CN111903811A - Eucommia male flower instant powder and preparation method and application thereof - Google Patents
Eucommia male flower instant powder and preparation method and application thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
- A23F3/00—Tea; Tea substitutes; Preparations thereof
- A23F3/34—Tea substitutes, e.g. matè; Extracts or infusions thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, 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
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/26—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by irradiation without heating
- A23L3/28—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by irradiation without heating with ultraviolet light
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, 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
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
- A23L5/27—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption
- A23L5/276—Treatment with inorganic compounds
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Abstract
The invention discloses eucommia male flower instant powder and a preparation method and application thereof, wherein the preparation method comprises the following steps: s1, preprocessing male flowers of eucommia ulmoides; s2, preparing an eucommia male flower extracting solution, mixing the eucommia male flower with water, adding a natural antioxidant, and carrying out ultrasonic crushing treatment to obtain the eucommia male flower extracting solution; s3, vacuum concentration of the eucommia male flower extracting solution, namely filtering the eucommia male flower extracting solution, and carrying out vacuum concentration treatment on the filtrate until the concentration of solid matters is 75-80% to obtain a concentrated extracting solution; s4, freeze-drying the concentrated extract, pre-freezing the concentrated extract, and then carrying out vacuum freeze-drying to obtain the eucommia male flower instant powder with the water content lower than 5%. The eucommia male flower instant powder obtained by the preparation method of the eucommia male flower instant powder has the advantages that the eucommia male flower instant powder is prepared from fresh eucommia male flowers, the storage life is effectively prolonged, and the original nutrition and active ingredients of the eucommia male flowers are well reserved.
Description
Technical Field
The invention relates to the field of eucommia male flowers, in particular to eucommia male flower instant powder. In addition, the invention also relates to a preparation method and application of the eucommia male flower instant powder.
Background
Eucommia bark is a peculiar rare medicinal plant in China, and at the present stage, research on eucommia bark mainly focuses on cultivation of eucommia bark, processing of eucommia bark leaves, seeds and bark and the like, relatively few processing researches on male flowers of eucommia bark are carried out, the male flowers of eucommia bark are male tree flowers of eucommia bark, and modern researches show that the male flowers of eucommia bark are rich in lignans, iridoids, phenylpropanoids, flavonoids and other medicinal components similar to the eucommia bark and leaves, and have various pharmacological effects of reducing blood pressure, reducing blood fat, resisting tumors, resisting bacteria, resisting viruses, resisting fatigue, protecting liver and benefiting gallbladder and the like; meanwhile, the health-care food also contains rich nutrient components such as crude protein, amino acid, polysaccharide, mineral elements and the like, and has high nutritional and health-care values. Eucommia male flowers are approved as new food raw materials at present, and products such as tea products, health care products, functional beverages and the like are developed by taking the eucommia male flowers as the raw materials, so that the eucommia male flowers are paid much attention in the market. The product is mainly eucommia male flower tea, and male flowers are eaten in a single mode by using a brewing tea drinking mode. The eucommia male flower has very low density, floats on the liquid surface after being flushed with water, seriously influences the comfort level during drinking, and can not completely release the active ingredients in the eucommia male flower by a simple soaking mode, thereby reducing the use value of the eucommia male flower.
Disclosure of Invention
The invention provides an instant eucommia male flower powder and a preparation method and application thereof, and aims to solve the technical problems that the utilization efficiency of eucommia male flowers is low, the leaching rate of active functional components is low, and the utilization of nutritional values is insufficient at the present stage.
The technical scheme adopted by the invention is as follows:
a preparation method of eucommia male flower instant powder comprises the following steps:
s1, pretreating male flowers of eucommia ulmoides, soaking the male flowers of eucommia ulmoides in disinfectant for disinfection and sterilization, washing with water, and draining;
s2, preparing an eucommia male flower extracting solution, namely mixing the eucommia male flower subjected to water draining in the step S1 with water to obtain a mixture, adding a natural antioxidant, wherein the mass-to-volume ratio (g/ml) of the natural antioxidant to the mixture is 0.05-0.1%, and performing ultrasonic crushing treatment to obtain the eucommia male flower extracting solution;
s3, vacuum concentration of the eucommia male flower extracting solution, namely filtering the eucommia male flower extracting solution in the step S2, and carrying out vacuum concentration treatment on the filtrate until the concentration of solid matters is 75% -80% to obtain a concentrated extracting solution;
s4, freeze-drying the concentrated extract, namely pre-freezing the concentrated extract in the step S3, and then carrying out vacuum freeze-drying to obtain the eucommia male flower instant powder with the water content of less than 5%.
