CN116515579A - Preparation method of fermented semi-sweet dendrobium candidum yellow wine - Google Patents
Preparation method of fermented semi-sweet dendrobium candidum yellow wine Download PDFInfo
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- 108090000623 proteins and genes Proteins 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
- C12G3/00—Preparation of other alcoholic beverages
- C12G3/02—Preparation of other alcoholic beverages by fermentation
- C12G3/021—Preparation of other alcoholic beverages by fermentation of botanical family Poaceae, e.g. wheat, millet, sorghum, barley, rye, or corn
- C12G3/022—Preparation of other alcoholic beverages by fermentation of botanical family Poaceae, e.g. wheat, millet, sorghum, barley, rye, or corn of botanical genus Oryza, e.g. rice
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
- C12G3/00—Preparation of other alcoholic beverages
- C12G3/02—Preparation of other alcoholic beverages by fermentation
- C12G3/026—Preparation of other alcoholic beverages by fermentation with health-improving ingredients, e.g. flavonoids, flavones, polyphenols or polysaccharides, added before or during the fermentation stage; with flavouring ingredients added before or during the fermentation stage
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a preparation method of fermented semi-sweet dendrobium candidum yellow wine, which comprises the following steps: 1. adding Dendrobium officinale refined powder into the soaked glutinous rice; 2. steaming glutinous rice and dendrobium candidum refined powder; 3. cooling and adding a distiller's yeast dropping cylinder; 4. pre-fermenting at 36-38 deg.c for 48-72 hr; 5. harrowing; 6. post-fermentation; 7. sterilizing, squeezing and clarifying when the post-fermentation physicochemical index reaches 14.0+/-0.5% of alcoholic strength, 45-55 g/L of sugar degree and 3.5-4.5g/L of acidity; 8. decocting wine at 88-89 deg.C; 9. stirring and standing the pressed raw wine for 2-3d, and clarifying; 10. and (5) sealing the jar, and storing the jar in a warehouse for ageing. The invention can more efficiently release the active ingredients such as polysaccharide, polyphenol, flavonoid and the like in the dendrobium to the yellow wine, and improve the nutrition and medicinal value of the yellow wine.
Description
Technical Field
The invention relates to a preparation method of yellow wine, in particular to a preparation method of fermented half-sweet dendrobium candidum yellow wine.
Background
Dendrobe is a traditional common traditional Chinese medicine in China, and the 5-medium-base source is the dendrobe collected in the Chinese pharmacopoeia of 2000 edition: dendrobium officinale (Dendrobium candidum wall. Ex Lindl.), dendrobium nobile (D.nobile Lindl.), dendrobium vernicifluum (D.fimbriatum hook. Var. Oculatum hook.), dendrobium chrysantheum (D.chrysanthemum wall.), dendrobium cycloartemia (D.loddigesii Rolfe.). Dendrobium officinale is one of the most resource-deficient, and is listed as an endangered medicinal material in the first book of China's rare endangered plant' in the early edition of 1989.
Dendrobium officinale is a traditional rare Chinese medicinal material in China, is also a national important protection variety, has the reputation of Chinese mesona chinensis, has thousands of years of medicinal history in China, has the statement of 'northbound ginseng and southbound dendrobe' from folk to folk, and is evaluated by Lishizhen in 'Ben Cao gang mu': "strengthen yin and replenish essence, thicken intestines and stomach, tonify internal deficiency, calm stomach qi, grow muscles, promote intelligence and remove convulsion, lighten body and prolong life". "Tang Kai" Tibet "refers to Dendrobium officinale as" the first part of Jiuda Mesona chinensis ", which is folk called" Jieduxiancao ". Compared with other dendrobium, the dendrobium candidum has higher medicinal value and has the effects of nourishing yin, promoting the production of body fluid, clearing throat, improving eyesight, moisturizing skin, protecting liver, promoting bile flow and the like.
