CN114794473A - Preparation method of oriental cherry pollen with activity of inhibiting AGE generation - Google Patents

Preparation method of oriental cherry pollen with activity of inhibiting AGE generation Download PDF

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CN114794473A
CN114794473A CN202210450428.0A CN202210450428A CN114794473A CN 114794473 A CN114794473 A CN 114794473A CN 202210450428 A CN202210450428 A CN 202210450428A CN 114794473 A CN114794473 A CN 114794473A
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cherry
temperature
activity
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extraction
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余斌
陆依秋
汪宣鹏
李景健
于婧
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Guangdong Qingyunshan Pharmaceutical Co ltd
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Guangdong Qingyunshan Pharmaceutical Co ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/16Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by heating loose unpacked materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D2011/002Counter-current extraction

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  • Chemical & Material Sciences (AREA)
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Abstract

The invention discloses a preparation method of oriental cherry powder with activity of inhibiting AGE generation, which comprises low-temperature processes of cleaning, countercurrent extraction, filtering, concentration, sterilization, freeze drying, sieving and the like. Combines countercurrent extraction and low-temperature membrane treatment for extraction of oriental cherry, adopts whole low-temperature process and full-closed intensive continuous production, the contents of total flavone, caffeoylglucose (1-O-caffeoyl-beta-D-glucopyranoside) and quercetin glucoside (quercetin-3-O-beta-D-glucopyranoside) contained in the cherry blossom are fully reserved, separated and enriched, active ingredients are fully extracted, the transfer rate is high, the yield of the active ingredients of the prepared cherry blossom powder is high, and the cherry blossom powder prepared by the method has obvious activity of inhibiting AGE generation by adopting a green film material, is high in safety and effectively enriches active ingredients, the AGE generation inhibition rate reaches 58% (when the concentration is 100 mu g/ml), and the IC50 reaches 67 mu g/ml.

Description

Preparation method of oriental cherry pollen with activity of inhibiting AGE generation
Technical Field
The invention belongs to the technical field of plant extraction and production, and particularly relates to a preparation method of oriental cherry powder with activity of inhibiting AGE generation.
Background
In the area of the northern hemisphere temperate zone with the clitocybe villosa native to oriental cherries, the cherries grow all over the world, 3 to 5 flowers are grown on each branch to form an umbrella-shaped inflorescence, the tips of petals are carved, and the flower colors are mostly white and pink. Usually in 3 months, the flowers are placed together with the leaves or bloom after the leaves, and the color of the cherry blossom is faint, fragrant and beautiful with the change of seasons, and is commonly used for ornamental in gardens. The cherry blossom can be divided into a single petal type and a multiple petal type, wherein the single petal type can blossom and bear fruits, and the multiple petal type can not bear fruits for the most part.
According to the examination of literature data, cherry blossom is cultivated in the aster of China in the Qin and Han period more than two thousand years ago. Oriental cherry has been commonly found in private courtyards in Tang dynasty. In the world of Japan, the pilgrimage of Japan brought the cherry blossom back to the Ying, which had been in Japan for over 1000 years. Cherry blossom is indicative of intense heat, purity and fashion. The quilt is distinguished as a Japanese flower, the flowering cherry blooms in four and five months each year, the flowers are brocade, the visitors weave as well as the Wanjia empty lane, and the quilt is one of the great festivals of the Japanese people.
The main active ingredients in the cherry blossom are flavone compounds such as cherry blossom extract, astragalin, isoquercitrin, cyanidin-3-glucoside, cyanidin-3-rutinoside, prunetin, genistein, quercetin, prunetin-4' -0-3-glucopyranoside, kaempferol-3-O-arabinofuranoside, kaempferol-3-O-beta-xyloside, genistin, kaempferol-3-O-glucoside and the like, and the cherry blossom extract has the effects of oxidation resistance, inflammation resistance, cancer resistance, whitening and the like and can be used as a potential cosmetic active ingredient. In addition, the oriental cherry also contains polysaccharide and organic acid, is rich in natural vitamin A, B, E, and has good effects of shrinking pores, strengthening mucous membrane, promoting sugar metabolism and balancing oil. Wherein caffeoylglucose (1-O-caffeoyl-beta-D-glucopyranoside) and quercetin-glucoside (quercetin-3-O-beta-D-glucopyranoside) are used as main functional components.
In 2021, 8 and 17 months, the national food safety risk assessment center issued "public request for new food material of Rosa kansuensis flower" and stipulated that the source thereof is the flower of Rosa kansuensis of Rosaceae, genus Prunus. Before that, the illegal use of cherry blossom as common food appears in China, the illegal use report of cherry blossom appears in the market, and the recording of cherry blossom as a new food raw material is proposed but never passed. Therefore, the oriental cherry in the domestic market is used for various products in the form of essence and spice at present, and the related reports of oriental cherry with common food as the visual angle are few, so that the research on the efficacy and the material basis is more insufficient. With the increasing use of the cherries in the future as common food, the development of functional food of the cherries will become hot, and the preparation and industrial production of green, safe, high-quality and effective cherry powder are urgent.
Advanced Glycation End products (AGEs) are excess sugar and protein-bound products that can combine with and destroy tissue cells of the body. The research proves that: AGEs accelerate aging in humans and cause many chronic degenerative diseases such as diabetes, alzheimer's disease, atherosclerosis, and the like. Inhibiting the production of AGEs can have anti-aging and prophylactic effects on various chronic degenerative diseases. Therefore, the research of AGEs becomes one of the most popular fields in the global medical field, and a plurality of scientific research institutions, universities, hospitals and pharmaceutical companies join the research of AGEs in various lines. The oriental cherry and the flavonoid compounds thereof have obvious activity of inhibiting AGEs generation, but related functional products in China still leave a blank. Therefore, the cherry pollen with the activity of inhibiting AGE generation has wide application prospect.
The development of cherry blossom has been reported, but most researches are on cultivation and raw material processing, and the extraction process and efficacy of the cherry blossom extract are not reported much:
the invention patent publication No. CN102883733B discloses an AGE formation inhibitor, which is obtained by extracting with alcohol and purifying with porous synthetic resin to obtain extract of flower and/or leaf of cherry rich in flavonoids, and has been studied and elucidated in the aspects of AGE formation inhibition activity, apoptosis inhibition activity, fibroblast collagen mesh promotion activity, and skin aging improvement activity. Although the content of flavonoids obtained by the preparation method is high, the organic solvent ethanol and the porous synthetic resin are used, so that the safety risk exists, the preparation method is not approved in the field of food, and a large amount of waste liquid is generated in the preparation process, so that the preparation cost is further increased.