Further, in the step S2, the mass-to-volume ratio (g/ml) of the mixture of the eucommia male flowers and the water is 1: 3-1: 5; in step S2, the ultrasonic disruption treatment is performed by using an ultrasonic cell disruptor.
Further, the conditions of the ultrasonication treatment were: the ultrasonic crushing frequency is 15 KHz-25 KHz, the ultrasonic treatment frequency is 3-5 times, the ultrasonic crushing time is 5 min-10 min each time, and the ultrasonic crushing interval is 30 s-60 s.
Further, the eucommia male flower in the step S2 is prepared into eucommia male flower powder and then is mixed with water; the preparation method of the eucommia male flower powder comprises the following steps: vacuum drying eucommia male flowers until the water content is less than or equal to 5 percent to obtain dried eucommia male flowers; coarsely crushing the eucommia male flower, and sieving with a 100-mesh sieve to obtain eucommia male flower coarse material; micronizing coarse material of male flower of Eucommiae cortex with cell-level micronizer to obtain male flower powder of Eucommiae cortex with particle size less than 50 μm.
Further, the vacuum degree of vacuum drying is-0.10 Mpa to-0.05 Mpa, and the vacuum temperature is 35-45 ℃.
Further, the step S1 specifically includes: placing eucommia male flower and disinfectant with concentration of 0.1% into vibration water tank, cleaning for 5min for sterilization, washing with ultrapure water for 5min to remove residual chloride ions, and draining water.
Further, filtering in the step S3 by adopting a sieve or gauze of 80-120 meshes; the vacuum degree of vacuum concentration is 0.08MPa to 0.10MPa, and the temperature is 60 ℃ to 80 ℃.
Further, pre-freezing the concentrated extract at-65 deg.C to-70 deg.C for 1-3 h in step S4; the vacuum degree of the vacuum freeze drying treatment is 1Pa to 5Pa, the temperature is-50 ℃ to-55 ℃, and the drying time is 24h to 48 h.
Further, the eucommia male flower is fresh eucommia male flower picked within 3 days; and/or, the natural antioxidant adopts Vc; and/or the disinfectant adopts sodium hypochlorite aqueous solution.
Further, the preparation method of the eucommia male flower instant powder also comprises the steps of hermetically packaging the eucommia male flower instant powder and carrying out ultraviolet lamp irradiation sterilization treatment; the ultraviolet lamp is used for irradiation sterilization at 30-50W for 0.5-1 h.
According to another aspect of the invention, the eucommia male flower instant powder obtained by the preparation method is also provided.
According to another aspect of the invention, the application of the eucommia male flower instant powder in a beverage is further provided, and the eucommia male flower instant powder is mixed with water to obtain the beverage.
The invention has the following beneficial effects:
the preparation method of the eucommia male flower instant powder creatively combines an ultrasonic crushing extraction technology and a freeze drying technology, extracts the eucommia male flower extract by ultrasonic crushing, improves the extraction rate of active ingredients in the eucommia male flower, improves the content of functional ingredients and nutrient ingredients of the product, and retains the activity of the nutrition and functional ingredients in the eucommia male flower to the maximum extent by using the freeze drying technology, so that the original efficacy and flavor of the eucommia male flower are retained. And the eucommia male flower extracting solution obtained by ultrasonic crushing is subjected to vacuum concentration, so that the oxidation of active ingredients in the eucommia male flower extracting solution is effectively inhibited.
