CN111500394A - Rosa roxburghii enzyme ice-melting wine and preparation process thereof - Google Patents

Rosa roxburghii enzyme ice-melting wine and preparation process thereof Download PDF

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CN111500394A
CN111500394A CN202010467330.7A CN202010467330A CN111500394A CN 111500394 A CN111500394 A CN 111500394A CN 202010467330 A CN202010467330 A CN 202010467330A CN 111500394 A CN111500394 A CN 111500394A
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rosa roxburghii
roxburghii tratt
temperature
enzyme
ice wine
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王瑜
杨小生
李立郎
杨娟
王道平
杨礼寿
万科
葛丽娟
高明
李良群
罗忠圣
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Key Laboratory of Natural Product Chemistry of Guizhou Academy of Sciences
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    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12GWINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
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    • C12G3/024Preparation of other alcoholic beverages by fermentation of fruits other than botanical genus Vitis
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    • C12H6/04Methods for increasing the alcohol content of fermented solutions or alcoholic beverages by freezing

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Abstract

The invention discloses a rosa roxburghii tratt enzyme iced wine which comprises, by weight, 40-50 parts of rosa roxburghii tratt fresh fruits, 30-60 parts of tea water, 10-20 parts of white sugar, 0.3-0.5 part of low-temperature yeast, 0.3-0.7 part of pectinase and 0.3-0.7 part of cellulase, wherein the alcoholicity of the rosa roxburghii tratt enzyme iced wine is 5-8% vol, and the sugar content of the rosa roxburghii tratt enzyme ice wine is 8-12%. The invention also discloses a preparation process of the rosa roxburghii tratt enzymatic ice wine. The reduction of the relative contents of acids and aldehydes in the volatile substances of the rosa roxburghii tratt enzymatic ice wine relieves the irritating sour taste and unpleasant peculiar smell of rosa roxburghii tratt caused by high-concentration acids and aldehydes, and the invention can also increase the fruit fragrance and ester fragrance of the product. The rosa roxburghii tratt enzyme iced wine disclosed by the invention is good in nutritive value, flavor and taste, free of potential food safety hazards and short in fermentation period.

Description

Rosa roxburghii enzyme ice-melting wine and preparation process thereof
Technical Field
The invention relates to the technical field of rosa roxburghii tratt enzymes, in particular to rosa roxburghii tratt enzyme ice-melting wine and a preparation process thereof.
Background
The Rosa roxburghii (Rosa steriis) is also called seedless Rosa roxburghii, is a fruit tree which is produced in early period, has high yield, developed root system and vigorous growth, is a green health food which can be used as food and medicine, is a special strain of Guizhou province, has higher nutrition and health care value, is called as 'Xinshan Zhen', is rich in vitamin C, folic acid, carotene, superoxide dismutase, amino acids required by human bodies and the like, also contains aspartic acid for resisting leukemia and also has the oxidation resistance. The rosa roxburghii tratt is a third-generation wild fruit tree with great development and utilization values, prolongs the life when eaten, and is a good product for human nutrition and health care. The Rosa roxburghii is planted and cultivated in a large area in Anshun city of Guizhou province, and deep processing and new product development and research are urgently needed.
At present, the related deep-processed products of the rosa roxburghii tratt on the market are mainly rosa roxburghii tratt juice and rosa roxburghii tratt blended beverage, the rosa roxburghii tratt juice is generally squeezed by a belt squeezing technology, and then subjected to high-temperature instantaneous sterilization treatment, and then aseptically filled to obtain a finished product, so that the active ingredients and the nutrient substances contained in the rosa roxburghii tratt can be retained to the maximum extent, but the rosa roxburghii tratt juice has sour and astringent taste after eating due to the acids, aldehydes and tannin substances contained in the rosa roxburghii tratt juice, and has special flavor, so that consumers are difficult to experience again unless the consumers who know the rosa roxburghi. Most consumers are willing to experience the golden roxburgh rose harmony beverage, the golden roxburgh rose harmony beverage covers unacceptable taste of the golden roxburgh rose by adding a series of food additives such as a flavoring agent, a sweetening agent and the like, but some unhealthy factors are introduced, so that the golden roxburgh rose harmony beverage is required by the current market to develop a golden roxburgh rose product which can retain nutritional active ingredients in the golden roxburgh rose and improve the flavor.
A large number of researches show that the enzyme technology can increase the added value of fruit and vegetable plants, and under the action of the microbial flora secretase, macromolecular substances in a fermentation substrate can be converted into micromolecular substances which are convenient for a human body to absorb, and meanwhile, the generated secondary metabolite increases the nutritional efficacy and flavor components of the product, thereby not only improving the nutritional value of the fermentation raw material, but also changing the tissue state and flavor of the product.
