouse or a freeze dryer for quick freezing to obtain frozen roxburgh rose pure juice; the temperature of the rapid freezing is-40 ℃;
(6) Vacuum sublimation drying: the frozen roxburgh rose pure juice bracket layered tray in the step (5) is sent into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and a frozen and dried roxburgh rose pure juice freeze-dried product after sterilization, namely a vacuum sublimation dried product is obtained; the vacuum degree of the vacuum sublimation drying is 30pa, the temperature is 40 ℃, and the water content of the vacuum sublimation drying product is 10+/-2%;
(7) Vacuum analysis and drying: collecting the vacuum sublimated and dried product, respectively loading the product and auxiliary materials into a bracket layered tray together, conveying the bracket layered tray into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimated and dried product and auxiliary materials to obtain a true quick analysis dried product and dried auxiliary materials; the vacuum degree of the vacuum analysis drying is 5pa, the temperature is 60 ℃, the relative humidity of air is 35%, and the water content of the true quick analysis drying product is 5+/-2%; the auxiliary materials are mixed auxiliary materials prepared by mixing microcrystalline cellulose, micro-powder silica gel and dextrin according to the mass ratio of (0.25:0.25:0.5).
(8) Mixing: stirring, mixing and homogenizing the vacuum analysis dried product and the drying auxiliary materials at a certain rotating speed according to the weight part ratio, and granulating, tabletting, coating, bottling and packaging to obtain the biological freeze-dried preparation of the roxburgh rose, namely the bottled, packaged and coated tablet; the mass ratio of the vacuum analysis dried product to the drying auxiliary material is=1:0.7; the roxburgh rose biological freeze-dried preparation is a coated tablet; the rotating speed is 580r/min; the content of VC in the roxburgh rose biological freeze-dried preparation is more than or equal to 35mg/g, the content of SOD (superoxide dismutase) biological activity is more than or equal to 23000-58000/g, and the content of flavone is more than or equal to 4.7mg/g; the critical relative humidity of the obtained roxburgh rose biological freeze-dried preparation is more than or equal to 70%, and the quality guarantee period is 18 months under the environment with the relative humidity of 60-75%.
Further, the clean level of the sterile environment is not lower than 30 ten thousand; the fluidization temperature of the coating is less than or equal to 60 ℃; a humidity control area of an aseptic or clean area, and the relative humidity of air is 20-40%; pathogenic bacteria (salmonella, shigella, staphylococcus aureus) are not detected.
Example 5
A preparation method of a roxburgh rose biological freeze-dried preparation comprises the following steps:
(1) Pretreatment: cleaning fresh fructus Rosae Normalis, and air drying to remove surface water;
(2) Juice squeezing: sending the fresh rosa roxburghii fruit processed in the step (1) into a juicer for juicing, and filtering and deslagging twice to obtain rosa roxburghii pure juice; the filter screen for the first filtering is 250 meshes, and the filter screen for the second filtering is 700 meshes;
(3) Non-heat sterilization (hpp+): filling and sealing the pure Rosa roxburghii juice obtained in the step (2) by using a large-package plastic bag or plastic bottle, then sending the plastic bag or plastic bottle filled with the pure Rosa roxburghii juice into a high-pressure cabin of a UHP, HHP or HPP ultrahigh-pressure container, adding medium high-grade hydraulic oil, sealing the high-pressure cabin, applying pressure to the ultrahigh-pressure container, maintaining pressure and sterilizing to obtain sterile pure Rosa roxburghii juice; when the medium in the ultrahigh pressure container is high-grade hydraulic oil, applying 500MPa pressure to the pure Rosa roxburghii juice packaged in the plastic flexible package or the plastic bottle; the dwell time is 15min;
(4) Cleaning and sterilizing the large package: the sterile Rosa roxburghii pure juice large package in the step (3) is conveyed to a sterile environment through a clean air curtain for cleaning, disinfection and sterilization;
(5) Quick freezing: under the aseptic environment, unpacking the large package cleaned and sterilized in the step (4), sub-packaging the sterile roxburgh rose pure juice into a bracket layered tray, and sending the bracket layered tray into a quick-freezing warehouse or a freeze dryer for quick freezing to obtain frozen roxburgh rose pure juice; the temperature of the rapid freezing is-35 ℃;
(6) Vacuum sublimation drying: the frozen roxburgh rose pure juice bracket layered tray in the step (5) is sent into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and a frozen and dried roxburgh rose pure juice freeze-dried product after sterilization, namely a vacuum sublimation dried product is obtained; the vacuum degree of the vacuum sublimation drying is 90pa, the temperature is 35 ℃, and the water content of the vacuum sublimation drying product is 10+/-2%;
(7) Vacuum analysis and drying: collecting the vacuum sublimated and dried product, respectively loading the product and auxiliary materials into a bracket layered tray together, conveying the bracket layered tray into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimated and dried product and auxiliary materials to obtain a true quick analysis dried product and dried auxiliary materials; the vacuum degree of the vacuum analysis drying is 25pa, the temperature is 50 ℃, the relative humidity of air is 30%, and the water content of the true quick analysis drying product is 5+/-2%; the auxiliary materials are mixed auxiliary materials prepared by mixing microcrystalline cellulose, micro-powder silica gel and dextrin according to the mass ratio of (0.3:0.3:0.4).