The eucommia male flower instant powder obtained by the preparation method of the eucommia male flower instant powder effectively prolongs the storage life, well retains the original nutrition and active ingredients of the eucommia male flower, further increases the solubility, dispersibility and absorbability of the eucommia male flower, ensures the product stability and product quality, increases the deep processing and utilization potential of the eucommia male flower product, and expands the comprehensive application range of the eucommia male flower. And the instant powder of the eucommia male flower has stable property, is convenient to carry and easy to store, and improves the additional value of the eucommia male flower product.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic process flow diagram of a preferred embodiment of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
As shown in fig. 1, the preparation method of the instant powder of eucommia male flowers in this embodiment includes the following steps:
s1, pretreating male flowers of eucommia ulmoides, soaking the male flowers of eucommia ulmoides in disinfectant for disinfection and sterilization, washing with water, and draining;
s2, preparing an eucommia male flower extracting solution, namely mixing the eucommia male flower subjected to water draining in the step S1 with water to obtain a mixture, adding a natural antioxidant, wherein the mass-to-volume ratio (g/ml) of the natural antioxidant to the mixture is 0.05-0.1%, and performing ultrasonic crushing treatment to obtain the eucommia male flower extracting solution;
s3, vacuum concentration of the eucommia male flower extracting solution, namely filtering the eucommia male flower extracting solution in the step S2, and carrying out vacuum concentration treatment on the filtrate until the concentration of solid matters is 75% -80% to obtain a concentrated extracting solution;
s4, freeze-drying the concentrated extract, namely pre-freezing the concentrated extract in the step S3, and then carrying out vacuum freeze-drying to obtain the eucommia male flower instant powder with the water content of less than 5%.
The preparation method of the eucommia male flower instant powder creatively combines an ultrasonic crushing extraction technology and a freeze drying technology, extracts the eucommia male flower extract by ultrasonic crushing, improves the extraction rate of active ingredients in the eucommia male flower, improves the content of functional ingredients and nutrient ingredients of the product, and retains the activity of the nutrition and functional ingredients in the eucommia male flower to the maximum extent by using the freeze drying technology, so that the original efficacy and flavor of the eucommia male flower are retained. And the eucommia male flower extracting solution obtained by ultrasonic crushing is subjected to vacuum concentration, so that the oxidation of active ingredients in the eucommia male flower extracting solution is effectively inhibited. The active ingredients of the eucommia male flower of the invention are mainly measured by the content of water-soluble polysaccharide and total amino acid. The active ingredients of the eucommia male flower comprise water-soluble polysaccharide and total amino acid.
The eucommia male flower instant powder obtained by the preparation method of the eucommia male flower instant powder effectively prolongs the storage life, well retains the original nutrition and active ingredients of the eucommia male flower, further increases the solubility, dispersibility and absorbability of the eucommia male flower, ensures the product stability and product quality, increases the deep processing and utilization potential of the eucommia male flower product, and expands the comprehensive application range of the eucommia male flower. And the instant powder of the eucommia male flower has stable property, is convenient to carry and easy to store, and improves the additional value of the eucommia male flower product.
In this embodiment, the mass-to-volume ratio (g/ml) of the mixture of the male flowers of eucommia ulmoides and water in step S2 is 1: 3 to 1: 5. The water can be distilled water. The eucommia male flower extract is prepared by water extraction, so that the difficulty of repeatedly extracting eucommia bark and eucommia leaves by using an organic solvent is overcome, and the volatilization pollution of the organic solvent is reduced. And strictly controlling the mass volume ratio (g/ml) of the eucommia male flowers to the water to be 1: 3-1: 5, and improving the extraction rate of active ingredients in the subsequent ultrasonic crushing treatment.