The traditional natural fermentation process is adopted to ferment the rosa roxburghii tratt, the fermentation time is generally 3-6 months, the fermentation period is long, the microbial flora is not easy to control, the nutritional value and the flavor of the fermented product are difficult to ensure, the taste is rough, and even food safety accidents can be caused by introducing mixed bacteria.
Therefore, the development of a rosa roxburghii tratt enzyme product which has good nutritive value, flavor and taste, no food safety hidden danger and short fermentation period is necessary.
Disclosure of Invention
The invention aims to provide a rosa roxburghii tratt enzyme iced wine and a preparation process thereof. The rosa roxburghii tratt enzyme iced wine disclosed by the invention is good in nutritive value, flavor and taste, free of potential food safety hazards and short in fermentation period.
The technical scheme of the invention is as follows: the rosa roxburghii tratt enzyme iced wine comprises, by weight, 40-50 parts of fresh rosa roxburghii tratt fruits, 30-60 parts of tea water, 10-20 parts of white sugar, 0.3-0.5 part of low-temperature yeast, 0.3-0.7 part of pectinase and 0.3-0.7 part of cellulase, wherein the alcoholic strength of the rosa roxburghii tratt enzyme iced wine is 5-8% vol, and the sugar content of the rosa roxburghii tratt enzyme iced wine is 8-12%.
The rosa roxburghii tratt enzymatic ice wine comprises, by weight, 42-48 parts of fresh rosa roxburghii tratt fruits, 40-50 parts of tea water, 12-18 parts of white sugar, 0.35-0.45 part of low-temperature yeast, 0.4-0.6 part of pectinase and 0.4-0.6 part of cellulase, wherein the alcoholic strength of the rosa roxburghii tratt enzymatic ice wine is 5-8% vol, and the sugar content of the rosa roxburghii tratt enzymatic ice wine is 8-12%.
The rosa roxburghii tratt enzyme-treated ice wine comprises, by weight, 45 parts of fresh rosa roxburghii tratt fruits, 45 parts of tea water, 15 parts of white sugar, 0.4 part of low-temperature yeast, 0.5 part of pectinase and 0.5 part of cellulase, wherein the tea water is black tea water, the weight ratio of the black tea to the water is 1:80, the alcoholic strength of the rosa roxburghii tratt enzyme-treated ice wine is 5% -8% vol, and the sugar content of the rosa roxburghii tratt enzyme-treated ice wine is 8% -12%.
In the rosa roxburghii tratt enzyme iced wine, the tea water is black tea water, wherein the weight ratio of black tea to water is 1: 50-100.
In the rosa roxburghii tratt enzymatic ice wine, the black tea water is prepared by adding black tea into water with the temperature of 20-30 ℃ for soaking for 5-10min, boiling and keeping for 3-5min, and filtering out tea leaves to obtain the black tea water.
In the above mentioned rosa roxburghii tratt enzymatic iced wine, the activity of the pectinase is 20000u/g, and the activity of the cellulase is 2000 u/g.
In the rosa roxburghii tratt enzymatic ice wine, the low-temperature yeast is obtained by domesticating Angel BV818 grape seedling bacteria powder at 8-10 ℃.
The preparation method of the rosa roxburghii tratt enzymatic ice wine comprises the following steps,
a. tea water fixation: removing pedicel from fresh fructus Rosae Normalis, cleaning, draining, adding white sugar, boiling in tea water, and keeping for 5-10min to obtain product A;
b. quick-freezing treatment: cooling product A to room temperature, freezing at-23 deg.C to-13 deg.C for 5-10h, pulping in frozen state, and crushing to obtain fructus Rosae Normalis pulp B;
c. low-temperature fermentation: transferring product B to a fermentation tank, controlling the temperature in the fermentation tank to be 20-30 ℃, adding cellulase and pectinase, adjusting the temperature in the fermentation tank to be 10-20 ℃, adding activated low-temperature yeast, adjusting the temperature in the fermentation tank to be 5-10 ℃, introducing oxygen for fermentation for 14-20 days, and stopping fermentation when the sugar degree is measured to be 8% -10% to obtain product C;
d. filter pressing clarification: filter-pressing product C to remove fruit residues, adding diatomite for natural clarification, and sterilizing the supernatant at 130 deg.C and 120 deg.C by ultra-high temperature instantaneous sterilization device to obtain product D;
e. freezing and concentrating: and (3) placing the product D at a temperature of between 5 ℃ below zero and 0 ℃ to obtain an ice-water mixture, separating and removing ice blocks until the alcoholic strength in the liquid is 5 to 8 percent vol, and thus obtaining the rosa roxburghii tratt enzymatic ice wine.
In the preparation method of the rosa roxburghii tratt enzymatic ice wine, in the step c, the activated low-temperature yeast is prepared by adding the low-temperature yeast into white sugar water with the temperature of 20-35 ℃ and the mass fraction of 3-5%, stirring and standing for 15-30 minutes to obtain the activated low-temperature yeast.