The invention patent with publication number CN113633589A discloses a cherry flower extract extraction process for cherry flower moisturizing conditioner, which adopts the methods of cleaning, crushing, squeezing, alcohol precipitation and ultrafiltration to prepare the cherry flower extract. Although the method is simple, the method also uses an organic solvent ethanol, and does not carry out innovative analysis and research on the functional components or the activity of the product.
The invention patent with publication number CN112206191A discloses a cherry blossom extract and an extraction method and application thereof, wherein in the extraction method, an extractant comprises a composition of C3-C6 micromolecule polyalcohol, ethanol and water; the hair-blackening function of the extract is elucidated. Because the polyhydric alcohol is introduced in the process, the activity and the stability of the active ingredients in the oriental cherry flower extract are kept, and the C3-C6 micromolecule polyhydric alcohol has good water locking and moisturizing functions and is suitable for hair conditioners, but the C3-C6 micromolecule polyhydric alcohol and the ethanol are used, so that the preparation method is not suitable for producing foods.
The invention patent with publication number CN113813203A discloses a cherry blossom enzymolysis zymolyte and a preparation method and application thereof, the preparation method uses enzyme liquid of aspergillus oryzae and aspergillus niger to carry out enzymolysis pretreatment on cherry blossom/jasmine flower, and then prepares a cherry blossom extract in a mode of fermenting the cherry blossom/jasmine flower by specific lactic acid bacteria and saccharomycetes.
Because the types of chemical components in the oriental cherry are complex, the processing method is various, and besides the methods, the processing method also comprises supercritical solvent extraction, molecular distillation, silica gel column chromatography, organic solvent extraction, ion exchange purification and the like. These methods either present safety risks and are not recognized in the food field; or the industrial cost is high, and the industrial production is not suitable; or the characteristic flavor of the product is lost and the stability is poor; or the content of the functional components is not high, and the transfer rate is insufficient; or lack of efficacy verification.
The industrial production of food oriental cherry powder is still blank, the related requirements are more urgent, the preparation of oriental cherry powder with activity of inhibiting AGE generation has wide application prospect, and on the other hand, in order to meet the requirements of food safety standard, the requirements of young consumption market and the modern industrial production requirements, a safer, greener, higher-quality and simpler industrial production method needs to be developed, and the obtained product can be used for functional foods such as beverages (including soft drinks), solid beverages, conventional tablets, capsules and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of safe green cherry powder with low cost, good flavor maintenance, simple and convenient production process and high yield of effective components for inhibiting AGE generation activity, thereby overcoming the problems of high industrial production cost, loss of flavor characteristics, complicated and uncomfortable industrial production, low content yield of active components and the like caused by adopting column chromatography and extraction method for separating and purifying the cherry extract at present.
In order to solve the above-mentioned problems, the present invention provides a method for preparing oriental cherry powder having activity of inhibiting AGE formation, comprising the steps of:
s1: cleaning, namely cleaning the cherry petals to obtain a cherry raw material;
preferably, the petals are crushed after cleaning so as to be more sufficient for subsequent extraction, and preferably, a traditional Chinese medicine crusher with a sieve mesh aperture of 20mm is adopted for crushing.
The cleaning is preferably performed by a traditional Chinese medicine cleaning machine.
S2: performing countercurrent extraction, namely putting the oriental cherry raw material into a continuous countercurrent extractor for extraction to obtain an extracting solution;
the technological conditions of the countercurrent extraction are as follows: the feeding speed is 180-220 kg/h, and the flow rate of the softened water injected into the extraction solvent is 1.0-1.4 m 3 The rotation speed of a rotating shaft of the extractor is 10-15 r/h, the total amount of the added solvent is 5-10 times of the weight of cherry blossom, so that the solvent fully immerses the materials, and the extraction temperature is controlled to be 10-50 DEG C;
The preferred extraction temperature is 38-42 ℃, the extraction effect is good, the yield is high, and the structure of effective components is not damaged;
the equipment comprises a medicinal material quantitative material conveying and controlling system, an extracted solvent flow and temperature controlling system, a herb residue separating and tunnel type drying processing system, an extracted liquid medicine residue-liquid separating system, an extracted tube section stirring system, an extracted tube section heating and heat preserving system, a online cleaning (WIP) system, a centralized electrical operation control system and the like, realizes continuous full-closed operation and dynamic countercurrent extraction on the basis of keeping the traditional extracting functions of traditional high-temperature decoction, thermal reflux, normal-low temperature percolation and the like, improves the production efficiency, lightens the labor intensity, reduces the solvent consumption, reduces the production cost, ensures the safety of the production process and avoids the pollution problem of herb residues to the environment.
S3: filtering, namely sequentially filtering the extracting solution by using a first filter bag of 38-180 mu m, a second filter bag of 1-10 mu m, a filtering membrane of 100-200 nm, a first ultrafiltration membrane of 2-5 WDa and a second ultrafiltration membrane of 1-5 KDa to form trapped solution;
wherein the first ultrafiltration membrane is preferably 4-5 WDa, and the loss of active ingredients is less; the second ultrafiltration membrane is preferably 2-4 KDa, and more active ingredients are reserved;
the filtering membrane is preferably a ceramic membrane, and ceramic membrane equipment is used; the first filter bag and the second filter bag are arranged in the pipeline filter for filtering.
S4: concentrating the trapped fluid by using a reverse osmosis membrane or a nanofiltration membrane until the relative density is 1.04-1.10 to form concentrated fluid;
preferably, the concentration is carried out until the relative density is 1.06-1.08, and in the range, the concentration speed is high, the efficiency is higher, and meanwhile, the concentrated solution is more beneficial to subsequent drying.
S5: sterilizing, namely sterilizing the concentrated solution;
preferably, an UHT (ultra high temperature) instantaneous sterilizer is adopted for sterilization, the sterilization temperature is 115-135 ℃, the sterilization time is 5-50 s, and the sterilized feed liquid is rapidly cooled to the room temperature, so that the active ingredients are prevented from being pyrolyzed;
the optimal sterilization temperature is 120-125 ℃, the optimal sterilization time is 35s, the sterilization effect is good, and the cooling is fast.
S6: freeze drying, sterilizing, placing the feed liquid into tray via tray separator, and freeze drying in freeze dryer to obtain dry extract;
wherein, the freeze drying process comprises the following steps:
s61: pre-freezing, and keeping the temperature at-55 to-30 ℃ for 2 to 6 hours at normal pressure;
s62: sublimation drying, raising the temperature from minus 55 to minus 30 ℃ to minus 25 to minus 15 ℃ at a constant speed in vacuum of 0 to 45Pa for 30 to 180min, and preserving the temperature for 2 to 7 hours; then under the vacuum of 0-45 Pa, the temperature is increased from minus 25 to minus 15 ℃ to minus 15 to minus 5 ℃ at a constant speed for 30-180 min, and the temperature is kept for 5-12 h;
s63: and (3) resolving and drying, raising the temperature from minus 15 to minus 5 ℃ to 30 to 55 ℃ at a constant speed for 30 to 240min under the vacuum of 5 to 50pa, and preserving the temperature for 3 to 9 hours.