(8) Mixing: stirring, mixing and homogenizing the vacuum analysis dried product and the drying auxiliary materials at a certain rotating speed according to the weight part ratio, and granulating, tabletting and packaging the mixture by using an aluminum-plastic bubble cap to obtain the biological freeze-dried preparation of the roxburgh rose, wherein the biological freeze-dried preparation is an aluminum-plastic bubble cap packaging non-coating tablet; the mass ratio of the vacuum analysis dried product to the drying auxiliary material is=1:1; the roxburgh rose biological freeze-dried preparation is a non-coated tablet; the rotating speed is 550r/min; the content of VC in the roxburgh rose biological freeze-dried preparation is more than or equal to 30mg/g, the content of SOD (superoxide dismutase) biological activity is more than or equal to 20000-50000 u/g, and the content of flavone is more than or equal to 4mg/g; the critical relative humidity of the obtained roxburgh rose biological freeze-dried preparation is more than or equal to 70%, and the quality guarantee period is 18 months under the environment with the relative humidity of 60-75%.
Further, the clean level of the sterile environment is not lower than 30 ten thousand; a humidity control area of an aseptic or clean area, and the relative humidity of air is 20-40%; pathogenic bacteria (salmonella, shigella, staphylococcus aureus) are not detected.
In order to verify the creativity of the technical scheme of the invention and the advancement compared with the prior art, the following experiment is carried out:
comparative example 1
The difference from example 1 is that: a freeze-dried biological preparation of roxburgh rose is prepared through high-temp sterilization, heating the freshly squeezed juice of roxburgh rose to 75-90 deg.C, sterilizing for 15-16 s, aseptic filling and other conditions.
In order to further illustrate that the technical effect of the invention can be achieved, the following experiment is carried out:
experiment one:
and (3) determining the content of main components of the non-heat-killing analytical dried product and the freeze-dried preparation of the Rosa roxburghii pure juice.
1. Purpose of test
The main component content of the freeze-dried roxburgh rose preparation prepared by mixing the dried roxburgh rose juice with auxiliary materials and granulating and other processes is changed.
2. Test materials
2.1 test article
2.1.1 analytical dried Rosa roxburghii pure juice
The analytical drying product is prepared by the method of example 1 after juicing, filtering, non-thermal sterilization, large package cleaning and sterilizing, quick freezing, vacuum sublimation drying and vacuum analytical drying processes of Rosa roxburghii.
2.1.2 biological lyophilized preparation of fructus Rosae Normalis;
according to the method of the embodiment 1, the non-heat sterilization roxburgh rose pure juice analysis dry product or freeze-dried powder is mixed with auxiliary materials, the mass ratio of the analysis dry product to the auxiliary materials is 1:1, and the roxburgh rose biological freeze-dried preparation is obtained after the processes of granulation, tabletting, coating, packaging and the like, and is an aluminum-plastic blister package coated tablet, and the mass ratio of the analysis dry product to the auxiliary materials is 0.6 g/tablet.
2.2 Experimental grouping
12 parts of Rosa roxburghii pure juice is taken for analysis, and 2 g/part is taken as a control group and numbered respectively.
Taking 12 parts of roxburgh rose biological agent, 3 tablets per part and 0.6g per tablet as investigation groups, and numbering respectively.