In this example, the ultrasonic cell disruptor was used for the ultrasonic disruption treatment in step S2. The folium Eucommiae and cortex Eucommiae contain 17 kinds of amino acids, 6 kinds of essential amino acids, and the total amount of amino acids in folium Eucommiae is 13.33%. The eucommia male flower contains 18 amino acids, the total amount of the amino acids reaches 21.88 percent, is 4.66 times of that of eucommia bark and is 1.45-2.57 times of that of eucommia leaves. The content of active ingredients of the eucommia male flower is high, the active ingredients of the eucommia male flower can be damaged by adopting a conventional organic solvent extraction method of eucommia leaves and barks, and the extraction efficiency is relatively low. According to the preparation method of the instant powder of the male eucommia ulmoides flower, an ultrasonic crushing extraction technology is adopted, the male eucommia ulmoides flower is mixed with water, a natural antioxidant is added, ultrasonic crushing treatment is carried out in an ultrasonic crusher, the cell wall of the male eucommia ulmoides flower is crushed, active ingredients are released and dissociated, and the extraction efficiency of the active ingredients is remarkably improved. After the ultrasonic crushing treatment, the obtained water-soluble active ingredients not only have the active functional ingredients such as protochlorogenic acid, iridoid, phenylpropanoid, flavonoid glycoside and the like similar to eucommia bark and eucommia leaf, but also contain water-soluble polysaccharide, amino acid, mineral substances and the like.
In this example, the conditions of the ultrasonication treatment were as follows: the ultrasonic crushing frequency is 15 KHz-25 KHz, the ultrasonic treatment frequency is 3-5 times, the ultrasonic crushing time is 5 min-10 min each time, and the ultrasonic crushing interval is 30 s-60 s. The higher the ultrasonication frequency and the longer the ultrasonication time, the better the cell disruption effect, but it follows that the high temperature of the solution caused by the ultrasonication causes the burning of the eucommia male flowers, and also leads to the denaturation or loss of the active ingredient. The above-described identification of the ultrasonication process was obtained by related experiments. Moreover, the ultrasonic crusher focuses on crushing eucommia male flower cells to enable water-soluble active ingredients to be dissociated, so that the ultrasonic time is short and only needs 5-10 min. Preferably, the ultrasonic crushing frequency is 15 KHz-20 KHz, the ultrasonic treatment frequency is 3-4 times, the ultrasonic crushing time is 6 min-9 min each time, and the ultrasonic crushing interval is 30 s-60 s. More preferably, the determination of the parameters has relevant experimental verification, the ultrasonic frequency is 20KHz, the ultrasonic treatment is carried out for 4 times, the ultrasonic time is 9min each time, the content of water-soluble polysaccharide and total amino acid in the active ingredients is highest, the obtained eucommia male flower instant powder has the highest yield, and the burning degree of the eucommia male flower extracting solution is minimum.
In this embodiment, the eucommia male flower in step S2 is prepared into eucommia male flower powder, and then mixed with water; the preparation method of the eucommia male flower powder comprises the following steps: vacuum drying eucommia male flowers until the water content is less than or equal to 5 percent to obtain dried eucommia male flowers; coarsely crushing the eucommia male flower, and sieving with a 100-mesh sieve to obtain eucommia male flower coarse material; micronizing coarse material of male flower of Eucommiae cortex with cell-level micronizer to obtain male flower powder of Eucommiae cortex with particle size less than 50 μm. In the step S2, the eucommia male flower is prepared into eucommia male flower powder with the particle size smaller than 50 microns, then the eucommia male flower powder is mixed with water, vacuum drying is carried out on the eucommia male flower, the eucommia male flower is prevented from being oxidized, active ingredients in the eucommia male flower are stored, the obtained eucommia male flower is coarsely crushed, the eucommia male flower powder is sieved through a 100-mesh sieve, and then cell-level superfine grinding is carried out continuously, so that the eucommia male flower powder reaches the cell-level fineness, cells are easy to crush in a subsequent extraction process, the active ingredients are easy to release, therefore, the extraction efficiency of the active ingredients of the eucommia male flower after the eucommia male flower powder is prepared is higher, and the yield of the obtained eucommia male flower instant powder is also high.
Preferably, the vacuum degree of the vacuum drying is-0.10 Mpa to-0.05 Mpa, and the vacuum temperature is 35-45 ℃. The eucommia male flower is dried under the vacuum condition, so that the space is isolated to prevent oxidation, the extraction rate of active ingredients in the eucommia male flower is further improved, and the product efficacy and the nutritional ingredients are improved.
In this embodiment, the step S1 includes the following steps: placing eucommia male flower and disinfectant with concentration of 0.1% into vibration water tank, cleaning for 5min for sterilization, washing with ultrapure water for 5min to remove residual chloride ions, and draining water. In the preparation process of the instant powder, sodium hypochlorite solution is adopted for disinfection and sterilization in the pretreatment stage of the eucommia male flowers, so that the safety and stability of the product are ensured, and the shelf life of the instant powder is prolonged.