S7: sieving, sieving the dry extract with a swing granulator, and collecting the sieved granule and fine powder to obtain oriental cherry powder;
a sieve with the size of 180-550 mu m is adopted in the swing granulator, and a sieve with the size of 250 mu m is preferably adopted.
Preferably, the continuous countercurrent extractor, the pipeline filter, the ceramic membrane equipment, the ultrafiltration membrane equipment, the reverse osmosis membrane equipment, the UHT sterilization equipment and the freeze dryer used in the above steps are all connected by closed pipelines, so that the fully-closed intensive continuous production is realized, and the quality and the safety of the product are ensured to the maximum extent.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method combines countercurrent extraction and low-temperature membrane treatment for extraction of cherry blossom, fully retains and separates and enriches the contents of total flavone, caffeoyl glucose (1-O-caffeoyl-beta-D-glucopyranoside) and quercetin glucoside (quercetin-3-O-beta-D-glucopyranoside) in the cherry blossom by low-temperature process (low-temperature extraction, low-temperature separation and purification, low-temperature concentration and low-temperature drying), fully extracts active ingredients, has high transfer rate, high yield of the prepared cherry blossom powder active ingredients, adopts green membrane material, has high safety, effectively enriches the active ingredients, ensures that the content of the total flavone exceeds 15 percent, the transfer rate exceeds 80 percent and the content of the caffeoyl glucose (1-O-caffeoyl-beta-D-glucopyranoside) exceeds 8 percent, the transfer rate exceeds 82%, the content of quercetin glucoside (quercetin-3-O-beta-D-glucopyranoside) exceeds 0.6%, and the transfer rate exceeds 85%. The cherry pollen prepared by the invention has obvious effect of inhibiting AGE generation activity, the AGE generation inhibition rate reaches 58% (when the concentration is 100 mug/ml), IC50 reaches 67 mug/ml, and the activity is superior to aminoguanidine hydrochloride (positive) and similar products in the market.
(2) The process is suitable for industrial production, the production intensification and automation degree are high, the special line continuous production of the closed pipeline is realized, the product safety is high, and meanwhile, the process is simple, the integration degree is high, the operation is easy, and the production cost is low.
(3) The quality of the prepared cherry pollen is in accordance with and far higher than the national food safety standard GB/T29602, the product is instant, the aqueous solution is clear and transparent, the flavor is kept excellent, and the dissolving speed and the flavor are obviously superior to those of common similar products; and the stability of the aqueous solution is high, which is obviously superior to the like products, and the aqueous solution can be used for functional foods, such as beverages (including soft drinks), solid beverages, conventional tablets, capsules and other various formulations.
(4) UHT ultrahigh temperature instantaneous sterilization is adopted, and then rapid cooling is carried out, so that the oxidative degradation of active ingredients is reduced while the microbial biomass is effectively controlled.
For a more convenient understanding of the patent technology, the explanation of some technical terms appearing in the process is now written as follows:
softened water is natural water containing only a small amount of soluble magnesium salt and calcium salt, and may be referred to as hard water subjected to softening treatment, soft water: 0-60 ppm. Application area of softened water: water supply for bathroom, kitchen, clothes washing, heating, boiler, central air-conditioning equipment, etc.
Countercurrent extraction means that during the extraction, the material and the solvent continuously move at the same time, but the moving directions are opposite.
Da, called Dalton (Dalton), is a unit commonly used for molecular weight, which is the algebraic sum of all atoms in a molecule by number of atomic weights, and is a unit used to measure the mass of an atom or molecule, and is defined as 1/12 for carbon 12 atomic mass, and proteins are large molecules and are therefore commonly represented in kDa (kilodalton).
Nanofiltration membrane with pore diameter of 1nm or more, typically 1-2 nm. Is a functional semi-permeable membrane that allows the passage of solvent molecules or certain low molecular weight solutes or low valent ions. It is a particular and promising type of separation membrane, which is named for the fact that it can retain substances of about nanometer size. Is used for removing organic matters and chromaticity of surface water, removing hardness of underground water, partially removing soluble salt, concentrating fruit juice, separating useful substances in medicines, and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings which are required to be used in the embodiments or the technical solutions in the prior art will be briefly described below.
FIG. 1 is a bar graph showing AGEs production inhibition ratios of cherry pollen prepared in examples of the present invention and comparative examples.
Detailed Description
In order to make the technical means, the original characteristics, the achieved purposes and the effects of the invention easily understood and obvious, the technical solutions in the embodiments of the present invention are clearly and completely described below to further illustrate the invention, and obviously, the described embodiments are only a part of the embodiments of the present invention, but not all the embodiments.
Example 1
S1: cleaning, namely taking 1000kg of cherry blossom petals, placing the cherry blossom petals in a traditional Chinese medicine cleaning machine (equipment model XY-500) for cleaning, placing cleaned cherry blossom raw materials in a traditional Chinese medicine crusher for coarse crushing, wherein the sieve mesh diameter is 20mm, and collecting the coarse crushed raw materials for later use.
S2: countercurrent extraction, immediately feeding the coarsely crushed oriental cherry raw material into a continuous countercurrent extractor, controlling the feeding speed at 200kg/h, starting to inject softened water, and controlling the flow rate of the softened water at 1.2m 3 The rotating speed of the rotating shaft of the extractor is 12r/h, so that the softened water fully immerses the materials, and the raw material extracting solution initially fed is nearly colorless and softThe total adding amount of the water is 7000L, the heater is turned on during the period, the temperature of the material liquid is controlled at 40 ℃, and the extracting solution is collected.
S3: and (3) filtering, namely filtering the extracting solution by a first filter bag with the diameter of 150 microns, flowing the filtrate into a pipeline filter with a built-in second filter bag with the diameter of 5 microns through a closed pipeline, filtering the filtrate by ceramic membrane equipment (equipment model KM1030-CM-122) with a built-in ceramic filter membrane with the diameter of 200nm, filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in first ultrafiltration membrane of 5WDa, and finally filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in second ultrafiltration membrane of 3KDa to obtain trapped fluid.