3. Experimental method
3.1VC (ascorbic acid) detection method: GB 5009.86-2016 (second method)
3.2SOD (superoxide dismutase) detection method: CTC-VM-007-2012
3.3 method for detecting flavone: total flavone in chapter IV of "technical Specification for inspection and evaluation of health food" 2003 edition
3.4 evaluation index
And respectively detecting the content of VC, SOD and flavone in the pure Rosa roxburghii juice analysis dried product and the Rosa roxburghii biological preparation.
Because the roxburgh rose biological agent is prepared by mixing the roxburgh rose pure juice analysis dried product and the auxiliary materials according to the mass ratio of 1:1, one half of the detection data of a single sample of the roxburgh rose pure juice analysis dried product is used as statistical data to ensure that the roxburgh rose pure juice analysis dried product and the roxburgh rose biological agent are comparable.
3.5 entrusting the detection of the comprehensive detection center of China inspection and quarantine science institute
Report number CAIQS002100391300607.
4. Statistical analysis
The experimental data are expressed by means of mean+ -SD, and each index is statistically analyzed by the mean t test of two samples between groups, p < 0.05, p < 0.01, p < 0.001, with significant differences, using statistical software of clinician statistics assistant V10.0.
5. Experimental results
The experimental results are shown in table 1 below.
Table 1 VC, SOD, flavone control and study test data
Note that: the data of the control group is 1/2 of the actual detection data.
Table 2 average number of VC, SOD and flavone samples
As can be seen from Table 2, compared with the investigation group, the contents of VC, SOD and flavone are respectively reduced by 1.84%, 1.14% and 2.79%, the p values are all greater than 0.05, and compared with the investigation group, namely, the pure juice analysis dry product of Rosa roxburghii, the comparison group is not significant in the differences of the contents of VC, SOD and flavone, namely, the pure juice analysis dry product of Rosa roxburghii is mixed with auxiliary materials, and the obtained Rosa roxburghii biological freeze-dried preparation has small damage degree of VC, SOD and flavone and no significant difference of the two.
Experiment II:
and (3) performing experiments of destroying the main nutritional ingredients of the roxburgh rose juice by heating sterilization and non-heating sterilization.
1. Purpose of test
The condition that the main nutrition components of the roxburgh rose juice are destroyed by heat sterilization and non-heat sterilization is examined.
2. Test materials
2.1 test article
Table 3 same batch of fresh Rosa roxburghii fruit juice
2.2 Experimental grouping
2.2.1 the pure juice of the roxburgh rose is obtained by adopting high-temperature sterilization and non-thermal sterilization according to the freshly squeezed juice of the roxburgh rose, and the pure juice is divided into 3 groups of 12 parts each, and the serial numbers are respectively given.
2.2.2 The freshly squeezed juice of the roxburgh rose in group 1 is used as a control group, and the freshly squeezed juice of the roxburgh rose in group 2 and group 3 are used as investigation groups.
3. Experimental method
3.1VC (ascorbic acid) detection method GB 5009.86-2016 (second method).
3.2SOD (superoxide dismutase) detection method: according to CTC-VM-007-2012.
3.3 method for detecting flavone: total flavone is prepared according to the fourth chapter of the technical specification for inspection and evaluation of health food 2003 edition.
3.4 evaluation index
Sterilizing fructus Rosae Normalis juice by high temperature sterilization and non-thermal sterilization, and detecting VC, SOD and flavone content of sterilized fructus Rosae Normalis juice.
3.5 entrusting the detection by the comprehensive detection center of China inspection and quarantine science institute
Report number: CAIQS002000391300407.
4. Statistical analysis
The experimental data are expressed by means of mean+ -SD, and each index is statistically analyzed by the mean t test of two samples between groups, p < 0.05, p < 0.01, p < 0.001, with significant differences, using statistical software of clinician statistics assistant V10.0.
6. Experimental results
Table 4 VC, SOD and flavone group detection data
Table 5 average number of samples of VC, SOD and flavone groups
As can be seen from table 5 and table 6, the data of the inspection groups 2 and 3 are reduced compared with the data of the comparison group 1, namely, the VC and the flavone are destroyed to different degrees no matter what the sterilization method is, but the damage degree of the 2 groups of heating sterilization methods is large, the values of the 2 groups of VC and the flavone are respectively reduced by 50.49 percent and 49.17 percent, and compared with the 1 group, the p values are less than 0.001, and the difference is significant; although the non-thermal high-pressure sterilization investigation group 3 is destroyed, the VC and the flavone are respectively reduced by 3.38 percent and 4.17 percent, the p value is more than 0.05, and the difference is not significant, that is, the non-thermal sterilization VC and the flavone have minimum destruction of nutrient components, and the non-thermal high-pressure sterilization investigation group 3 is the best sterilization method and the difference is not significant.