In this embodiment, the filtering in step S3 is performed by using a 80-120 mesh screen or gauze. The vacuum degree of vacuum concentration is 0.08MPa to 0.10MPa, and the temperature is 60 ℃ to 80 ℃. The eucommia male flower extract is subjected to filtration treatment to filter out water-insoluble components or large-particle substances, so that when the prepared eucommia male flower instant powder is directly mixed with water for drinking, the water-insoluble components or the large-particle substances influence the drinking taste effect. The vacuum degree of the vacuum concentration is 0.08MPa to 0.10MPa, and the temperature is 60 ℃ to 80 ℃. Vacuum concentration is adopted, on one hand, drying is carried out under a vacuum condition, oxidation of active ingredients in the eucommia male flower extracting solution is reduced, and accordingly loss of the active ingredients is reduced, on the other hand, vacuum concentration processing speed is high, through early-stage research, the concentration time is fastest under the conditions that the vacuum degree is 0.10MPa and the temperature is 65 ℃, and the content of the obtained active ingredients, namely water-soluble polysaccharide and total amino acid is highest.
In the embodiment, the pre-freezing treatment in step S4 is performed by pre-freezing the concentrated extract at-65 ℃ to-70 ℃ for 1h to 3 h. The vacuum degree of the vacuum freeze drying treatment is 1Pa to 5Pa, the temperature is-50 ℃ to-55 ℃, and the drying time is 24h to 48 h. The concentrated extracting solution is pre-frozen before vacuum freeze drying, the cooling rate is high, the supercooling degree and the supersaturation degree of the concentrated extracting solution are increased, the granularity of critical crystallization is small, the nucleation speed is accelerated, fine crystals with small particle granularity are formed, and therefore after ice crystals are sublimated, the pore size formed in the eucommia male flower instant powder is small, the drying rate is low, but the rehydration performance is good, and the method has important significance for forming the eucommia male flower instant powder. And (3) after pre-freezing, putting the frozen powder into a vacuum freeze dryer for freeze drying, controlling the vacuum degree to be between 1 and 5Pa, the temperature to be between 50 and 55 ℃ below zero, and the drying time to be between 24 and 48 hours, thus obtaining the dried powder with the water content of less than 5 percent, wherein the drying time parameter is determined mainly by the water content of the freeze-dried powder. The eucommia male flower instant powder obtained by the vacuum freeze-drying machine can be directly brewed for drinking and can also be used in other foods.
In this example, the eucommia male flower was fresh eucommia male flower picked within 3 days. And/or, the natural antioxidant adopts Vc; and/or the disinfectant adopts sodium hypochlorite aqueous solution. The Vc is mainly used for reducing the loss of active ingredients in the eucommia male flowers from being oxidized in the process of preparing the freeze-dried powder, and the adopted content is low and is only 0.05-0.1%.
In this embodiment, the preparation method of the instant powder of eucommia ulmoides male flower further includes hermetically packaging the instant powder of eucommia ulmoides male flower, and sterilizing the packaged instant powder of eucommia ulmoides male flower by irradiation of an ultraviolet lamp. The ultraviolet lamp is used for irradiation sterilization at 30-50W for 0.5-1 h. The safety and the stability of the product are ensured by twice sterilization and disinfection through sodium hypochlorite solution and ultraviolet irradiation.
According to another aspect of the invention, the eucommia male flower instant powder obtained by the preparation method is also provided.
According to another aspect of the invention, the application of the eucommia male flower instant powder in a beverage is further provided, and the eucommia male flower instant powder is mixed with water to obtain the beverage. The application of the eucommia male flower instant powder in the beverage extracts eucommia male flowers through ultrasonic crushing, so that cell structures are easy to crush, active ingredients are dissociated, and the extraction effect of the active ingredients is improved. The vacuum concentration and the vacuum drying ensure the soluble nutrient and the functional components of the eucommia male flower, the obtained eucommia male flower instant powder is more easily dissolved in water, and the dispersibility and the absorbability brought by the improvement of the solubility are correspondingly improved. The relevant performance test data show that the water extract (mass fraction) of the eucommia male flower instant powder is more than 98 percent, no particles exist after the eucommia male flower instant powder is dissolved in water, the eucommia male flower instant powder is uniformly dissolved, and the eucommia male flower instant powder is prepared.