S4: concentrating the retentate with reverse osmosis membrane equipment (equipment model KM8040-NF-G16), and concentrating to relative density of 1.07 to obtain concentrated solution.
S5: sterilizing, sterilizing the concentrated solution with UHT ultra high temperature instant sterilizer at 125 deg.C for 35s, and rapidly cooling to room temperature.
S6: freeze drying, sterilizing, loading into tray, and freeze drying in freeze dryer to obtain dry extract. The freeze drying process comprises the following steps:
Figure BDA0003618360840000091
s7: sieving, collecting dried extract, sieving with a sieve having a mesh size of 250 μm in a swing granulator, and collecting sieved granule and fine powder to obtain oriental cherry powder.
In each process, the continuous production is carried out by adopting a special closed pipeline, the operation is easy, and the product safety is high.
The experimental detection is carried out on the prepared cherry blossom powder, the content of each effective component in the active ingredients is shown in table 1, the comparison of AGEs generation inhibition rate is shown in table 2, and the sense and dissolution conditions are shown in table 3:
a) average dry powder yield: 28.3 percent;
b) average total flavone content: 16.8 percent and the transfer rate of effective components is 84.3 percent;
c) average caffeoyl glucose content: 8.1 percent and the transfer rate of effective components is 78.2 percent;
d) average quercetin glucoside content: 0.83 percent and the transfer rate of effective components is 90.0 percent;
the finished product has pure color, aroma and taste, can be quickly dissolved in an aqueous solution, is clear and transparent and has good stability.
Example 2
S1: cleaning, namely taking 1000kg of cherry petals, putting the cherry petals into a traditional Chinese medicine cleaning machine (equipment model XY-500) for cleaning, and collecting cherry raw materials for later use.
S2: countercurrent extraction, immediately feeding cleaned oriental cherry raw material into continuous countercurrent extractor, controlling feeding speed at 190kg/h, starting to inject softened water, and controlling softened water flow rate at 1.3m 3 And h, rotating the rotating shaft of the extractor at a speed of 14r/h to ensure that the softened water fully immerses the materials, the raw material extracting solution fed initially is nearly colorless, the total adding amount of the softened water is about 6000L, the temperature of the material liquid is controlled to be 45 ℃ by starting a heater during the period, and the extracting solution is collected.
S3: and (3) filtering, namely filtering the extracting solution by a first filter bag with the diameter of 75 micrometers, flowing the filtrate into a pipeline filter with a second filter bag with the diameter of 1 micrometer through a closed pipeline, filtering the filtrate by ceramic membrane equipment (equipment model KM1030-CM-122) with a built-in 100nm ceramic filter membrane, filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in 3WDa first ultrafiltration membrane, and filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in 3KDa second ultrafiltration membrane to obtain trapped fluid.
S4: concentrating the trapped fluid by reverse osmosis membrane equipment (equipment model KM8040-NF-G16), and concentrating to relative density of 1.05 to obtain concentrated solution.
S5: sterilizing, namely sterilizing the concentrated solution by using an UHT ultrahigh temperature instant sterilizer at the sterilization temperature of 130 ℃ for 20s, and quickly cooling the sterilized feed liquid to room temperature.
S6: freeze drying, sterilizing, loading into tray, and freeze drying in freeze dryer to obtain dry extract. The freeze drying process comprises the following steps:
Figure BDA0003618360840000101
s7: sieving, collecting dried extract, sieving with a sieve having a pore size of 380 μm in a swing granulator, and collecting sieved granule and fine powder to obtain oriental cherry powder.
In each process, the continuous production is carried out by adopting a special closed pipeline, the operation is easy, and the product safety is high.
The experimental detection is carried out on the prepared cherry blossom powder, the content of each effective component in the active ingredients is shown in table 1, the comparison of AGEs generation inhibition rate is shown in table 2, and the sense and dissolution conditions are shown in table 3:
a) average dry powder yield: 29.6 percent;
b) average total flavone content: 16.3 percent and the transfer rate of effective components is 85.5 percent;
c) average caffeoyl glucose content: 7.9 percent and the transfer rate of effective components is 79.8 percent;
d) average quercetin glucoside content: 0.80 percent and the transfer rate of effective components is 90.7 percent;
the finished product has pure color, aroma and taste, can be quickly dissolved in an aqueous solution, is clear and transparent and has good stability.
Example 3
S1: cleaning, namely taking 1000kg of cherry petals, putting the cherry petals into a traditional Chinese medicine cleaning machine (equipment model XY-500) for cleaning, and collecting cherry raw materials for later use.
S2: countercurrent extraction, immediately feeding cleaned oriental cherry raw material into continuous countercurrent extractor, controlling feeding speed at 210kg/h, starting to inject softened water, and controlling softened water flow rate at 1.1m 3 And h, rotating the rotating shaft of the extractor at a speed of 11r/h to ensure that the softened water fully immerses the materials, the raw material extracting solution fed initially is nearly colorless, the total adding amount of the softened water is about 9000L, the temperature of the material liquid is controlled to be 30 ℃ by starting a heater during the period, and the extracting solution is collected.
S3: and (3) filtering the extracting solution, namely filtering the extracting solution by a first filter bag with the diameter of 48 mu m, flowing the filtrate into a pipeline filter with a built-in second filter bag with the diameter of 5 mu m through a closed pipeline, filtering the filtrate by ceramic membrane equipment (equipment model KM1030-CM-122) with a built-in 200nm ceramic filter membrane, filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in first 2WDa ultrafiltration membrane, and filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in second 2KDa ultrafiltration membrane to obtain trapped fluid.
S4: concentrating the retentate with reverse osmosis membrane equipment (equipment model KM8040-NF-G16), and concentrating to relative density of 1.09 to obtain concentrated solution.
S5: sterilizing, sterilizing the concentrated solution with UHT ultra high temperature instant sterilizer at 120 deg.C for 10s, and rapidly cooling to room temperature.
S6: freeze drying, sterilizing, placing the feed liquid into tray via tray separator, and freeze drying in freeze dryer to obtain dry extract; wherein, the freeze drying process comprises the following steps:
Figure BDA0003618360840000121
s7: sieving, collecting dried extract, sieving with a sieve having aperture of 325 μm in a swing granulator, and collecting sieved granule and fine powder to obtain oriental cherry powder.
In each process, the continuous production is carried out by adopting a special closed pipeline, the operation is easy, and the product safety is high.