Dendrobium officinale has a long folk eating habit, combines the traditional eating habit of China, comprehensively considers local requirements, and refers to related international management experience, and the national institute Wei Jian committee of 11 months in 2019 formally brings the dendrobium officinale into the national medicine and food homologous catalogue. As the dendrobium candidum stems are formally brought into the food and drug quality production and management test points, the dendrobium candidum will formally enter the food market, and the market demand of the dendrobium candidum will be larger and larger.
As a medicine and food homologous variety, the active ingredients in the dendrobium candidum mainly comprise chemical components such as polysaccharides, alkaloids, flavonoids, stilbenes, amino acids and the like, and the dendrobium candidum has high importance in the aspects of efficacy raw materials of medicines, health-care foods and cosmetics, such as antioxidation, anti-aging, treatment of certain diseases and the like, by scientific researchers, doctors, health-care families and cosmetic engineers.
Yellow wine (Huangjiu) is one of the oldest wines in the world, has a brewing history of over 4000 years, is derived from China, and is prepared by taking glutinous rice, millet, black rice, corn and the like as raw materials, steaming the materials, mixing with wheat yeast, rice yeast or wine medicine, saccharifying and fermenting. The alcohol content is 14-20% in general, belonging to low alcohol brewing wine. The yellow wine contains various microelements and amino acids beneficial to health, including selenium, zinc and other elements, is a wine variety which is suitable for drinking and beneficial to health, and has higher cost performance. Therefore, the yellow rice wine is more and more popular with consumers, the consumption is continuously increased, and the consumption area is gradually expanded.
The nutritional value of yellow wine exceeds that of beer and nutrient-rich wine which are called as liquid bread. Yellow wine contains multiple amino acids. According to detection, the main components in the yellow wine contain more than 18 amino acids besides ethanol and water, and 8 of the main components cannot be synthesized by a human body. The content of the 8 amino acids in the yellow wine is the most complete, and the content of the 8 amino acids is one to several times higher than that of beer and wine in the same amount, and the content of the 8 amino acids is the first of various brewed wines, especially lysine which can promote the development of human bodies. The heat energy of the yellow wine is 3-5 times of that of the beer and 1-2 times of that of the wine. The hydrogen compound is contained in an amount of 1.6 to-2.8 g/L, and the saccharide is contained in an amount of 28 to 200 g/L.
Besides, yellow wine has extremely high medicinal value, and 69 kinds of medicinal wine mentioned in Ben Cao gang mu are all prepared from yellow wine.
The Chinese patent application CN107805581A discloses a dendrobium yellow wine which is prepared by infusing medicinal materials, and medicinal components are extracted from medicinal materials such as dendrobium through alcohol in the yellow wine. The dendrobium yellow wine has the problem of low analysis rate of medicinal ingredients.
The Chinese patent application CN114231373A discloses a brewing method of dendrobium health-preserving yellow wine, which is used for preparing yellow wine by fermenting dendrobium powder and rice together. Compared with the yellow wine brewing mode, the method can improve the content of the medicinal components of the dendrobium in the yellow wine. However, the method still can not release the active ingredients such as polysaccharide, polyphenol and flavonoid in the dendrobium into the yellow wine with high efficiency.
Disclosure of Invention
The invention aims to provide a preparation method of fermented half-sweet dendrobium candidum yellow wine. The method can more efficiently release the active ingredients such as polysaccharide, polyphenol, flavonoid and the like in the dendrobium to the yellow wine, and improve the nutrition and medicinal value of the yellow wine.