In the preparation method of the rosa roxburghii tratt enzymatic ice wine, in the step c, the oxygen is introduced to 25-30% of the volume fraction of oxygen in the air in the fermentation tank. The oxygen introduction amount can promote the rapid propagation and growth of microorganisms, enter a logarithmic phase, accelerate the decomposition of macromolecular substances into micromolecular substances and avoid the influence on flavor and taste caused by the accumulation of a large amount of ethanol which is a main metabolite of low-temperature yeast when the microorganisms enter a stationary phase in advance.
In the preparation method of the rosa roxburghii tratt enzymatic ice wine, in the step d, the adding amount of the diatomite is 1-3% of the weight of the product C after the pomace is removed.
In the preparation method of the rosa roxburghii tratt enzymatic ice wine, the alcoholic strength of the product D is 3-4% vol.
Compared with the prior art, the invention provides the formula of the golden roxburgh rose ferment iced wine taking the fresh golden roxburgh rose fruits, the tea water, the white sugar, the low-temperature yeast, the pectinase and the cellulase as the raw materials, the invention uses the single low-temperature yeast for fermentation, and the prepared golden roxburgh rose ferment iced wine has better nutritional value according to the mixture ratio of the raw materials in the invention, can remove irritant sour taste and unpleasant peculiar smell in volatile substances in the wine, and has better flavor and taste; according to the invention, the black tea is adopted for green removing treatment, so that on one hand, the loss of active ingredients in the rosa roxburghii tratt is reduced by using antioxidant ingredients (tea polyphenol) in the tea, and meanwhile, microorganisms carried by the rosa roxburghii tratt can be effectively killed so as to avoid influencing later-stage fermentation, and a foundation is laid for later-stage pure yeast targeted fermentation; the method adopts oxygen-introducing low-temperature fermentation, and the oxygen-introducing fermentation can promote the rapid propagation and growth of microorganisms, enter a logarithmic phase and accelerate the decomposition of macromolecular substances into micromolecular substances so as to prevent the influence on flavor and taste caused by the accumulation of a large amount of ethanol which is a main metabolite of low-temperature yeast when the microorganisms enter a stationary phase in advance; the invention utilizes the principle that ethanol and water are different in freezing point, and removes part of water in the Rosa roxburghii enzymatic fermentation broth in an ice manner to achieve the purpose of freeze concentration, wherein the mass fraction of ethanol in the oxygen-introducing fermentation product is 3-5%, the set temperature is-5-0 ℃, the state of ice-water mixing can be achieved, and the purpose of freeze concentration can be achieved by deicing; according to the method, most aldehydes in volatile substances of the rosa roxburghii tratt fruit pulp can be converted into organic acids through fermentation, meanwhile, the generated alcohols and a large amount of ester substances can improve the fruit fragrance and ester fragrance properties of the product, so that the relative content of the acids and the aldehydes in the volatile substances of the rosa roxburghii tratt enzymatic ice wine is reduced, and the irritating sour taste and unpleasant peculiar smell of rosa roxburghii tratt caused by high-concentration acids and aldehydes are relieved. The fermentation time of the invention is less than 1 month, and the fermentation time is shorter. The rosa roxburghii tratt enzyme iced wine disclosed by the invention is good in nutritive value, flavor and taste, free of potential food safety hazards and short in fermentation period.
Drawings
FIG. 1 is an ion chromatogram of flavor of sample B in example 3;
FIG. 2 is an ion chromatogram of flavor ion stream of sample E in example 3.
Detailed Description
The invention is further illustrated by the following figures and examples, which are not to be construed as limiting the invention.
Example 1. The Rosa roxburghii enzymatic ice wine comprises the following raw materials in parts by weight: 40 parts of fresh rosa roxburghii tratt fruit, 60 parts of tea water, 10 parts of white sugar, 0.5 part of low-temperature yeast, 0.3 part of pectinase and 0.7 part of cellulase, wherein the tea water comprises the following components in parts by weight: 1/50 the preparation method comprises soaking black tea in water at 20 deg.C for 10min, boiling for 3min, and filtering to obtain tea solution.
The low-temperature yeast is obtained by domesticating Angel BV818 grape seedling bacterial powder at 9 ℃.