Examples
Example 1
S1, pretreatment of the eucommia male flower: placing the fresh eucommia male flowers into a vibration water tank of sodium hypochlorite water solution with the mass solubility of 0.1% for cleaning for 5min for disinfection and sterilization, flushing with ultrapure water for 5min to remove residual chloride ions, fishing out the eucommia male flowers and draining water, wherein the eucommia male flowers are required to be free of pollution, rot and oxidation blackening;
s2, preparing an eucommia male flower extracting solution, mixing drained eucommia male flowers with distilled water according to the mass-volume ratio (g/ml) of 1: 3 to obtain a mixture, adding Vc, performing ultrasonic crushing by using an ultrasonic cell crusher under the conditions that the mass-volume ratio (g/ml) of the Vc to the mixture is 0.08%, and stirring the mixture while performing ultrasonic crushing: ultrasonic crushing frequency of 20KHz, ultrasonic processing for 4 times, each ultrasonic crushing time of 6min, and each ultrasonic processing time interval of 45s to obtain Eucommiae cortex male flower extractive solution;
s3, vacuum concentration of the eucommia male flower extracting solution, namely filtering the eucommia male flower extracting solution by using 1-2 layers of 100-mesh gauze, carrying out vacuum concentration treatment on the filtrate under the conditions that the vacuum degree is 0.08MPa and the temperature is 70 ℃, and concentrating until the solid concentration is 80% to obtain a concentrated extracting solution;
s4, freeze-drying the concentrated extract, namely pre-freezing the concentrated extract at the temperature of-65 ℃ for 2 hours, then putting the concentrated extract into a vacuum freeze-drying machine for freeze-drying, controlling the vacuum degree to be 3Pa, the temperature to be-50 ℃ and the drying time to be 24 hours, and obtaining the eucommia male flower instant powder with the water content of less than 5 percent;
s5, sealing and packaging the eucommia ulmoides male flower instant powder, sterilizing for 0.5h by a 50W ultraviolet lamp, and drying and storing at normal temperature in a dark place.
Example 2
S1, pretreatment of the eucommia male flower: placing the fresh eucommia male flowers into a vibration water tank of sodium hypochlorite water solution with the mass solubility of 0.1% for cleaning for 5min for disinfection and sterilization, flushing with ultrapure water for 5min to remove residual chloride ions, fishing out the eucommia male flowers and draining water, wherein the eucommia male flowers are required to be free of pollution, rot and oxidation blackening;
s2, preparing an eucommia male flower extracting solution, namely uniformly spreading the drained eucommia male flowers in a stainless steel disc, placing the stainless steel disc in a vacuum drying oven, drying the eucommia male flowers under the conditions that the vacuum degree is-0.10 Mpa and the temperature is 40 ℃, stirring at intervals, measuring the water content, controlling the water content to be lower than 5%, coarsely crushing the eucommia male flowers, and sieving by a 100-mesh sieve to obtain eucommia male flower coarse materials for later use; starting a temperature reduction system of the ultrafine grinder, setting experiment temperature and grinding time, starting a main machine for preheating for 30min until the machine runs normally, starting the grinding system of the grinder, grinding for 5min, and automatically stopping after grinding is finished to obtain eucommia male flower powder with the particle size of less than 50 microns; mixing eucommia male flower powder with distilled water at a mass-to-volume ratio (g/ml) of 1: 5 to obtain a mixture, adding Vc, wherein the mass-to-volume ratio (g/ml) of Vc to the mixture is 0.08%, performing ultrasonic disruption by using an ultrasonic cell disruption instrument while stirring under the ultrasonic disruption conditions: ultrasonic crushing at 20KHz for 3 times, each ultrasonic crushing time being 9min, and each ultrasonic treatment time interval being 40s to obtain Eucommiae cortex male flower extractive solution;
s3, vacuum concentration of the eucommia male flower extracting solution, filtering the eucommia male flower extracting solution by using a 100-mesh sieve, carrying out vacuum concentration treatment on the filtrate under the conditions that the vacuum degree is 0.09MPa and the temperature is 68 ℃, and concentrating until the solid concentration is 78% to obtain a concentrated extracting solution;
s4, freeze-drying the concentrated extract, namely pre-freezing the concentrated extract at the temperature of-65 ℃ for 2 hours, then putting the pre-frozen extract into a vacuum freeze-drying machine for freeze-drying, controlling the vacuum degree to be 4Pa, the temperature to be-53 ℃ and the drying time to be 40 hours, and obtaining the eucommia male flower instant powder with the water content of less than 5 percent;
s5, sealing and packaging the eucommia ulmoides male flower instant powder, sterilizing for 0.5h by a 50W ultraviolet lamp, and drying and storing at normal temperature in a dark place.