The technical scheme of the invention is as follows: a preparation method of fermented semi-sweet dendrobium candidum yellow wine comprises the following steps:
1. adding Dendrobium officinale refined powder into the soaked glutinous rice;
2. steaming glutinous rice and dendrobium candidum refined powder;
3. cooling and adding a distiller's yeast dropping cylinder;
4. pre-fermenting at 36-38 deg.c for 48-72 hr; in the process, the saccharification temperature is equal to the fermentation temperature of yeast, saccharification and fermentation are alternately carried out, and the fermentation is thorough;
5. harrowing;
6. after the fermentation, the fermentation is carried out,
7. sterilizing, squeezing and clarifying when the post-fermentation physicochemical index reaches 14.0+/-0.5% of alcoholic strength, 45-55 g/L of sugar degree and 3.5-4.5g/L of acidity;
8. decocting wine at 88-89 deg.C;
9. stirring and standing the pressed raw wine for 2-3d, and clarifying;
10. and (5) sealing the jar, and storing the jar in a warehouse for ageing.
In the preparation method of the fermented semi-sweet dendrobium candidum yellow wine, the addition amount of the dendrobium candidum refined powder is 5% -8% of the brewed wine weight.
In the preparation method of the fermentation type half-sweet dendrobium candidum yellow wine, a tunnel type steam cooking machine is adopted for cooking, the temperature in the machine is 110 ℃, the pressure is 0.9MPa, and the cooking time is 12min; the temperature of the cooled mixed raw materials in the step (3) is 28-30 ℃, and the cylinder falling temperature is 26-28 ℃, so that the production efficiency can be improved, and the activity of the yeast can be ensured. When the jar temperature is too high, the saccharomycetes are deactivated due to high Wen Daliang, and when the temperature is too high, the saccharomycetes are not activated, so that the fermentation efficiency is low. The cooking operation can expand the glutinous rice serving as the grain raw material, so that the glutinous rice can reach a high-temperature and high-pressure state in a short time, and the glutinous rice is quickly deflated and depressurized to normal pressure after the cooking is finished. In the cooking process, rice grains are softened due to the high temperature and high pressure, and the water contained in the rice grains is in a liquid state with a high boiling point; deflating after the steaming is finished, and enabling the pressure to suddenly decrease, so that the moisture can be instantaneously evaporated and expanded, the internal tissues of the glutinous rice are damaged, and the subsequent fermentation process is facilitated; for the dendrobium candidum components, the effective components in the dendrobium candidum are easy to leach out by steaming and boiling, and are easy to extract in the subsequent fermentation process.
In the preparation method of the fermented half-sweet dendrobium candidum yellow wine, in the fifth step, the harrow is started for 4 times, the first harrow is started at the temperature of 34-36 ℃ for the second time after 4 hours, the temperature of the product is 34 ℃ at the moment, the third time is started after 4 hours, the temperature of the product is 32 ℃ at the moment, the fourth time is started after 3-5 hours, and the temperature of the product is 32 ℃; the temperature rise is faster after the primary fermentation stage, the yeast is easy to be attenuated, and the temperature in the jar is uniform up and down through repeated harrowing; on the other hand, a great amount of carbon dioxide exists in the discharged wine liquid; and then delivering fresh oxygen to the fermentation broth.
In the preparation method of the fermented semi-sweet dendrobium candidum yellow wine, the preparation method of the dendrobium candidum refined powder comprises the following steps:
(1) selecting fresh dendrobium candidum stem strips, cleaning, airing and cutting off to obtain dendrobium candidum strips;
(2) crushing dendrobium candidum segments, and separating liquid and slag to obtain juice and coarse slag;
(3) drying the coarse slag at high temperature, and concentrating juice at medium temperature under reduced pressure;
(4) crushing the dried coarse slag to 100-180 meshes to obtain powder A;
(5) mixing and granulating the powder A and the juice after low-temperature concentration, and naturally drying by ventilation to obtain particles B;
(6) extruding and puffing the granules B to obtain a puffed material C, and drying the puffed material C;
(7) and (3) sending the dried puffed product C into a wall breaking machine for wall breaking treatment to obtain the dendrobium candidum refined powder.
In the preparation method of the fermented half-sweet dendrobium candidum yellow wine, in the step (3), the drying temperature of the coarse slag is 90-120 ℃, and the coarse slag is dried until the water content is lower than 10%; the medium temperature and reduced pressure concentration temperature of the juice is 60-70 ℃, and the juice is concentrated into paste with the water content of 30-35%.