Compared with the non-thermal sterilization of the group 3, the VC and the flavone of the group 2 are damaged to a much greater extent, the p values of the VC and the flavone of the group 2 are smaller than 0.001, and the difference is significant.
Table 6 comparison of detection data for each group of VC, SOD and flavone
As can be seen from tables 5 and 6, the heat sterilization method of group 2 has a decrease of 30.36% in SOD and a greater destruction of SOD, and the difference is significant because the p value is less than 0.001, compared with the heat sterilization method of group 1.
As can be seen from tables 5 and 6, the SOD of the non-heat autoclaving group 3 was not only not reduced but also increased by 56.98% compared with that of group 1, and the difference was significant; the SOD was 125.41% higher in the non-autoclaved 3 groups compared to the autoclaved 2 groups, and the difference was significant.
The aim of high pressure sterilization is to kill harmful bacteria and inactivate (inhibit) enzyme activity to prevent fermentation, spoilage and deterioration of foods, fruit juices, etc.
In the world and in the country, we find that the original juice of the roxburgh rose is sterilized under non-heat and high pressure for the first time, the SOD is not destroyed, and the active content of the SOD of the pure juice of the roxburgh rose is improved.
In the actual product detection, the active content of SOD breaks through 10000u/g to 12500u/g, and the formation mechanism is not clear, but the following reasons are considered in theory:
(1) by autoclaving, the cell wall is broken under high pressure, and the SOD existing in the cell is released.
(2) The two subunits of superoxide dismutase (Cu/Zn SOD), copper and zinc, form coordination bonds with histidine side chains on the active site, are bound together mainly through hydrophobic and electrostatic interactions, and have no SOD activity when the hydrophobic and electrostatic interactions are insufficient to bind them; and the SOD is combined under the action of pressure to have SOD activity and release. The active sites of Mn SOD and Fe SOD have the same type of amino acid coordinated with metal ions.
(3) There are free protein modules or fragments or short chain proteins and metal ions inside or outside the cell, which are in the free state in normal juice or pulp, and which are made possible to combine when subjected to pressure.
7. Conclusion of the experiment
From the experiment, the pure juice of the roxburgh rose is heated for sterilization, and the VC, the SOD and the flavone are destroyed in a large amount, but the non-heat high-pressure sterilization is adopted, the damage of the VC and the flavone is small, and the activity of the SOD in the pure juice of the roxburgh rose can be activated.
Experiment III:
sterilizing and non-sterilizing the pure Rosa roxburghii juice to obtain the freeze-dried powder microorganism detection experiment.
1. Purpose of test
And (5) examining microbial indexes of freeze-dried powder prepared by sterilizing and non-sterilizing pure juice of roxburgh rose.
2. Test article
2.1 sterilizing and freeze-drying powder and analytical drying product of pure Rosa roxburghii juice
The method of example 1 is followed by juicing, filtering, non-thermal sterilization, large package cleaning and sterilizing, quick freezing, vacuum sublimation drying, and vacuum resolution drying to obtain sterilized resolution dried product or lyophilized powder.
2.2 non-sterilizing freeze-dried powder and analytical dried product of pure juice of Rosa roxburghii
The non-sterilizing analytical dried product or freeze-dried powder is prepared by the method of the embodiment 1 after juicing, filtering, cleaning and sterilizing (without non-heat sterilization) the big package, quick freezing, vacuum sublimation drying and vacuum analytical drying processes.
3. Experimental method
3.1 respectively sampling the sterilizing freeze-dried powder of the pure juice of the roxburgh rose and the non-sterilizing freeze-dried powder of the pure juice of the roxburgh rose, respectively coding the sterilizing freeze-dried powder of the pure juice of the roxburgh rose into a number 1 and a number 2, and making the sterilizing freeze-dried powder and the non-sterilizing freeze-dried powder of the pure juice of the roxburgh rose into two parts in parallel.
3.2 measurement method
Pathogenic bacteria include Salmonella, shigella, and Staphylococcus aureus, as measured according to the method specified in GB/T4789.21.