The preparation process of the rosa roxburghii tratt enzymatic ice wine comprises the following steps:
A. tea water fixation: removing flower stalks of fresh rosa roxburghii tratt fruits, cleaning and draining, adding the fresh rosa roxburghii tratt fruits and white sugar into prepared tea water according to the feeding proportion of fermentation raw materials, boiling and keeping for 5 minutes to complete tea water enzyme deactivation;
B. quick-freezing treatment: cooling the tea water containing the rosa roxburghii tratt fruit obtained in the step A to normal temperature, then placing the cooled tea water in a quick-freezing cold storage at the temperature of minus 23 ℃ for freezing for 10 hours, and pulping and crushing the cooled tea water in an icing state to obtain rosa roxburghii tratt fruit pulp;
C. low-temperature fermentation: transferring the Rosa roxburghii fruit pulp obtained in the step B to a fermentation tank, adding cellulase and pectinase according to a proportion when the temperature in the fermentation tank reaches 20 ℃, adjusting the temperature in the fermentation tank to be 10 ℃, adding activated low-temperature yeast according to the feeding proportion of fermentation raw materials, adjusting the temperature of the fermentation tank to be 5 ℃, introducing oxygen until the volume fraction of oxygen in the air in the fermentation tank is 25%, fermenting for 20 days, and stopping fermentation when the sugar degree is measured to be 8%; the preparation method of the activated low-temperature yeast comprises the steps of adding the low-temperature yeast into white sugar water with the temperature of 20 ℃ and the mass fraction of 3%, stirring and standing for 15 minutes to obtain the activated low-temperature yeast;
D. filter pressing clarification: removing fruit residues from fermented Rosa roxburghii by using a filter pressing device, adding diatomite for natural clarification, taking supernatant, and sterilizing by using an ultrahigh temperature instantaneous sterilization device at a sterilization temperature of 120 ℃;
E. and D, freezing and concentrating, namely, setting the alcoholic strength of the rosa roxburghii tratt fermentation liquor treated in the step D to be 3% vol, placing the fermentation liquor at the temperature of 0 ℃ to obtain an ice-water mixture, separating and removing ice blocks, and determining that the alcoholic strength of the liquid is 5%, so that the rosa roxburghii tratt enzymatic ice wine is obtained.
Wherein in the step C, in the low-temperature fermentation link, the activity of the pectinase is 20000u/g, and the activity of the cellulase is 2000 u/g; and D, performing filter pressing clarification, wherein the dosage of the diatomite accounts for 1 percent of the weight of the fermentation liquor to be clarified.
The alcoholic strength of the finally obtained rosa roxburghii tratt enzyme iced wine is 5% vol, and the sugar degree is 10%.
Example 2. The Rosa roxburghii enzymatic ice wine comprises the following raw materials in parts by weight: 50 parts of fresh rosa roxburghii tratt fruit, 30 parts of tea water, 20 parts of white sugar, 0.3 part of low-temperature yeast, 0.7 part of pectinase and 0.3 part of cellulase, wherein the tea water comprises the following components in parts by weight: 1/100 the preparation method comprises soaking black tea in water at 30 deg.C for 5min, boiling for 5min, and filtering to obtain tea solution.
The low-temperature yeast is obtained by domesticating Angel BV818 grape seedling bacterial powder under 9.
The preparation process of the rosa roxburghii tratt enzymatic ice wine comprises the following steps:
A. tea water fixation: removing flower stalks of fresh rosa roxburghii tratt fruits, cleaning and draining, adding the fresh rosa roxburghii tratt fruits and white sugar into prepared tea water according to the feeding proportion of fermentation raw materials, boiling and keeping for 10 minutes to complete tea water enzyme deactivation;
B. quick-freezing treatment: cooling the tea water containing the rosa roxburghii tratt fruit obtained in the step A to normal temperature, then placing the cooled tea water in a quick-freezing cold storage at the temperature of-13 ℃ for freezing for 5 hours, and pulping and crushing the cooled tea water in an icing state to obtain rosa roxburghii tratt fruit pulp;
C. low-temperature fermentation: transferring the Rosa roxburghii fruit pulp obtained in the step B to a fermentation tank, adding cellulase and pectinase according to a proportion when the temperature in the fermentation tank reaches 30 ℃, adjusting the temperature in the fermentation tank to be reduced to 20 ℃, adding activated low-temperature yeast according to the feeding proportion of fermentation raw materials, adjusting the temperature of the fermentation tank to be 10 ℃, introducing oxygen until the volume fraction of oxygen in the air in the fermentation tank is 30%, fermenting for 14 days, and stopping fermentation when the sugar degree is measured to be 10%;
the preparation method of the activated low-temperature yeast comprises the steps of adding the low-temperature yeast into white sugar water with the temperature of 35 ℃ and the mass fraction of 5%, stirring and standing for 30 minutes to obtain the activated low-temperature yeast;
D. filter pressing clarification: removing fruit residues from fermented Rosa roxburghii by using a filter pressing device, adding diatomite for natural clarification, taking supernatant, and sterilizing by using an ultrahigh temperature instantaneous sterilization device at a sterilization temperature of 130 ℃;
E. and D, freezing and concentrating, namely, setting the alcoholic strength of the rosa roxburghii tratt fermentation liquor treated in the step D to be 4% vol, placing the fermentation liquor at the temperature of minus 5 ℃ to obtain an ice-water mixture, separating and removing ice blocks, and determining that the alcoholic strength of the liquid is 8%, so that the rosa roxburghii tratt enzymatic ice wine is obtained.