In the preparation method of the fermented half-sweet dendrobium candidum yellow wine, the drying temperature of the puffed material C in the step (6) is 70-90 ℃, and the puffed material C is dried until the water content is lower than 8%.
In the preparation method of the fermented half-sweet dendrobium candidum yellow wine, preferably, in the step (5), starch with a mass percentage of 1% -3% is added during mixing and granulating. More preferably, the mixture is aged for 1-2 hours after mixing to enable the starch to be incorporated into the dendrobium officinale tissue. Wherein, 2 percent of starch by mass percent is added during mixing granulation, and the effect is optimal. Because the expansion rate of the starch is obviously higher than that of the dendrobium candidum, the whole expansion rate of the dendrobium candidum can be further improved when the starch is fused into the dendrobium candidum tissue and then expanded.
In the preparation method of the fermentation type half-sweet dendrobium candidum yellow wine, in the step (5), the particle size of the particles B is 2-4mm, and the water content is 20% -25%.
Compared with the prior art, the dendrobium candidum fine powder and the glutinous rice are steamed together, so that harmful microorganisms attached to the dendrobium candidum fine powder are killed, and the dendrobium candidum powder is softened better, thereby being beneficial to degradation of effective components and functions of the dendrobium candidum fine powder by the microorganisms; meanwhile, as the dendrobium candidum powder and the glutinous rice are fermented together, the dendrobium candidum powder participates in the whole fermentation process, and microorganisms fully utilize the nutrient substances of the dendrobium candidum and the glutinous rice, so that macromolecular substances are fully degraded, and the dendrobium candidum powder is favorable for human absorption. In addition, the yellow wine contains rich proteins, amino acids and rich microelements, and can be complemented with polysaccharide, oligosaccharide and the like in the dendrobium candidum, so that the nutritional value and the health care effect of the yellow wine can be effectively improved. The preparation method of the fermented half-sweet dendrobium candidum yellow wine does not need to greatly increase equipment and investment, has simple process procedures and easily controlled quality.
On the other hand, the preparation process of the dendrobium candidum refined powder is improved, so that the process market can be reduced, and the release of nutrients is lower than that of the dendrobium candidum refined powder, so that the final yellow wine product can contain more nutrients: according to the invention, the fresh dendrobium candidum stem strips are crushed and subjected to slag-liquid separation, the fresh dendrobium candidum stem strips are separated into coarse slag mainly containing coarse fibers and juice containing most of nutrients, and the two components are subjected to drying and concentration treatment respectively, so that the influence of high-temperature drying on the nutrient components of dendrobium candidum can be reduced. And then the two materials are mixed again by using a granulating process, so that various substances in the original dendrobium candidum can be mixed more uniformly, and compared with the segment state, the particle has better air permeability, and the moisture content can be reduced rapidly by using simple ventilation and natural drying. On the basis, the invention can solve the problem of influence of fiber stress on puffing in the prior art by reusing the extrusion puffing process, so that the puffing degree is greatly improved, and the porosity of the puffed material is higher. And finally, the refined powder obtained after being crushed by a wall breaking machine can also have a loose structure in the powder, so that the release of nutrient substances is facilitated, and the utilization rate of active ingredients of the refined powder can be greatly improved no matter the refined powder is used for extracting the nutrient substances or is directly eaten.
Drawings
FIG. 1 is a graph of the change in alcoholicity during the post-fermentation process of example 7 of the invention;
FIG. 2 is a graph of the post-fermentation process reducing sugar change of example 7 of the present invention;
FIG. 3 is a graph showing the total acid change in the post-fermentation process of example 7 of the present invention;
FIG. 4 is a graph showing the change in yeast amount during the post-fermentation in example 7 of the present invention.