3.3 measurement index
And respectively measuring microbial indexes of the non-bactericidal freeze-dried powder of the pure juice of the roxburgh rose and the bactericidal freeze-dried powder of the pure juice of the roxburgh rose, wherein pathogenic bacteria comprise salmonella, shigella and staphylococcus aureus.
4. Measurement results
The microbial determination results of the roxburgh rose pure juice sterilization freeze-dried powder and the roxburgh rose pure juice non-sterilization freeze-dried powder are shown in the following table 7.
TABLE 7
| Numbering device | Salmonella bacteria | Shigella bacteria | Staphylococcus aureus |
| 1 | Not detected | Not detected | Not detected |
| 2 | Detection of | Detection of | Detection of |
| 1′ | Not detected | Not detected | Not detected |
| 2′ | Detection of | Detection of | Detection of |
From the measurement results in the table 7, it is clear that all the roxburgh rose sterilization freeze-dried powder does not detect pathogenic bacteria, and all the non-sterilization roxburgh rose freeze-dried powder detects pathogenic bacteria, which indicates the importance of sterilization of the freeze-dried powder in the prior process. The fresh rosa roxburghii fruit can carry bacteria, and can be polluted in the processes of transferring, cleaning, juicing and filtering, so that the product can be used as food, and the quality and safety of the product can be ensured only by adopting a sterilization process to ensure that the product is free of pathogenic bacteria.
Experiment IV:
roxburgh rose freeze-dried powder and roxburgh rose biological agent deliquescence experiment
1. Experimental method
According to the methods of example 1, example 2 and example 3, coated tablets, uncoated tablets and granules of non-heat sterilization analytical dry products, namely, roxburgh rose freeze-dried powder and roxburgh rose biological freeze-dried preparation are respectively prepared.
And (3) respectively spreading the prepared roxburgh rose freeze-dried powder (non-thermal sterilization analysis dry product) and a proper amount of non-packaged roxburgh rose biological freeze-dried preparation coated tablets, non-coated tablets and granules, namely bare tablets on paper, placing for 30d in an environment with RH of 75% at room temperature, and observing the appearance condition of the tested product every 3 days. The test sample is melted and deformed and adhered to together are defined as easy moisture absorption (+ ++). The moisture and insoluble deformation of the test sample are more prone to moisture absorption (++); the test sample is slightly moist (+); the test article showed no change and was designated as (one).
2. Experimental results
Table 8 deliquescence experiment of Rosa roxburghii freeze-dried powder and Rosa roxburghii biological agent
| Sequence number | Observation time | Freeze-dried powder | Coated tablet | Non-coated tablets | Granule preparation | Remarks |
| 1 | Day 3 | + | - | - | - | - |
| 2 | Day 6 | ++ | - | - | - | - |
| 3 | Day 9 | +++ | - | - | - | - |
| 4 | Day 12 | Complete liquefaction | - | - | - | - |
| 5 | Day 15 | Complete liquefaction | - | - | - | - |
| 6 | Day 18 | Complete liquefaction | - | - | - | - |
| 7 | Day 21 | Complete liquefaction | - | - | - | - |
| 8 | Day 24 | Complete liquefaction | - | - | - | - |
| 9 | Day 27 | Complete liquefaction | - | - | - | - |
| 10 | Day 30 | Complete liquefaction | - | - | - | - |
As can be seen from table 8, the non-heat sterilized analytical dry product, i.e. the lyophilized powder, was slightly hygroscopic on day 3; moisture was absorbed on day 6, but no dissolution deformation; absorbing moisture on the 9 th day, dissolving, deforming and adhering together; complete liquefaction was achieved by day 12. While coated tablets, uncoated tablets, granules of the pear organism freeze-dried preparation did not see any change in appearance at day 30.
In industrial production, the non-thermal sterilization analysis drying product, namely the freeze-dried powder, is not subjected to subsequent mixing with proper auxiliary materials, and the granules are subjected to granulation, microencapsulation or tablet treatment by industrial process processes such as granulation, tabletting, coating and the like, so that the stability of the quality of the freeze-dried powder is difficult to ensure. The coated tablets, non-coated tablets and granules of the pear biological freeze-dried preparation are mixed with proper auxiliary materials in advance and are subjected to industrial process treatment such as granulation, microencapsulation, tabletting, coating and the like, and the moisture absorption prevention process treatment, so that the stability of the quality of the pear biological freeze-dried preparation is well ensured.