Wherein in the step C, in the low-temperature fermentation link, the activity of the pectinase is 20000u/g, and the activity of the cellulase is 2000 u/g; and D, performing filter pressing clarification, wherein the dosage of the diatomite accounts for 1 percent of the weight of the fermentation liquor to be clarified.
The alcoholic strength of the finally obtained rosa roxburghii tratt enzyme iced wine is 8% vol, and the sugar degree is 12%.
Example 3. The Rosa roxburghii enzymatic ice wine comprises the following raw materials in parts by weight: 45 parts of fresh rosa roxburghii tratt fruit, 45 parts of tea water, 15 parts of white sugar, 0.4 part of low-temperature yeast, 0.5 part of pectinase and 0.5 part of cellulase, wherein the tea water comprises the following components in parts by weight: 1/80 the preparation method comprises soaking black tea in water at 25 deg.C for 8min, boiling for 4 min, and filtering to obtain tea solution.
The low-temperature yeast is obtained by domesticating Angel BV818 grape seedling bacterial powder at 9 ℃.
The preparation process of the rosa roxburghii tratt enzymatic ice wine comprises the following steps:
A. tea water fixation: removing flower stalks of fresh rosa roxburghii tratt fruits, cleaning and draining, adding the fresh rosa roxburghii tratt fruits and white sugar into prepared tea water according to the feeding proportion of fermentation raw materials, boiling and keeping for 8 minutes to complete tea water enzyme deactivation;
B. quick-freezing treatment: cooling the tea water containing the rosa roxburghii tratt fruit obtained in the step A to normal temperature, then placing the cooled tea water in a quick-freezing cold storage at the temperature of 18 ℃ below zero for freezing for 8 hours, and pulping and crushing the cooled tea water in an icing state to obtain rosa roxburghii tratt fruit pulp;
C. low-temperature fermentation: transferring the Rosa roxburghii fruit pulp obtained in the step B to a fermentation tank, adding cellulase and pectinase according to a proportion when the temperature in the fermentation tank reaches 25 ℃, adjusting the temperature in the fermentation tank to be reduced to 15 ℃, adding activated low-temperature yeast according to the feeding proportion of fermentation raw materials, adjusting the temperature of the fermentation tank to be 8 ℃, introducing oxygen until the volume fraction of oxygen in the air in the fermentation tank is 26%, fermenting for 18 days, and stopping fermentation when the sugar degree is measured to be 9%;
the preparation method of the activated low-temperature yeast comprises the steps of adding the low-temperature yeast into white sugar water with the temperature of 33 ℃ and the mass fraction of 4%, stirring, and standing for 22 minutes to obtain the activated low-temperature yeast.
D. Filter pressing clarification: removing fruit residues from fermented Rosa roxburghii by using a filter pressing device, adding diatomite for natural clarification, taking supernatant, and performing sterilization treatment by using an ultrahigh-temperature instantaneous sterilization device at a sterilization temperature of 125 ℃;
E. and D, freezing and concentrating, namely, setting the alcoholic strength of the rosa roxburghii tratt fermentation liquor treated in the step D to be 3.5% vol, placing the fermentation liquor at the temperature of 0 ℃ to obtain an ice-water mixture, separating and removing ice blocks, and determining that the alcoholic strength of the liquid is 6%, namely, the rosa roxburghii tratt enzymatic ice wine.
Wherein in the step C, in the low-temperature fermentation link, the activity of the pectinase is 20000u/g, and the activity of the cellulase is 2000 u/g; and D, performing filter pressing clarification, wherein the dosage of the diatomite accounts for 1 percent of the weight of the fermentation liquor to be clarified.
The alcoholic strength of the finally obtained rosa roxburghii tratt enzyme iced wine is 6% vol, and the sugar degree is 11%.
Experimental example 1. Comparison experiment of beneficial effects.
In order to further verify that the fermentation mode combining the enzymatic process and the wine freezing process disclosed by the invention can effectively improve the flavor development substances and optimize the taste of the golden roxburgh rose product, the contents of flavor development amino acids, organic acids and volatile flavor substances in the samples of the golden roxburgh rose before and after the fermentation by the process are detected, and the specific detection method and the detection data are as follows:
firstly, a sampling method:
sample B in example 3 was taken as test sample A before fermentation, and sample E in example 3 was taken as sample B after fermentation.
Secondly, a detection method comprises the following steps:
(1) amino acid determination, referring to GB/T5009.124-2003 'determination method of amino acid in food', accurately measuring 5m L sample solution to be determined, adding 6 mol/L hydrochloric acid into a hydrolysis tube, sealing the tube under the condition of nitrogen gas charging, placing the sealed tube in a constant temperature drying oven at (110 +/-1) DEG C, hydrolyzing for 22h, taking out and cooling, opening the tube, filtering the hydrolysate, washing the tube with deionized water for multiple times, transferring all the hydrolysate into a 50m L volumetric flask, dissolving with 1m L buffer solution with pH2.2 for instrument determination, accurately sucking 0.20m L mixed amino acid standard, using 5m L buffer solution with pH2.2, using the standard diluent solution with concentration of 5.00nmol/50 mu L as the amino acid standard for on-machine determination, and determining the amino acid content of the sample determination solution by a standard method other than an automatic amino acid analyzer.