Detailed Description
The invention is further illustrated by the following figures and examples, which are not intended to be limiting.
Examples:
1. the preparation process of the dendrobium candidum refined powder is compared.
Design example 6, using the same process as follows, only part of the parameters were adjusted: (1) selecting fresh dendrobium candidum stem strips, cleaning, airing and cutting off to obtain dendrobium candidum strips;
(2) crushing dendrobium candidum segments, and separating liquid and slag to obtain juice and coarse slag;
(3) drying the coarse slag at high temperature until the water content is lower than 10%; concentrating the juice at medium temperature under reduced pressure to obtain paste with water content of 30%;
(4) crushing the dried coarse slag to 100-180 meshes to obtain powder A;
(5) mixing and granulating the powder A and the juice after low-temperature concentration, and naturally drying by ventilation to obtain particles B; the particle size of the particles B is 2-4mm, and the water content is 20%;
(6) the pellets B were subjected to extrusion expansion treatment (7.5 kgf/cm) 2 ) Obtaining a puffed material C, and drying the puffed material C until the water content is lower than 8%;
(7) and (3) sending the dried puffed product C into a wall breaking machine for wall breaking treatment to obtain the dendrobium candidum refined powder.
In comparative example 1, fresh strips of dendrobium candidum stem are adopted, dried at 140 ℃ until the water content reaches below 8%, and then treated into fine powder by a wall breaking machine.
Comparative example 2, using fresh strips of Dendrobium officinale stem, oven drying at 140deg.C until the water content is below 8%, and extrusion puffing (7.5 kgf/cm) 2 ) Then, the mixture is processed into fine powder by using a wall breaking machine.
Comparative example 3, using fresh strips of Dendrobium officinale stem, oven drying at 140deg.C until the water content is below 8%, and extrusion puffing (9 kgf/cm) 2 ) Then, the mixture is processed into fine powder by using a wall breaking machine.
The following specific examples and comparative examples were obtained by adjusting the respective process descriptions with respect to the above-described processes of the present invention.
In example 6, starch and vegetable oil were added in an amount of 2% by mass and 0.3% by mass, respectively, in the course of granulation in combination with the base of example 2.
In each example and comparative example, 10 batches of fresh dendrobium candidum stem strips in the same batch are prepared respectively, and the refined powder of 10 batches is mixed for use as a final experiment.
From the comparison of the weight of the fresh branch of dendrobium candidum required for preparing the fine powder with the same weight, the utilization rate of the fresh branch of dendrobium candidum in the examples 1-6 is obviously higher than that of other comparative examples. Since a certain amount of starch is added in example 6, and the amount of starch should be deducted when comparing, 3.5g of starch and 0.5g of vegetable oil are added for every 100g of dendrobium nobile refined powder in example 6, the use of 238.2g of fresh dendrobium candidum strips in example 6 can be calculated to prepare 96g of refined powder, and the conversion can prepare 100g of refined powder, 248.1g is needed, and still less is needed than other examples.
Comparative experiment 1. Solvent separation extraction of Dendrobium officinale.
The experimental method comprises the following steps: respectively extracting with 70% ethanol, n-hexane and ethyl acetate, separating, and collecting extract components with different polarities. Taking 100g of dried dendrobium candidum powder, adding 4 times of 70% ethanol for leaching, centrifuging, removing ethanol precipitate, taking supernatant, concentrating, drying, and pulverizing to obtain crude extract DOE powder.
Dissolving DOE in 500ml distilled water, fully mixing with n-hexane according to a ratio of 1:1, standing and extracting for 1 hour in a separating funnel, collecting the uppermost nonpolar extract and the lowermost aqueous layer extract of the extract, concentrating, drying and pulverizing respectively to obtain extract components DOH and DOW1.
Dissolving DOW1 in 500ml distilled water, fully mixing with ethyl acetate according to a ratio of 1:1, standing and extracting for 1 hour in a separating funnel, collecting an upper layer and a lower layer of an extract, concentrating, drying and crushing respectively to obtain extract components DOEA and DOW2.