The experimental detection is carried out on the prepared cherry blossom powder, the content of each effective component in the active ingredients is shown in table 1, the comparison of AGEs generation inhibition rate is shown in table 2, and the sense and dissolution conditions are shown in table 3:
a) average dry powder yield: 27.7 percent;
b) average total flavone content: 16.7 percent and the transfer rate of effective components is 82.0 percent;
c) average caffeoyl glucose content: 8.2 percent and the transfer rate of effective components is 77.5 percent;
d) average quercetin glucoside content: 0.84 percent and the transfer rate of effective components is 89.1 percent;
the finished product has pure color, aroma and taste, can be quickly dissolved in an aqueous solution, is clear and transparent and has good stability.
Example 4
S1: cleaning, namely taking 1000kg of cherry petals, putting the cherry petals into a traditional Chinese medicine cleaning machine (equipment model XY-500) for cleaning, and collecting cherry raw materials for later use.
S2: countercurrent extraction, immediately feeding cleaned oriental cherry raw material into continuous countercurrent extractor, controlling feeding speed at 220kg/h, starting to inject softened water, and controlling softened water flow rate at 1.0m 3 And h, rotating the rotating shaft of the extractor at a speed of 15r/h to ensure that the softened water fully immerses the materials, the raw material extracting solution fed initially is nearly colorless, the total adding amount of the softened water is about 5000L, the heater is started during the period to control the temperature of the material liquid to be 10 ℃, and the extracting solution is collected.
S3: and (2) filtering the extracting solution, namely filtering the extracting solution by a first filter bag with the diameter of 180 mu m, flowing the filtrate into a pipeline filter with a built-in second filter bag with the diameter of 10 mu m through a closed pipeline, filtering the filtrate by ceramic membrane equipment (equipment model KM1030-CM-122) with a built-in ceramic filter membrane with the diameter of 200nm, filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in first 5WDa ultrafiltration membrane, and filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in second 5KDa ultrafiltration membrane to obtain trapped solution.
S4: concentrating the retentate with reverse osmosis membrane equipment (equipment model KM8040-NF-G16), and concentrating to relative density of 1.10 to obtain concentrated solution.
S5: sterilizing, sterilizing the concentrated solution with UHT ultra high temperature instant sterilizer at 135 deg.C for 50s, and cooling the sterilized solution to room temperature.
S6: freeze drying, sterilizing, placing the feed liquid into tray via tray separator, and freeze drying in freeze dryer to obtain dry extract; wherein, the freeze drying process comprises the following steps:
Figure BDA0003618360840000131
s7: sieving, collecting dried extract, sieving with a sieve having a pore size of 550 μm in a swing granulator, and collecting sieved granule and fine powder to obtain oriental cherry powder.
In each process, the continuous production is carried out by adopting a special closed pipeline, the operation is easy, and the product safety is high.
The experimental detection is carried out on the prepared cherry blossom powder, the content of each effective component in the active ingredients is shown in table 1, the comparison of AGEs generation inhibition rate is shown in table 2, and the sense and dissolution conditions are shown in table 3:
a) average dry powder yield: 25.4 percent;
b) average total flavone content: 16.5 percent and the transfer rate of effective components is 74.3 percent;
c) average caffeoyl glucose content: 8.0 percent and the transfer rate of effective components is 69.4 percent;
d) average quercetin glucoside content: 0.78 percent and the transfer rate of effective components is 75.9 percent;
the finished product has pure color, aroma and taste, can be quickly dissolved in an aqueous solution, is clear and transparent and has good stability.
Example 5
S1: cleaning, namely taking 1000kg of cherry petals, putting the cherry petals into a traditional Chinese medicine cleaning machine (equipment model XY-500) for cleaning, and collecting cherry raw materials for later use.
S2: countercurrent extraction, immediately feeding cleaned oriental cherry raw material into continuous countercurrent extractor, controlling feeding speed at 180kg/h, starting to inject softened water, and controlling softened water flow rate at 1.4m 3 And h, rotating the rotating shaft of the extractor at a speed of 10r/h to ensure that the softened water fully immerses the materials, the raw material extracting solution fed initially is nearly colorless, the total adding amount of the softened water is about 10000L, and the heater is started to control the temperature of the material liquid to be 50 ℃ during the period, and the extracting solution is obtained by collection.
S3: and (3) filtering the extracting solution, namely filtering the extracting solution by a 38-micron first filter bag, allowing the filtrate to flow into a pipeline filter with a built-in 1-micron second filter bag through a closed pipeline, filtering the filtrate by ceramic membrane equipment (equipment model KM1030-CM-122) with a built-in 100-nm ceramic filter membrane, filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in 2WDa first ultrafiltration membrane, and filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in 1KDa second ultrafiltration membrane to obtain trapped fluid.
S4: concentrating the trapped fluid by reverse osmosis membrane equipment (equipment model KM8040-NF-G16) to obtain concentrated solution with relative density of 1.04.
S5: sterilizing, namely sterilizing the concentrated solution by an UHT (ultra high temperature) instantaneous sterilizer at 115 ℃ for 5s, and rapidly cooling the sterilized feed liquid to room temperature.
S6: freeze drying, sterilizing, placing the feed liquid into tray via tray separator, and freeze drying in freeze dryer to obtain dry extract;
wherein, the freeze drying process comprises the following steps:
Figure BDA0003618360840000151
s7: sieving, collecting dried extract, sieving with a sieve having a pore size of 180 μm in a swing granulator, and collecting sieved granule and fine powder to obtain oriental cherry powder.
In each process, the continuous production is carried out by adopting a special closed pipeline, the operation is easy, and the product safety is high.
The experimental detection is carried out on the prepared cherry blossom powder, the content of each effective component in the active ingredients is shown in table 1, the comparison of AGEs generation inhibition rate is shown in table 2, and the sense and dissolution conditions are shown in table 3:
a) average dry powder yield: 30.3 percent;
b) average total flavone content: 16.2 percent and the transfer rate of the effective components is 87.0 percent;
c) average caffeoyl glucose content: 7.8 percent and the transfer rate of effective components is 80.7 percent;
d) average quercetin glucoside content: 0.81 percent and the transfer rate of effective components is 94.0 percent;
the finished product has pure color, aroma and taste, can be quickly dissolved in an aqueous solution, is clear and transparent and has good stability.
Comparative example 1
In the comparative example, the conventional extraction tank is adopted to extract the cherry petals, the process conditions of other procedures are kept consistent with those of the example 1, and the performances of the cherry pollen obtained by the process and preparation are as follows:
s1: cleaning, namely taking 1000kg of cherry blossom petals, placing the cherry blossom petals in a traditional Chinese medicine cleaning machine (equipment model XY-500) for cleaning, placing cleaned cherry blossom raw materials in a traditional Chinese medicine crusher for coarse crushing, wherein the sieve mesh diameter is 20mm, and collecting the coarse crushed raw materials for later use.