(2) The organic acid is determined by high performance liquid chromatography, wherein the chromatographic conditions comprise a Carbomix H-NP chromatographic column (7.80mm × mm, 10 μm), a column temperature of 55 ℃, an optical component temperature of 55 ℃, a room temperature, a mobile phase of 2.50 mmol/L H2SO4, a flow rate of 0.50m L/min, a sample injection volume of 10 μ L1, and a standard curve drawing, wherein the sample injection volume comprises the steps of respectively taking appropriate amounts of oxalic acid, citric acid, malic acid, L-lactic acid and acetic acid, precisely weighing the appropriate amounts, dissolving the mobile phase and fixing the volume to 5m L3, respectively precisely sucking 1m L of each reference substance for mixing to obtain reference substance solutions with concentrations of 160 μ g/m L, 152.10 μ g/m L, 161.30 μ g/m L, 158.40 μ g/m L, 166.80 μ g/m L of oxalic acid, citric acid, malic acid, L-lactic acid and acetic acid, accurately weighing the reference substance solutions of different ratios, preparing different concentrations, accurately diluting the reference substance solutions, respectively, obtaining different concentrations, accurately weighing the reference substance solutions, preparing different ratios, respectively, diluting the reference substance solutions, and obtaining a reference substance sample injection peak area, and measuring the peak area by a precise chromatographic method, wherein the sample injection time of the reference substance sample injection is 0.5 μm of the reference substance is obtained by a precise chromatographic method.
(3) The method comprises the steps of detecting volatile components of a sample to be detected by SPME-GC-MS, uniformly mixing Rosa roxburghii fruit pulp (namely sample A and sample B) before and after fermentation, taking 5m L, placing the mixture into a sampling bottle of a 10m L solid phase micro-extractor, inserting a manual sample injector with an extraction fiber head, performing headspace extraction for 48min under a flat plate heating condition at 60 ℃, performing GC-MS analysis after 5min thermal analysis, carrying out gas chromatography under the conditions that a chromatographic column is an HP-5MS (60m × 0.25mm × 0.25.25 μm) elastic quartz capillary column, the column temperature is 45 ℃, keeping for 2min, heating to 270 ℃ at 5 ℃/min, the running time is 72min, the vaporization chamber temperature is 250 ℃, carrier gas is high-purity He (99.999%), the pre-column pressure is 16.32psi, the carrier gas flow is 1.0m L/min, non-split flow injection, solvent delay time mass spectrometry time 3min, the ion source is an NIinstein source, the quadrupole energy rod temperature is 150 ℃, the emission voltage is 70.32 psi, the relative emission current is obtained by adopting a standard voltage scanning, the national standard ST 34V, and the national standard method, and the national standard ST 17 mm of a standard method is adopted for researching the relevant analytical method, and the national standard analytical method of a standard analytical method, and the national standard analytical method is adopted for searching method.
II, detecting results:
(1) the changes of flavor-developing amino acids before and after fermentation are shown in Table 1
TABLE 1 amino acid content changes before and after fermentation of Rosa roxburghii Tratt enzymatic ice wine
Figure BDA0002513077250000111
Figure BDA0002513077250000121
Note: "" is an essential amino acid; "-" is not detected.
The types and contents of hydrolyzed amino acids before and after the fermentation process of the rosa roxburghii tratt through the enzyme deicing wine are shown in table 1, a sample A before fermentation contains 17 amino acids, wherein 3 umami amino acids, 7 sweet amino acids, 3 aromatic amino acids and 4 bitter amino acids, a sample B after fermentation contains 12 amino acids, wherein 1 umami amino acid, 5 sweet amino acids, 3 aromatic amino acids and 3 bitter amino acids are contained, the total content and the number of the amino acids are reduced, wherein the umami amino acid content is reduced from 27.43% to 2.51% of the total amino acids, the umami amino acid content is reduced by 24.92% of the total amino acids, but the sweet amino acid content is increased from 36.84% to 42.62% of the total amino acids, the bitter amino acid content is increased from 33.82% to 41.78% of the total amino acids, the aromatic amino acid content is increased from 1.9% to 13% of the total amino acids, the sweet amino acid content is increased from 33.82% to 41.78% of the total amino acids, the aromatic amino acid content is increased from 1.9% to 13% of the total amino acids, the amino acids in the sample B after fermentation, the amino acids are converted into phenylalanine, the amino acids and the amino acids are reduced to α%, respectively, and the amino acids are converted into the amino acids after the biological enzymes are converted into the biological enzymes, and the biological enzymes after fermentation, and the biological enzymes are converted into the biological enzymes, so that the biological flavor development of the biological enzymes are reduced into the biological flavor development of the biological flavor development is reduced.