The yields of DOE, DOW1, DOEA and DOW2 were measured.
Comparative experiment 2. Analysis of polysaccharide, polyphenol and flavonoid content (mainly for crude extract DOE).
The polysaccharide content is detected by a phenol-sulfuric acid method.
The polyphenol content is detected by adopting a Fu Lin Fen method.
The total flavonoid content was measured by DMACA method.
Experimental results.
Comparing the results.
Table 1. Yields of doh, DOE, DOW1, DOEA and DOW2.
The results show that the yields of the extracts of example 6 are the highest in many examples, while the yields of the individual extracts of examples 1-5 are comparable to those of comparative examples 2 and 3 (the extraction method disclosed in CN107981352 a), but the yields of the other extracts are further improved, which is a more remarkable omnibearing improvement compared with comparative example 1, so that the method of the invention can further improve the release of nutrients in the dendrobium officinale fine powder. Comparative examples 4 to 7 have a problem that the yield of individual extracts is low although the yield of individual extracts is high, because of the problem of temperature control, which results in denaturation of a part of the nutrients, which cannot be obtained by the extraction method.
2. The crude extract contains polysaccharides, polyphenols and flavonoids.
TABLE 2 content of polysaccharide, polyphenol and flavonoid in DOE
The results show that the polysaccharide, polyphenol and flavonoid contents of examples 1-6 are generally higher than those of the comparative examples, and that examples 2 and 3, although comparable in percentage of these several ingredients to the examples, are relatively small in terms of the amount of these nutrients because the dry basis weight itself is smaller than that of the examples.
In conclusion, when the method is used for preparing the dendrobium candidum refined powder, the utilization rate of fresh branches of dendrobium candidum is greatly improved, and the obtained dendrobium candidum refined powder has higher yield when being extracted, so that the method is also beneficial to releasing nutrient substances of dendrobium candidum. Finally, the content of polysaccharide, polyphenol and flavonoid in the crude extract is measured, so that the dendrobium candidum refined powder prepared by the method can well retain the nutritional ingredients of dendrobium candidum.
2. The preparation process of the yellow wine is compared.
Design example 7: a preparation method of fermented half-sweet dendrobium candidum yellow wine comprises the following steps.
1. Adding dendrobium candidum refined powder on the soaked glutinous rice, wherein the adding amount of the dendrobium candidum refined powder is 5% of the weight of brewed wine, and the dendrobium candidum refined powder is prepared by adopting the method of the optimal example 6;
2. steaming glutinous rice and dendrobium candidum refined powder; adopting a tunnel steam cooking machine to cook, wherein the temperature in the machine is 110 ℃, the pressure is 0.9MPa, and the cooking time is 12min; the temperature of the mixed raw materials after cooling in the step (3) is 28-30 ℃, and the cylinder falling temperature is 26-28 ℃;
3. cooling, adding distiller's yeast jar, and mixing distiller's yeast with rhizopus yeast;
4. pre-fermenting at 36 deg.c for 72 hr;
5. harrowing; the harrow is started for 4 times, the temperature of the head harrow is controlled to be 34-36 ℃, the harrow is started for the second time after 4 hours, the temperature of the head harrow is 34 ℃, the harrow is started for the third time after 4 hours, the temperature of the head harrow is 32 ℃, the harrow is started for the fourth time after 3-5 hours, and the temperature of the head harrow is 32 ℃;
6. after the fermentation, the fermentation is carried out,
7. sterilizing, squeezing and clarifying when the post-fermentation physicochemical index reaches 14.0+/-0.5% of alcoholic strength, 45-55 g/L of sugar degree and 3.5-4.5g/L of acidity; the specific index changes are shown in fig. 1.
8. Decocting wine at 88-89 deg.C;
9. stirring and standing the pressed raw wine for 2-3d, and clarifying;
10. and (5) sealing the jar, and storing the jar in a warehouse for ageing.