Experiment five:
determination of critical relative humidity of biological freeze-dried Rosa roxburghii preparation
1. Purpose of experiment
The critical relative humidity of the coated tablets, the uncoated tablets and the granules of the roxburgh rose biological freeze-dried preparation prepared by the technical scheme is measured so as to ensure the quality of the product.
2. Test article
Coated tablets, uncoated tablets and granules of the biological lyophilized preparations of Rosa roxburghii were prepared according to the methods of example 1, example 2 and example 3, respectively.
3. Experimental method
And (3) drying proper amounts of prepared roxburgh rose biological freeze-dried preparation coated tablets, uncoated tablets and granules respectively to constant weight, uniformly putting the coated tablets, the uncoated tablets and granules with the thickness of about 2mm at the bottom of a flat weighing bottle with constant weight respectively, accurately weighing, putting the coated tablets, the uncoated tablets and the granules into 8 supersaturated solutions of different RH% respectively, and weighing after keeping the temperature for 7 days at room temperature. Because ambient humidity greatly affects coated tablets, uncoated tablets and granules, the critical relative humidity of coated tablets, uncoated tablets and granules was determined for this purpose.
Preparing supersaturated solutions of different salts according to Table 9, respectively placing in a glass drier, standing at room temperature for 48 hours to balance the internal humidity to form environments with different relative humidity, placing 2 tablets of each of the sample coated tablet, the uncoated tablet and the granule dried to constant weight 1.20g and 1.00g in a constant weight flat weighing bottle, precisely weighing, opening a weighing bottle cap, placing in the drier with different humidity, absorbing moisture to constant weight at constant temperature, precisely weighing to calculate the moisture absorption rate, and measuring Critical Relative Humidity (CRH) in 2 parts in parallel, wherein the results are shown in tables 10, 11 and 12 and figures 2, 3 and 4 respectively.
TABLE 9 relative humidity at 25℃of saturated solutions of different salts
Table 10 critical relative humidity measurement data for coated tablets
| Number RH | 22.45 | 33.00 | 42.76 | 57.70 | 75.28 | 84.26 | 92.48 | 100.00 |
| Tablet weight (g) | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 |
| 1 moisture weight (g) | 0.00 | 0.01 | 0.03 | 0.07 | 0.22 | 0.43 | 0.74 | 0.96 |
| Water absorption (%) | 0.00 | 0.83 | 2.50 | 5.83 | 18.33 | 35.83 | 61.67 | 80.00 |
| Tablet weight (g) | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 |
| 2 weight of moisture (g) | 0.00 | 0.02 | 0.04 | 0.08 | 0.20 | 0.44 | 0.76 | 0.94 |
| Water absorption (%) | 0.00 | 1.67 | 3.33 | 6.67 | 16.67 | 36.67 | 63.33 | 78.33 |
| Average Water absorption (%) | 0.00 | 1.25 | 2.92 | 6.25 | 17.50 | 36.25 | 62.50 | 79.17 |
Table 11 critical relative humidity measurement data for uncoated tablets
| Number RH | 22.45 | 33.00 | 42.76 | 57.70 | 75.28 | 84.26 | 92.48 | 100.00 |
| Tablet weight (g) | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 |
| 1 moisture weight (g) | 0.00 | 0.02 | 0.04 | 0.08 | 0.23 | 0.44 | 0.76 | 1.00 |
| Water absorption (%) | 0.00 | 1.67 | 3.33 | 6.67 | 19.17 | 36.67 | 63.33 | 83.33 |
| Tablet weight (g) | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 |
| 2 weight of moisture (g) | 0.00 | 0.01 | 0.03 | 0.08 | 0.24 | 0.45 | 0.77 | 0.95 |
| Water absorption (%) | 0.00 | 0.83 | 2.50 | 6.67 | 20.00 | 37.50 | 64.17 | 79.17 |
| Average Water absorption (%) | 0.00 | 1.25 | 2.92 | 6.67 | 19.58 | 37.08 | 63.75 | 81.25 |
TABLE 12 Critical relative humidity determination data for granules
4. Analysis of results
The graph is drawn by taking the percentage% of moisture absorption or water absorption in tables 10, 11 and 12 as an ordinate and the relative humidity RH% as an abscissa, respectively, and the tangential lines at two ends of the graph in the drawing are the critical relative humidity, which is the abscissa corresponding to the intersection point of the two tangential lines, so as to obtain the graph of fig. 2, 3 and 4. From the experimental items, the critical relative humidity CRH of the coated tablet, the uncoated tablet and the granule of the roxburgh rose biological freeze-dried preparation is 74.92%, 72.41% and 72.37%, namely, the environmental humidity is controlled below 72% and 74% when the coated tablet, the uncoated tablet and the granule of the roxburgh rose biological freeze-dried preparation are packaged, stored and transported, so as to reduce the influence of moisture on the properties and stability of the coated tablet, the uncoated tablet and the granule of the roxburgh rose biological freeze-dried preparation.