Comparative example 1
The difference from embodiment 1 is that no Vc is added in step S2.
Comparative example 2
The difference from example 1 is that the mass-to-volume ratio (g/ml) of the drained eucommia male flower to the distilled water is 1: 3 in step S2 to obtain a mixture, Vc is added, the mass-to-volume ratio (g/ml) of Vc to the mixture is 0.08%, and the mixture is mixed, stirred and extracted by a magnetic stirring device for 30min to obtain an eucommia male flower extract.
Comparative example 3
The difference from example 1 is that the concentrated extract was directly put into a vacuum freeze dryer to be freeze-dried in step S4.
Example 3
The technological parameters of the ultrasonic crushing treatment are as follows:
carrying out single-factor tests by taking the ultrasonic crushing frequency, the ultrasonic treatment frequency and the ultrasonic crushing time of each time as single factors, wherein the ultrasonic crushing frequency is 10, 15, 20 and 25; the ultrasonic treatment times are 3, 4, 5 and 6; the time for each sonication was 6, 9, 12, 15 and 10min, the rest being the same as in example 1.
The above examples 1, 2, comparative examples 1, 2 and 3 were subjected to performance tests; detecting the content of water-soluble polysaccharide, the content of total amino acids and the appearance of the extracting solution of the ultrasonic crushing treatment in example 3, wherein the content of water-soluble polysaccharide in the freeze-dried powder is determined by adopting a high performance liquid chromatography; the total amino acid content in the freeze-dried powder is determined by adopting a method for determining amino acid in GB 5009.124-2016 national food safety standard food.
TABLE 1 Performance testing of examples and comparative examples
TABLE 2 ultrasonic fragmentation frequency Single factor test results
TABLE 3 ultrasonic treatment times Single factor test results
TABLE 4 Single-factor test results for each sonication time
As shown in table 1, the instant powder of eucommia male flower obtained in example 1 and example 2 has a high content of water-soluble polysaccharide and a high content of total amino acids, which shows that the extraction rate of active ingredients in eucommia male flower is improved by combining the ultrasonic crushing extraction technology and the freeze drying technology, and example 2 is superior to example 1 in that the extraction efficiency of active ingredients of eucommia male flower after preparing eucommia male pollen powder is higher, and comparative example 1 is no Vc is added, and the addition of Vc does not increase the extraction rate of active ingredients, so as to prevent the active ingredients from being oxidized.
As shown in tables 2, 3 and 4, when the ultrasonic frequency is 20KHz, the ultrasonic treatment is carried out for 4 times, and the ultrasonic time is 9min each time, the content of water-soluble polysaccharide and total amino acid in the active ingredients is highest, the obtained eucommia male flower instant powder has the highest yield, the burning degree of the eucommia male flower extracting solution is the lowest, and the use cost of equipment is also saved.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of eucommia male flower instant powder is characterized by comprising the following steps:
s1, pretreating male flowers of eucommia ulmoides, soaking the male flowers of eucommia ulmoides in disinfectant for disinfection and sterilization, washing with water, and draining;
s2, preparing an eucommia male flower extracting solution, namely mixing the eucommia male flower subjected to water draining in the step S1 with water to obtain a mixture, adding a natural antioxidant, wherein the mass-to-volume ratio (g/ml) of the natural antioxidant to the mixture is 0.05-0.1%, and performing ultrasonic crushing treatment to obtain the eucommia male flower extracting solution;
s3, vacuum concentration of the eucommia male flower extracting solution, namely filtering the eucommia male flower extracting solution in the step S2, and carrying out vacuum concentration treatment on the filtrate until the concentration of solid matters is 75% -80% to obtain a concentrated extracting solution;
s4, freeze-drying the concentrated extract, namely pre-freezing the concentrated extract in the step S3, and then carrying out vacuum freeze-drying to obtain the eucommia male flower instant powder with the water content of less than 5%.