Comparative example 8, which was prepared by the same process as in example 7, except that the dendrobium candidum fine powder was replaced with comparative example 1.
Comparative example 9, the same refined dendrobium candidum powder as in example 7 was used, but the refined dendrobium candidum powder and distiller's yeast were put into a jar without cooking.
And (5) comparing experiments. 93.75g
1. Wine yield comparison (per 1kg of glutinous rice).
In conclusion, in the embodiment 7 of the invention, the obtained yellow wine has obviously improved alcoholicity and dendrobium polysaccharide content compared with the comparative examples 8 and 9. In comparative example 8, even though the same process as in example 7 is adopted, the dendrobium polysaccharide content in the final yellow wine is relatively low because the conventional dendrobium officinale fine powder has relatively weak nutrient release capability. In contrast, in comparative example 9, the release of dendrobium candidum polysaccharide is less than in example 7 because the dendrobium candidum refined powder is not involved in the cooking process.
Claims (10)
1. The preparation method of the fermented semi-sweet dendrobium candidum yellow wine is characterized by comprising the following steps of:
1. adding Dendrobium officinale refined powder into the soaked glutinous rice;
2. steaming glutinous rice and dendrobium candidum refined powder;
3. cooling and adding a distiller's yeast dropping cylinder;
4. pre-fermenting at 36-38 deg.c for 48-72 hr;
5. harrowing;
6. post-fermentation;
7. sterilizing, squeezing and clarifying when the post-fermentation physicochemical index reaches 14.0+/-0.5% of alcoholic strength, 45-55 g/L of sugar degree and 3.5-4.5g/L of acidity;
8. decocting wine at 88-89 deg.C;
9. stirring and standing the pressed raw wine for 2-3d, and clarifying;
10. and (5) sealing the jar, and storing the jar in a warehouse for ageing.
2. The preparation method of the fermented semi-sweet dendrobium candidum yellow wine according to claim 1, which is characterized in that: the adding amount of the dendrobium candidum refined powder is 5% -8% of the weight of brewed wine.
3. The preparation method of the fermented semi-sweet dendrobium candidum yellow wine according to claim 1, which is characterized in that: the second step adopts a tunnel type steam cooking machine for cooking, the temperature in the machine is 110 ℃, the pressure is 0.9MPa, and the cooking time is 12min; the temperature of the mixed raw materials after cooling in the step (3) is 28-30 ℃, and the cylinder falling temperature is 26-28 ℃.
4. The preparation method of the fermented semi-sweet dendrobium candidum yellow wine according to claim 1, which is characterized in that: in the fifth step, the harrow is started for 4 times, the temperature of the head harrow is controlled to be 34-36 ℃, the harrow is started for the second time after 4 hours, the temperature of the head harrow is 34 ℃, the harrow is started for the third time after 4 hours, the temperature of the head harrow is 32 ℃, the harrow is started for the fourth time after 3-5 hours, and the temperature of the head harrow is 32 ℃.
5. The preparation method of the fermented semi-sweet dendrobium candidum yellow wine according to claim 1, wherein the preparation method of the dendrobium candidum fine powder in the second step comprises the following steps:
(1) selecting fresh dendrobium candidum stem strips, cleaning, airing and cutting off to obtain dendrobium candidum strips;
(2) crushing dendrobium candidum segments, and separating liquid and slag to obtain juice and coarse slag;
(3) drying the coarse slag at high temperature, and concentrating juice at medium temperature under reduced pressure;
(4) crushing the dried coarse slag to 100-180 meshes to obtain powder A;
(5) mixing and granulating the powder A and the juice after low-temperature concentration, and naturally drying by ventilation to obtain particles B;
(6) extruding and puffing the granules B to obtain a puffed material C, and drying the puffed material C;
(7) and (3) sending the dried puffed product C into a wall breaking machine for wall breaking treatment to obtain the dendrobium candidum refined powder.