From the above experiments, the critical relative humidity CRH of the coated tablet, the uncoated tablet and the granule of the roxburgh rose biological freeze-dried preparation is 74.92%, 72.41% and 72.37%, respectively, which is just the critical relative humidity of the coated tablet, the uncoated tablet and the granule in the case of bare tablets, for example, the critical relative humidity of the coated tablet, the uncoated tablet is higher after the coated tablet and the uncoated tablet are packaged in an aluminum-plastic blister package, or in a sterile bag, or in a bottle and the granule are packaged in a sterile way, and the shelf life is longer, so that the stability of the product is ensured.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (8)
1. The preparation method of the roxburgh rose biological freeze-dried preparation is characterized by comprising the following steps:
(1) Pretreatment: cleaning fresh fructus Rosae Normalis, and air drying to remove surface water;
(2) Juice squeezing: sending the fresh rosa roxburghii fruit processed in the step (1) into a juicer for juicing, and filtering and deslagging twice to obtain rosa roxburghii pure juice;
(3) Non-heat sterilization treatment: sealing the pure Rosa roxburghii juice obtained in the step (2) by using a large-package plastic bag or a plastic bottle, then sending the plastic bag or the plastic bottle filled with the pure Rosa roxburghii juice into a high-pressure cabin of an ultrahigh-pressure container, adding a medium, then sealing the high-pressure cabin, applying pressure to the ultrahigh-pressure container, maintaining pressure and sterilizing to obtain sterile pure Rosa roxburghii juice;
(4) Cleaning and sterilizing the large package: the sterile Rosa roxburghii pure juice large package in the step (3) is conveyed to a sterile environment through a clean air curtain for cleaning, disinfection and sterilization; the large package is a plastic flexible package or a plastic bottle for filling;
(5) Quick freezing: under the aseptic environment, unpacking the large package cleaned and sterilized in the step (4), sub-packaging the sterile roxburgh rose pure juice into a bracket layered tray, and sending the bracket layered tray into a quick-freezing warehouse or a freeze dryer for quick freezing to obtain frozen roxburgh rose pure juice;
(6) Vacuum sublimation drying: the frozen roxburgh rose pure juice bracket layered tray in the step (5) is sent into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and a frozen and dried roxburgh rose pure juice freeze-dried product after sterilization, namely a vacuum sublimation dried product is obtained;
(7) Vacuum analysis and drying: collecting the vacuum sublimated and dried product, respectively loading the product and auxiliary materials into a bracket layered tray together, conveying the bracket layered tray into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimated and dried product and auxiliary materials to obtain a vacuum analysis dried product and dried auxiliary materials;
(8) Mixing: stirring, mixing and homogenizing the vacuum analysis dried product and the drying auxiliary materials at a certain rotating speed according to the weight part ratio, and preparing tablets, granules, powder or capsules according to actual conditions to obtain the roxburgh rose biological freeze-dried preparation;
in the step (3), the medium is water or high-grade hydraulic oil; when the medium in the ultrahigh pressure container is water, applying 400-600 MPa pressure to the pure juice of the roxburgh rose packaged in the plastic bag or the plastic bottle, and keeping the pressure for 5-15 min; when the medium in the ultrahigh pressure container is high-grade hydraulic oil, applying 100-1000 MPa to the pure juice of the roxburgh rose packaged in the plastic bag or the plastic bottle; the dwell time is 1-30 min.
2. The method for preparing the biological freeze-dried preparation of roxburgh rose according to claim 1, which is characterized in that: the granule is prepared by granulating, microencapsulating and aseptically packaging the mixture; the tablet is prepared by granulating, tabletting, coating, and packaging with aluminum-plastic bubble cap or sterile bag or bottle.