S2: extracting, immediately putting the coarsely crushed oriental cherry raw materials into a multifunctional extraction tank, adding 7000L of softened water, heating to 40 deg.C, extracting for 6h, and collecting to obtain extractive solution.
S3: and (3) filtering, namely filtering the extracting solution by a first filter bag with the diameter of 150 microns, flowing the filtrate into a pipeline filter with a built-in second filter bag with the diameter of 5 microns through a closed pipeline, filtering the filtrate by ceramic membrane equipment (equipment model KM1030-CM-122) with a built-in ceramic filter membrane with the diameter of 200nm, filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in first ultrafiltration membrane of 5WDa, and finally filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in second ultrafiltration membrane of 3KDa to obtain trapped fluid.
S4: concentrating the retentate with reverse osmosis membrane equipment (equipment model KM8040-NF-G16), and concentrating to relative density of 1.07 to obtain concentrated solution.
S5: sterilizing, sterilizing the concentrated solution with UHT ultra high temperature instant sterilizer at 125 deg.C for 35s, and rapidly cooling to room temperature.
S6: freeze drying, sterilizing, loading into tray, and freeze drying in freeze dryer to obtain dry extract. The freeze drying process comprises the following steps:
Figure BDA0003618360840000161
s7: sieving, collecting dried extract, sieving with a sieve having a mesh size of 250 μm in a swing granulator, and collecting sieved granule and fine powder to obtain oriental cherry powder.
In each process, the continuous production is carried out by adopting a special closed pipeline, the operation is easy, and the product safety is high.
The experimental detection is carried out on the prepared cherry blossom powder, the content of each effective component in the active ingredients is shown in table 1, the comparison of AGEs generation inhibition rate is shown in table 2, and the sense and dissolution conditions are shown in table 3:
a) dry powder yield: 22.8 percent of the total weight of the steel,
b) the content of total flavonoids is as follows: 14.3 percent and the transfer rate of effective components is 57.8 percent;
c) content of caffeoyl glucose: 7.2 percent and the transfer rate of effective components is 56.0 percent;
d) content of quercetin glucoside: 0.71 percent and the transfer rate of effective components is 62.0 percent;
the finished product has pure color, aroma and taste, can be quickly dissolved in an aqueous solution, is clear and transparent and has good stability.
Wherein, the yield of the dry powder and the transfer rate of each effective component are obviously lower than those of the embodiment 1, and the analysis reason is that the solvent amount and the extraction frequency required by the conventional extraction tank are more, and the oriental cherry raw material in the embodiment can not be fully extracted.
Comparative example 2
In the comparative example, the first ultrafiltration membrane and the second ultrafiltration membrane are not used for filtration, other procedures and process conditions are kept consistent with those of example 1, and the performances of the cherry pollen obtained by the process and the preparation are as follows:
s1: cleaning, namely taking 1000kg of cherry blossom petals, placing the cherry blossom petals in a traditional Chinese medicine cleaning machine (equipment model XY-500) for cleaning, placing cleaned cherry blossom raw materials in a traditional Chinese medicine crusher for coarse crushing, wherein the sieve mesh diameter is 20mm, and collecting the coarse crushed raw materials for later use.
S2: countercurrent extraction, immediately feeding the coarsely crushed oriental cherry raw material into a continuous countercurrent extractor, controlling the feeding speed at 200kg/h, starting to inject softened water, and controlling the flow rate of the softened water at 1.2m 3 And h, rotating the rotating shaft of the extractor at a speed of 12r/h to ensure that the softened water fully immerses the materials, the raw material extracting solution fed initially is nearly colorless, the total adding amount of the softened water is about 7000L, the heater is started during the period, the temperature of the material liquid is controlled to be 40 ℃, and the extracting solution is collected.
S3: filtering, wherein the extractive solution is firstly filtered by a first filter bag with 150 μm, the filtrate flows into a pipeline filter with a built-in second filter bag with 5 μm through a closed pipeline, and is then filtered by ceramic membrane equipment (equipment model KM1030-CM-122) with a built-in 200nm ceramic filter membrane, to obtain filtrate.
S4: concentrating the filtrate with reverse osmosis membrane equipment (equipment model KM8040-NF-G16), and concentrating to relative density of 1.07 to obtain concentrated solution.
S5: sterilizing, sterilizing the concentrated solution with UHT ultra high temperature instant sterilizer at 125 deg.C for 35s, and rapidly cooling to room temperature.
S6: freeze drying, sterilizing, loading the sterilized material liquid into tray via tray separator, and freeze drying in freeze drier to obtain dry extract. The freeze drying process comprises the following steps:
Figure BDA0003618360840000181
s7: sieving, collecting dried extract, sieving with a sieve having a mesh size of 250 μm in a swing granulator, and collecting sieved granule and fine powder to obtain oriental cherry powder.
In each process, the continuous production is carried out by adopting a special closed pipeline, the operation is easy, and the product safety is high.
The experimental detection is carried out on the prepared cherry blossom powder, the content of each effective component in the active ingredients is shown in table 1, the comparison of AGEs generation inhibition rate is shown in table 2, and the sense and dissolution conditions are shown in table 3:
a) dry powder yield: 41.5 percent;
b) the content of total flavonoids is as follows: 11.3 percent and the transfer rate of the effective components is 83.1 percent;
c) content of caffeoyl glucose: 5.6 percent and the transfer rate of effective components is 79.3 percent;
d) content of quercetin glucoside: 0.58 percent and the transfer rate of the effective components is 92.2 percent;
the finished product has pure color, aroma and taste, can be quickly dissolved in an aqueous solution, is clear and transparent, but has poor solution stability and more precipitates;
the yield of the dry powder is obviously higher than that of the dry powder in example 1, because the ultrafiltration membrane is not adopted for separation and purification, the content of each effective component is obviously lower than that of the dry powder in example 1, and impurities such as macromolecular protein, polysaccharide, micromolecular sugar, organic acid and the like in the extract are not removed.
Comparative example 3
In this comparative example, the conventional external circulation concentrator was used for concentration, the other steps and the process conditions were kept the same as in example 1, and the cherry pollen obtained by the process and preparation had the following properties:
s1: cleaning, namely taking 1000kg of cherry blossom petals, placing the cherry blossom petals in a traditional Chinese medicine cleaning machine (equipment model XY-500) for cleaning, placing cleaned cherry blossom raw materials in a traditional Chinese medicine crusher for coarse crushing, wherein the sieve mesh diameter is 20mm, and collecting the coarse crushed raw materials for later use.