6. The preparation method of the fermented half-sweet dendrobium candidum yellow wine according to claim 5, which is characterized in that: in the step (3), the drying temperature of the coarse slag is 90-120 ℃, and the coarse slag is dried until the water content is lower than 10%; the medium temperature and reduced pressure concentration temperature of the juice is 60-70 ℃, and the juice is concentrated into paste with the water content of 30-35%.
7. The preparation method of the fermented half-sweet dendrobium candidum yellow wine according to claim 5, which is characterized in that: and (3) drying the puffed material C in the step (6) at a temperature of 70-90 ℃ until the water content is lower than 8%.
8. The preparation method of the fermented half-sweet dendrobium candidum yellow wine according to claim 5, which is characterized in that: in the step (5), starch with the mass percentage of 1-3% is added during mixing granulation.
9. The preparation method of the fermented semi-sweet dendrobium candidum yellow wine of claim 8, which is characterized in that: in the step (5), starch with a mass percentage of 2% is added during mixing granulation.
10. The preparation method of the fermented half-sweet dendrobium candidum yellow wine according to claim 5, which is characterized in that: in the step (5), the particle size of the particles B is 2-4mm, and the water content is 20% -25%.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101810330A (en) * | 2010-04-19 | 2010-08-25 | 奉化益珍海藻科技有限公司 | Enteromorpha clathrata-dendrobium refined flour |
CN103865721A (en) * | 2014-03-22 | 2014-06-18 | 浙江农林大学 | Dendrobium officinale wheat-starter yellow rice wine and brewing method thereof |
CN105983061A (en) * | 2015-03-04 | 2016-10-05 | 安徽千方生物科技有限公司 | Preparation process for active dendrobium officinale freeze-dried powder |
CN107981352A (en) * | 2017-10-20 | 2018-05-04 | 植然方适(杭州)健康科技有限公司 | A kind of preparation method and applications of high anti-oxidation activity iron sheet Herba Dendrobii extract |
CN110951574A (en) * | 2019-12-23 | 2020-04-03 | 清华大学无锡应用技术研究院 | Method for jointly producing yellow wine and table vinegar by utilizing dendrobium |
CN113388471A (en) * | 2021-06-24 | 2021-09-14 | 贵州大学 | Preparation method of dendrobium rice wine |
-
2023
- 2023-06-09 CN CN202310682050.1A patent/CN116515579A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101810330A (en) * | 2010-04-19 | 2010-08-25 | 奉化益珍海藻科技有限公司 | Enteromorpha clathrata-dendrobium refined flour |
CN103865721A (en) * | 2014-03-22 | 2014-06-18 | 浙江农林大学 | Dendrobium officinale wheat-starter yellow rice wine and brewing method thereof |
CN105983061A (en) * | 2015-03-04 | 2016-10-05 | 安徽千方生物科技有限公司 | Preparation process for active dendrobium officinale freeze-dried powder |
CN107981352A (en) * | 2017-10-20 | 2018-05-04 | 植然方适(杭州)健康科技有限公司 | A kind of preparation method and applications of high anti-oxidation activity iron sheet Herba Dendrobii extract |
CN110951574A (en) * | 2019-12-23 | 2020-04-03 | 清华大学无锡应用技术研究院 | Method for jointly producing yellow wine and table vinegar by utilizing dendrobium |
CN113388471A (en) * | 2021-06-24 | 2021-09-14 | 贵州大学 | Preparation method of dendrobium rice wine |
Non-Patent Citations (2)
Title |
---|
周美玲等: "铁皮石斛黄酒工艺优化及其抗氧化活性的研究", 江西农业学报, vol. 33, no. 05, 15 May 2021 (2021-05-15), pages 97 * |
徐兴阳等: "香菇粉挤压膨化产品研发及其性质研究", 食品研究与开发, vol. 37, no. 01, 10 January 2016 (2016-01-10), pages 85 - 89 * |
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