3. The method for preparing the biological freeze-dried preparation of roxburgh rose according to claim 1, which is characterized in that: in the step (2), the filter screen for the first filtering is 200-300 meshes, and the filter screen for the second filtering is 400-800 meshes.
4. The method for preparing the biological freeze-dried preparation of roxburgh rose according to claim 1, which is characterized in that: in the step (5), the rapid freezing temperature is-30 to-40 ℃.
5. The method for preparing the biological freeze-dried preparation of roxburgh rose according to claim 1, which is characterized in that: in the step (6), the vacuum degree of vacuum sublimation drying is 30-150 pa, the temperature is 30-40 ℃, and the water content of the vacuum sublimation drying product is 10+/-2%.
6. The method for preparing the biological freeze-dried preparation of roxburgh rose according to claim 1, which is characterized in that: in the step (7), the vacuum degree of vacuum analysis drying is 5-30 pa, the temperature is 40-60 ℃, the relative air humidity is 20-40%, and the water content of the vacuum analysis drying product is 5+/-2%; the auxiliary materials are mixed auxiliary materials prepared by mixing microcrystalline cellulose, micro powder silica gel and dextrin according to the mass ratio of = (0.3-0.4): (0.2-0.4), and the mass ratio of the three auxiliary materials is added to be 1.
7. The method for preparing the biological freeze-dried preparation of roxburgh rose according to claim 1, which is characterized in that: in the step (8), the mass ratio of the vacuum analysis dried product to the drying auxiliary material is=1:x, and x is less than or equal to 1; the rotating speed is 500-600 r/min.
8. The method for preparing the biological freeze-dried preparation of roxburgh rose according to claim 1, which is characterized in that: the content of VC in the roxburgh rose biological freeze-dried preparation is more than or equal to 30mg/g, the content of SOD biological activity is more than or equal to 20000-50000 u/g, and the content of flavone is more than or equal to 4mg/g; pathogenic bacteria, namely salmonella, shigella and staphylococcus aureus, are not detected in the roxburgh rose biological freeze-dried preparation; the critical relative humidity of the roxburgh rose biological freeze-dried preparation is more than or equal to 70 percent.
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| CN105360277A (en) * | 2015-12-03 | 2016-03-02 | 贵州华南理工生物工程有限公司 | Superhigh-pressure fresh keeping method for fresh rosa roxburghii |
| CN106036604A (en) * | 2016-05-26 | 2016-10-26 | 安顺职业技术学院 | Vacuum freeze-drying processing technology of rosa sterilis fruits |
| CN107535787A (en) * | 2016-06-23 | 2018-01-05 | 上海蓝王医药科技发展有限公司 | A kind of Rosa roxburghii freezes the preparation method of particle |
| CN110140909A (en) * | 2019-05-30 | 2019-08-20 | 重庆康菌泰生物科技股份有限公司 | A kind of Rosa roxburghii Tratt comprehensive enzyme and preparation method thereof |
| CN111265657A (en) * | 2020-02-26 | 2020-06-12 | 中国农业大学 | Superoxide dismutase solid preparation and preparation method thereof |
| CN112006191A (en) * | 2020-07-27 | 2020-12-01 | 遵义师范学院 | Roxburgh rose fruit juice beverage and preparation method thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105360277A (en) * | 2015-12-03 | 2016-03-02 | 贵州华南理工生物工程有限公司 | Superhigh-pressure fresh keeping method for fresh rosa roxburghii |
| CN106036604A (en) * | 2016-05-26 | 2016-10-26 | 安顺职业技术学院 | Vacuum freeze-drying processing technology of rosa sterilis fruits |
| CN107535787A (en) * | 2016-06-23 | 2018-01-05 | 上海蓝王医药科技发展有限公司 | A kind of Rosa roxburghii freezes the preparation method of particle |
| CN110140909A (en) * | 2019-05-30 | 2019-08-20 | 重庆康菌泰生物科技股份有限公司 | A kind of Rosa roxburghii Tratt comprehensive enzyme and preparation method thereof |
| CN111265657A (en) * | 2020-02-26 | 2020-06-12 | 中国农业大学 | Superoxide dismutase solid preparation and preparation method thereof |
| CN112006191A (en) * | 2020-07-27 | 2020-12-01 | 遵义师范学院 | Roxburgh rose fruit juice beverage and preparation method thereof |
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