2. The method for producing an instant powder of eucommia ulmoides male flower according to claim 1,
in the step S2, the mass-to-volume ratio (g/ml) of the mixture of the eucommia male flowers and the water is 1: 3-1: 5;
the ultrasonic disruption treatment in the step S2 adopts an ultrasonic cell disruptor.
3. The method for producing an instant powder of eucommia ulmoides male flower according to claim 2,
the conditions of the ultrasonic crushing treatment are as follows: the ultrasonic crushing frequency is 15 KHz-25 KHz, the ultrasonic treatment frequency is 3-5 times, the ultrasonic crushing time is 5 min-10 min each time, and the ultrasonic crushing interval is 30 s-60 s.
4. The method for producing an instant powder of eucommia ulmoides male flower according to claim 1,
preparing the eucommia male flower in the step S2 into eucommia male flower powder, and mixing the eucommia male flower powder with water;
the preparation method of the eucommia male flower powder comprises the following steps:
vacuum drying eucommia male flowers until the water content is less than or equal to 5 percent to obtain dried eucommia male flowers;
coarsely crushing the eucommia male flower dried powder, and sieving the crushed eucommia male flower dried powder with a 100-mesh sieve to obtain eucommia male flower coarse material;
micronizing coarse material of male flower of Eucommiae cortex with cell-level micronizer to obtain male flower powder of Eucommiae cortex with particle size less than 50 μm.
5. The method for producing an instant powder of eucommia ulmoides male flower according to claim 4,
the vacuum degree of the vacuum drying is-0.10 Mpa to-0.05 Mpa, and the vacuum temperature is 35 ℃ to 45 ℃.
6. The method for producing an instant powder of eucommia ulmoides male flower according to claim 1,
the step S1 includes the following steps: placing eucommia male flowers and disinfectant with concentration of 0.1% into a vibration water tank, cleaning for 5min for disinfection and sterilization, washing with ultrapure water for 5min to remove residual chloride ions, and draining water;
filtering in the step S3 by adopting a sieve or gauze of 80-120 meshes, wherein the vacuum degree of vacuum concentration is 0.08-0.10 MPa, and the temperature is 60-80 ℃;
in the pre-freezing treatment in the step S4, the concentrated extracting solution is pre-frozen for 1 to 3 hours at the temperature of between 65 ℃ below zero and 70 ℃ below zero, the vacuum degree of the vacuum freeze drying treatment is between 1 and 5Pa, the temperature of between 50 ℃ below zero and 55 ℃ below zero, and the drying time is between 24 and 48 hours.
7. The method for producing an instant powder of eucommia ulmoides male flower according to claim 1,
the eucommia male flower is fresh eucommia male flower picked within 3 days; and/or
The natural antioxidant adopts Vc; and/or
The disinfectant adopts a sodium hypochlorite aqueous solution.
8. The method for producing an instant powder of eucommia ulmoides male flower according to claim 1,
the preparation method of the eucommia male flower instant powder also comprises the steps of hermetically packaging the eucommia male flower instant powder and carrying out ultraviolet lamp irradiation sterilization treatment;
the ultraviolet lamp is used for irradiation sterilization at 30-50W for 0.5-1 h.
9. An instant powder of eucommia male flowers obtained by the preparation method according to claims 1 to 8.
10. Use of the eucommia ulmoides male flower instant powder according to claim 9 in a beverage, wherein the eucommia ulmoides male flower instant powder is mixed with water to obtain the beverage.
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