S2: countercurrent extraction, immediately feeding the coarsely crushed oriental cherry raw material into a continuous countercurrent extractor, controlling the feeding speed at 200kg/h, starting to inject softened water, and controlling the flow rate of the softened water at 1.2m 3 And h, rotating the rotating shaft of the extractor at a speed of 12r/h to ensure that the softened water fully immerses the materials, the raw material extracting solution fed initially is nearly colorless, the total adding amount of the softened water is about 7000L, the heater is started during the period, the temperature of the material liquid is controlled to be 40 ℃, and the extracting solution is collected.
S3: and (3) filtering, namely filtering the extracting solution by a first filter bag with the diameter of 150 microns, flowing the filtrate into a pipeline filter with a built-in second filter bag with the diameter of 5 microns through a closed pipeline, filtering the filtrate by ceramic membrane equipment (equipment model KM1030-CM-122) with a built-in ceramic filter membrane with the diameter of 200nm, filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in first ultrafiltration membrane of 5WDa, and finally filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in second ultrafiltration membrane of 3KDa to obtain trapped fluid.
S4: concentrating, pumping the trapped solution into an external circulation concentrator for concentrating, controlling the vacuum degree to be-0.08 MPa and the temperature to be 68 ℃, and concentrating to the relative density of 1.07 to obtain concentrated solution.
S5: sterilizing, sterilizing the concentrated solution with UHT ultra high temperature instant sterilizer at 125 deg.C for 35s, and rapidly cooling to room temperature.
S6: freeze drying, sterilizing, loading into tray, and freeze drying in freeze dryer to obtain dry extract. The freeze drying process comprises the following steps:
Figure BDA0003618360840000191
Figure BDA0003618360840000201
s7: sieving, collecting dried extract, sieving with a sieve having a mesh size of 250 μm in a swing granulator, and collecting sieved granule and fine powder to obtain oriental cherry powder.
In each process, the continuous production is carried out by adopting a special closed pipeline, the operation is easy, and the product safety is high.
The experimental detection is carried out on the prepared cherry blossom powder, the content of each effective component in the active ingredients is shown in table 1, the comparison of AGEs generation inhibition rate is shown in table 2, and the sense and dissolution conditions are shown in table 3:
a) dry powder yield: 28.8 percent;
b) the content of total flavonoids is as follows: 13.5 percent and the transfer rate of effective components is 68.9 percent;
c) content of caffeoyl glucose: 6.3 percent and the transfer rate of effective components is 61.9 percent;
d) content of quercetin glucoside: 0.73 percent and the transfer rate of effective components is 80.6 percent;
although the cherry essence can be quickly dissolved in an aqueous solution, the cherry essence is clear and transparent, the finished product has no obvious characteristic aroma of cherry blossom, the stability of the solution is poor, and a small amount of precipitate is generated because vacuum reduced pressure concentration is adopted in the case, a large amount of aroma components are lost in the process, and meanwhile, heating is needed to cause partial polymerization of phenolic acid components in the feed liquid to form unstable supramolecular insoluble substances.
Comparative example 4
In the comparative example, spray drying was used for drying, other processes and process conditions were kept the same as in example 1, and the cherry pollen obtained by the processes and preparation had the following properties:
s1: cleaning, namely taking 1000kg of cherry blossom petals, placing the cherry blossom petals in a traditional Chinese medicine cleaning machine (equipment model XY-500) for cleaning, placing cleaned cherry blossom raw materials in a traditional Chinese medicine crusher for coarse crushing, wherein the sieve mesh diameter is 20mm, and collecting the coarse crushed raw materials for later use.
S2: countercurrent extraction of crude extractImmediately feeding the crushed oriental cherry raw material into a continuous countercurrent extractor, controlling the feeding speed at 200kg/h, starting to inject softened water, and controlling the flow rate of the softened water at 1.2m 3 And h, rotating the rotating shaft of the extractor at a speed of 12r/h to ensure that the softened water fully immerses the materials, the raw material extracting solution fed initially is nearly colorless, the total adding amount of the softened water is about 7000L, the heater is started during the period, the temperature of the material liquid is controlled to be 40 ℃, and the extracting solution is collected.
S3: and (3) filtering, namely filtering the extracting solution by a first filter bag with the diameter of 150 microns, flowing the filtrate into a pipeline filter with a built-in second filter bag with the diameter of 5 microns through a closed pipeline, filtering the filtrate by ceramic membrane equipment (equipment model KM1030-CM-122) with a built-in ceramic filter membrane with the diameter of 200nm, filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in first ultrafiltration membrane of 5WDa, and finally filtering the filtrate by ultrafiltration membrane equipment (equipment model KM8040-NF-G6) with a built-in second ultrafiltration membrane of 3KDa to obtain trapped fluid.
S4: concentrating the retentate with reverse osmosis membrane equipment (equipment model KM8040-NF-G16), and concentrating to relative density of 1.07 to obtain concentrated solution.
S5: sterilizing, sterilizing the concentrated solution with UHT ultra high temperature instant sterilizer at 125 deg.C for 35s, and rapidly cooling to room temperature.
S6: drying, sterilizing, and drying in a spray dryer with air inlet temperature of 180 deg.C and air outlet temperature of 85 deg.C.
S7: sieving, collecting dried extract, sieving with a sieve having a mesh size of 250 μm in a swing granulator, and collecting sieved granule and fine powder to obtain oriental cherry powder.
In each process, the continuous production is carried out by adopting a special closed pipeline, the operation is easy, and the product safety is high.
The experimental detection is carried out on the prepared cherry blossom powder, the content of each effective component in the active ingredients is shown in table 1, the comparison of AGEs generation inhibition rate is shown in table 2, and the sense and dissolution conditions are shown in table 3:
a) dry powder yield: 27.7 percent;
b) the content of total flavonoids is as follows: 14.7 percent and the transfer rate of effective components is 72.2 percent;
c) content of caffeoyl glucose: 6.7 percent and the transfer rate of effective components is 63.3 percent;
d) content of quercetin glucoside: 0.77 percent and the transfer rate of effective components is 81.7 percent;
although the product can be dissolved in an aqueous solution, is clear and transparent, the finished product has no obvious characteristic fragrance of cherry blossom, the stability of the solution is poor, and a small amount of precipitate is generated because spray drying is adopted in the embodiment, fragrance components are lost in the process, and meanwhile, heating is needed to ensure that phenolic acid components in the feed liquid are partially polymerized to form unstable supermolecule insoluble substances.
In order to fully illustrate the performance of the cherry pollen produced by the process method, quercetin glucoside, aminoguanidine hydrochloride (positive), rose pollen and the like are purchased from the market respectively for test.