(2) The change of organic acid before and after fermentation of the Rosa roxburghii Tratt enzyme deicing wine is shown in Table 2
TABLE 2 organic acid content Change before and after fermentation of Rosa roxburghii Tratt enzyme iced wine
Figure BDA0002513077250000122
Figure BDA0002513077250000131
Note: "-" is not detected.
It can be seen from table 2 that the types and contents of organic acids before and after the fermentation of the rosa roxburghii tratt enzymatic iced wine are significantly changed, the newly added organic acids after the fermentation include three types of malic acid, lactic acid and acetic acid, in addition, the original citric acid content after the fermentation is 3.42 times of that of the sample A before the fermentation, and the malic acid content is increased by 7.51 times.
(3) The change of the volatile flavor components before and after the fermentation of the rosa roxburghii tratt enzyme iced wine is shown in Table 3
TABLE 3 detection results of volatile compounds before and after fermentation of Rosa roxburghii Tratt enzyme iced wine
Figure BDA0002513077250000132
Figure BDA0002513077250000141
Figure BDA0002513077250000151
Figure BDA0002513077250000161
Figure BDA0002513077250000171
As can be seen from Table 3, 98 volatile aroma components are detected in sample A before and after the fermentation of the Rosa roxburghii Tratt ferment iced wine, including 22.22% of alcohol (14), 2.39% of aldehyde (14), 4.11% of ester (20), 1.13% of ketone (12), 50.74% of acid (11), 2.31% of alkane and olefin (17), 0.73% of other types (10), 46.02% of alcohol (15), 0.65% of aldehyde (6) and 36.63% of ester (36), the relative percentage of ketones (6 types) is 0.20%, the relative percentage of acids (9 types) is 2.66%, the relative percentage of alkane and olefin (14 types) is 0.90%, and the relative percentage of other types (9 types) is 3.80%. From the data, the contents of the rosa roxburghii tratt are acids, alcohols and esters which are obviously changed after the rosa roxburghii tratt is subjected to the fermentation treatment; wherein, the relative content percentages of the alcohols and the esters are respectively increased by 23.79 percent and 32.52 percent, and the relative content percentages of the acids, the aldehydes and the ketones are respectively reduced by 48.08 percent, 1.73 percent and 0.93 percent. The alcohol is a main metabolite of yeast fermentation, and the flavor of the alcoholic beverage mostly presents fresh flower and grass fragrance, wherein the content of ethanol is obviously increased, and the ethanol is endowed with the sweet and fragrant flavor characteristic of apples, so that the sweet and fragrant flavor of the rosa roxburghii tratt enzymatic ice wine can be effectively increased. The ester compounds are representative of aromatic flavor, after fermentation, the contents of ethyl acetate and ethyl caproate are obviously increased, and the ethyl acetate is endowed with fruity and ester flavor attributes; the ethyl caproate has fruit fragrance, and fragrance of koji and pineapple fragrance; the aromatic flavor of the rosa roxburghii tratt enzymatic ice wine is obviously improved. Meanwhile, new aromatic ester compounds are generated, such as cis-4-octenoic acid ethyl ester with apple fragrance [27], nonanal ester with obvious rose and orange fragrance, and ethyl lactate with buffering effect on pungent taste. The acid compound and the aldehyde compound are remarkably reduced in content, the caproic acid and the caprylic acid in the acid compound are remarkably reduced, the relative percentage content is respectively reduced to 0.95% and 0.72% from 32.2% and 15.2%, and research shows that caproic acid is used as a precondition substance of ethyl caproate, the low-content caproic acid shows a certain fragrance in fruits, but the high-concentration caproic acid can cause irritant sour taste, the caproic acid is converted into ethyl caproate with fragrant flavor after fermentation, the aldehyde compound is remarkably reduced after the fermentation process, and the aldehyde substance is reduced into alcohol or oxidized into acid due to instability.
In conclusion, after the rosa roxburghii tratt is treated by the enzyme deicing wine process, the proportion of sweet amino acid, bitter amino acid and aromatic amino acid in the total amino acid is relatively increased; the content and the quantity of the organic acid are increased, the newly increased organic acid after fermentation treatment comprises three types of malic acid, lactic acid and acetic acid, the newly generated organic acid extends the durability of the taste of the rosa roxburghii tratt enzyme iced wine, the taste saturation is soft, fresh and cool, and the rosa roxburghii tratt enzyme iced wine is full, fresh, fast, durable and layered; the volatile flavor substances are changed remarkably, wherein the specific fruit aroma and ester aroma of the rosa roxburghii tratt iced wine are endowed by increasing the relative content percentage of the alcohols and the esters, and the pungent sour taste and unpleasant peculiar smell of the rosa roxburghii tratt caused by high-concentration acids and aldehydes are relieved by reducing the relative content of the acids and the aldehydes and ketones.
The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it should be understood that various changes and modifications can be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

1. The Rosa roxburghii enzymatic ice wine is characterized in that: the rosa roxburghii tratt enzyme-treated ice wine comprises, by weight, 40-50 parts of fresh rosa roxburghii tratt fruits, 30-60 parts of tea water, 10-20 parts of white sugar, 0.3-0.5 part of low-temperature yeast, 0.3-0.7 part of pectinase and 0.3-0.7 part of cellulase, wherein the alcoholic strength of the rosa roxburghii tratt enzyme-treated ice wine is 5-8% vol, and the sugar content of the rosa roxburghii tratt enzyme-treated ice wine is 8-12%.
2. The rosa roxburghii enzymatic ice wine according to claim 1, wherein: the rosa roxburghii tratt enzyme-treated ice wine comprises, by weight, 42-48 parts of fresh rosa roxburghii tratt fruits, 40-50 parts of tea water, 12-18 parts of white sugar, 0.35-0.45 part of low-temperature yeast, 0.4-0.6 part of pectinase and 0.4-0.6 part of cellulase, wherein the alcoholic strength of the rosa roxburghii tratt enzyme-treated ice wine is 5-8% vol, and the sugar content of the rosa roxburghii tratt enzyme-treated ice wine is 8-12%.
3. The rosa roxburghii enzymatic ice wine according to claim 2, wherein: the rosa roxburghii tratt enzyme-fermented ice wine comprises, by weight, 45 parts of fresh rosa roxburghii tratt fruits, 45 parts of tea water, 15 parts of white sugar, 0.4 part of low-temperature yeast, 0.5 part of pectinase and 0.5 part of cellulase, wherein the tea water is black tea water, the weight ratio of black tea to water is 1:80, the alcoholic strength of the rosa roxburghii tratt enzyme-fermented ice wine is 5% -8% vol, and the sugar content of the rosa roxburghii tratt enzyme-fermented ice wine is 8% -12%.
4. The rosa roxburghii enzymatic ice wine according to any one of claims 1-3, wherein: the tea water is black tea water, wherein the weight ratio of black tea to water is 1: 50-100.
5. The rosa roxburghii enzymatic ice wine according to claim 4, wherein: the black tea water is prepared by soaking black tea in water of 20-30 deg.C for 5-10min, boiling, maintaining for 3-5min, and filtering to obtain black tea water.
6. The rosa roxburghii enzymatic ice wine according to claim 1, wherein: the activity of the pectinase is 20000u/g, and the activity of the cellulase is 2000 u/g.
7. The method for preparing the rosa roxburghii enzymatic ice wine according to any one of claims 1 to 6, wherein: comprises the following steps of (a) carrying out,
a. tea water fixation: removing pedicel from fresh fructus Rosae Normalis, cleaning, draining, adding white sugar, boiling in tea water, and keeping for 5-10min to obtain product A;
b. quick-freezing treatment: cooling product A to room temperature, freezing at-23 deg.C to-13 deg.C for 5-10h, pulping in frozen state, and crushing to obtain fructus Rosae Normalis pulp B;
c. low-temperature fermentation: transferring product B to a fermentation tank, controlling the temperature in the fermentation tank to be 20-30 ℃, adding cellulase and pectinase, adjusting the temperature in the fermentation tank to be 10-20 ℃, adding activated low-temperature yeast, adjusting the temperature in the fermentation tank to be 5-10 ℃, introducing oxygen for fermentation for 14-20 days, and stopping fermentation when the sugar degree is measured to be 8% -10% to obtain product C;
d. filter pressing clarification: filter-pressing product C to remove fruit residues, adding diatomite for natural clarification, and sterilizing the supernatant at 130 deg.C and 120 deg.C by ultra-high temperature instantaneous sterilization device to obtain product D;
e. freezing and concentrating: and (3) placing the product D at a temperature of between 5 ℃ below zero and 0 ℃ to obtain an ice-water mixture, separating and removing ice blocks until the alcoholic strength in the liquid is 5 to 8 percent vol, and thus obtaining the rosa roxburghii tratt enzymatic ice wine.
8. The method for preparing the rosa roxburghii enzymatic ice wine according to claim 7, wherein the method comprises the following steps: and in the step c, the preparation method of the activated low-temperature yeast comprises the steps of adding the low-temperature yeast into white sugar water with the temperature of 20-35 ℃ and the mass fraction of 3-5%, stirring and standing for 15-30 minutes to obtain the activated low-temperature yeast.
9. The method for preparing the rosa roxburghii enzymatic ice wine according to claim 7, wherein the method comprises the following steps: in the step c, oxygen is introduced until the volume fraction of oxygen in the air in the fermentation tank is 25-30%.
10. The method for preparing the rosa roxburghii enzymatic ice wine according to claim 7, wherein the method comprises the following steps: in the step d, the adding amount of the diatomite is 1-3% of the weight of the product C after the pomace is removed.
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