The AGEs generation inhibition rate test method comprises the following steps:
to a phosphate buffer (pH7.4, 900mL) containing D-glucose (10%) and bovine serum albumin (1%), 3. mu.g/mL, 10. mu.g/mL, 30. mu.g/mL, 100. mu.g/mL, 300. mu.g/mL of a sample solution containing the oriental cherry extract (examples 1 to 5, comparative examples 1 to 4) and the component (quercetin glucoside) thereof was added 100mL, and the mixture was allowed to stand at 60 ℃ for 2 days. The solution was diluted with pure water so that the fluorescence intensity became about 500, and the fluorescence intensity was measured (measurement wavelength: 370nm, excitation wavelength: 440 nm).
The extract was diluted with purified water, and the components were dissolved in DMSO, and then diluted with phosphate buffer so that the final DMSO concentration was 1%.
TABLE 1 content of oriental cherry powder under different process conditions
Figure BDA0003618360840000221
TABLE 2 comparison of AGEs formation inhibition rate of oriental cherry pollen under different process conditions (n. 3)
Figure BDA0003618360840000231
Note: each value is expressed as the mean and standard error of 3 experiments, compared to the blank (group not treated with drug): p < 0.05, x: p is less than 0.01.
To compare the above data more intuitively, the data is now made into a histogram as shown in fig. 1.
TABLE 3 organoleptic and dissolution of oriental cherry powder under different process conditions
Figure BDA0003618360840000232
Figure BDA0003618360840000241
As can be seen from tables 1 to 3 and fig. 1, the contents of active ingredients are lost by the methods of extraction in a common extraction tank (comparative example 1), heating concentration (comparative example 2) and spray drying (comparative example 4), and meanwhile, the effective ingredients are purified without using an ultrafiltration membrane (comparative example 2), so that the content of efficacy is low, so that the AGEs formation inhibition rate is low, and the solubility and stability of an aqueous solution are poor, and because unstable and easily polymerizable impurities are removed by membrane treatment, the cherry pollen prepared by the preparation method of the cherry pollen with the activity of inhibiting the AGE formation is far inferior to the cherry pollen prepared by the preparation method of the cherry pollen with the activity of inhibiting the AGE formation.
Having thus described the principal technical features and basic principles of the invention, and the advantages associated therewith, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, but is capable of 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.
Furthermore, it should be understood that although the present description is described in terms of various embodiments, not every embodiment includes only a single embodiment, and such descriptions are provided for clarity only, and those skilled in the art will recognize that the embodiments described herein can be combined as a whole to form other embodiments as would be understood by those skilled in the art.

Claims (10)

1. A method for producing cherry pollen having an activity of inhibiting AGE production, comprising the steps of:
s1: cleaning, namely cleaning cherry petals to obtain a cherry raw material;
s2: performing countercurrent extraction, namely putting the oriental cherry raw material into a continuous countercurrent extractor for extraction to obtain an extracting solution;
s3: filtering, namely sequentially filtering the extracting solution by using a first filter bag of 38-180 mu m, a second filter bag of 1-10 mu m, a filtering membrane of 100-200 nm, a first ultrafiltration membrane of 2-5 WDa and a second ultrafiltration membrane of 1-5 KDa to form trapped solution;
s4: concentrating the trapped fluid by using a reverse osmosis membrane or a nanofiltration membrane until the relative density is 1.04-1.10 to form concentrated fluid;
s5: sterilizing, namely sterilizing the concentrated solution;
s6: freeze drying, placing the sterilized concentrated solution in a freeze dryer for freeze drying to obtain dry extract;
s7: sieving, grading the dry extract, and collecting the granules and fine powder.
2. The method for producing cherry pollen having an activity of inhibiting AGE formation according to claim 1, wherein: in step S1, a chinese medicine washing machine is used to wash the cherry blossom, and a chinese medicine crusher is used to crush the petals after washing.
3. The method for producing cherry pollen having an activity of inhibiting AGE formation according to claim 1, wherein: in the step ofIn S2, the technological conditions of the countercurrent extraction are as follows: the feeding speed is 180-220 kg/h, and the flow rate of the softened water injected into the extraction solvent is 1.0-1.4 m 3 The rotation speed of a rotating shaft of the extractor is 10-15 r/h, the total amount of the added solvent is 5-10 times of the weight of the cherry blossom, and the extraction temperature is 10-50 ℃.
4. The method for producing cherry pollen having an activity of inhibiting AGE formation according to claim 3, wherein: the extraction temperature is 38-42 ℃, and the countercurrent extractor adopts a pipeline type countercurrent extractor.
5. The method for producing cherry pollen having an activity of inhibiting AGE formation according to claim 1, wherein: in step S3, the first ultrafiltration membrane is 4-5 WDa, and the second ultrafiltration membrane is 2-4 KDa; the filter membrane is a ceramic membrane, and the first filter bag and the second filter bag are arranged in the pipeline filter for filtering.
6. The method for producing cherry pollen having an activity of inhibiting AGE formation according to claim 1, wherein: in step S4, the mixture is concentrated to a relative density of 1.06 to 1.08.
7. The method for producing cherry pollen having an activity of inhibiting AGE formation according to claim 1, wherein: and in step S5, a UHT ultrahigh-temperature instantaneous sterilizer is adopted for sterilization, the sterilization temperature is 115-135 ℃, the sterilization time is 5-50S, and the sterilized feed liquid is rapidly cooled to the room temperature.
8. The method for producing cherry pollen having an activity of inhibiting AGE formation according to claim 1, wherein: in step S6, the freeze-drying process is:
s61: pre-freezing, and keeping the temperature at-55 to-30 ℃ for 2 to 6 hours at normal pressure;
s62: sublimation drying, raising the temperature from minus 55 to minus 30 ℃ to minus 25 to minus 15 ℃ at a constant speed in vacuum of 0 to 45Pa for 30 to 180min, and preserving the temperature for 2 to 7 hours; then under the vacuum of 0-45 Pa, the temperature is increased from minus 25 to minus 15 ℃ to minus 15 to minus 5 ℃ at a constant speed for 30-180 min, and the temperature is kept for 5-12 h;
s63: and (3) resolving and drying, raising the temperature from minus 15 to minus 5 ℃ to 30 to 55 ℃ at a constant speed for 30 to 240min under the vacuum of 5 to 50pa, and preserving the temperature for 3 to 9 hours.
9. The method for producing cherry pollen having an activity of inhibiting AGE formation according to claim 1, wherein: in step S7, the dried paste is granulated and sieved by using a shaking granulator with a screen of 180 to 550 μm.
10. The method for producing cherry pollen having an activity of inhibiting AGE formation according to claim 1, wherein: all the procedures are connected by closed pipelines, and the full-closed continuous production is realized.
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