CN110055154A - The preparation method of compound vinegar of fruit and grain - Google Patents
The preparation method of compound vinegar of fruit and grain Download PDFInfo
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- CN110055154A CN110055154A CN201910381290.1A CN201910381290A CN110055154A CN 110055154 A CN110055154 A CN 110055154A CN 201910381290 A CN201910381290 A CN 201910381290A CN 110055154 A CN110055154 A CN 110055154A
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12J—VINEGAR; PREPARATION OR PURIFICATION THEREOF
- C12J1/00—Vinegar; Preparation or purification thereof
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
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Abstract
The present invention provides a kind of preparation method of compound vinegar of fruit and grain, belongs to the production technology field of Composite vinegar.It include: to select no disease and pests harm, mature apple and hawthorn；Apple is cut into diced apple after cleaning, and hawthorn is cut into hawthorn fourth, and impregnates color protection；Hawthorn fourth after diced apple and immersion after immersion is respectively placed in beater and pectase mashing is added, enzymatic hydrolysis obtains cider and haw juice；It sterilizes, is obtained to fermentation liquid after the pol of juice after enzymatic hydrolysis is adjusted to 12%；Alcoholic fermentation；Acetic fermentation and semicontinuous acetic fermentation；The fermentation liquid of Dichlorodiphenyl Acetate after fermentation obtains apple Hawthorn Vinegar after being filtered；With end acetic fermentation in the immersion sorghum mature vinegar production of apple Hawthorn Vinegar and just through the smoked unstrained spirits smoked, leaching vinegar is carried out；Ageing is carried out to vinegar liquid, sterilization, canned obtains compound vinegar of fruit and grain.The present invention provides a kind of preparation method of compound vinegar of fruit and grain for having both grain vinegar and fruit vinegar performance.
Description
Technical field
The present invention relates to the technical field of producing of Composite vinegar, in particular to a kind of preparation method of compound vinegar of fruit and grain.
Background technique
The type of vinegar on the market includes fruit vinegar and grain vinegar etc. at present.Fruit vinegar is to be with fruit or Fruit quality leftover bits and pieces
Primary raw material, full of nutrition, flavorful acid drink or flavouring made of being brewed through alcoholic fermentation, acetic fermentation.Fruit
Vinegar contains the microelements such as potassium necessary to abundant human body, zinc, vitamin, and a variety of organic acids have and boost metabolism, and adjusts
Acid-base balance eliminates fatigue, reduces cholesterol and blood pressure, enhances body immunity, and anti-cancer, beauty and skin care, delays antibacterial anti-inflammatory
The effects of aging, weight-reducing.Grain vinegar is a kind of international important flavouring, is the traditional brewing class acid condiment in China,
There is more than 2000 years history in China.Modern scientific research shows that grain vinegar not only has seasoning function, also has centainly
Alimentary health-care function, including lowering blood pressure and blood fat, antifatigue, antibiotic and sterilizing, adjust blood glucose and anti-oxidant and other effects.Based on it
These advantages, how by grain vinegar and fruit vinegar carry out Composite vinegar that is compound and obtaining having both grain vinegar and fruit vinegar performance by
The extensive concern of society.
Summary of the invention
In order to prepare a kind of compound vinegar of fruit and grain for having both grain vinegar and fruit vinegar performance, the present invention provides a kind of composite fruit
The preparation method of grain vinegar.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of preparation method of compound vinegar of fruit and grain comprising following steps:
Step 1, no disease and pests harm, mature apple and hawthorn are selected；Apple is cut into the diced apple of 10-30mm after cleaning, put
In the mixing colour protecting liquid for entering the citric acid that concentration is 0.10% and the NaCl that concentration is 0.1%, the liquid level covering of colour protecting liquid is mixed
Diced apple impregnates 10min and carries out color protection, can 3~5 batches of diced apples of continuous dipping with the mixing colour protecting liquid once prepared；Hawthorn is cut into
The hawthorn fourth of 10-20mm is placed in the Sodium Metabisulfite solution that concentration is 40mg/L, the liquid level of Sodium Metabisulfite solution
It covers hawthorn fourth and impregnates 5min progress color protection, it can 3~5 batches of hawthorn fourths of continuous dipping with the colour protecting liquid once prepared；
Step 2, the hawthorn fourth after the diced apple and immersion color protection after immersion color protection is taken out from corresponding colour protecting liquid, point
It is not placed in beater, and pectase 30g is added altogether in two times by every 100kg fruit fourth and is beaten, and is digested at 35~50 DEG C
Two hours；
Step 3, by after enzymatic hydrolysis cider and haw juice mix in proportion after immediately sugar addition be 12%, and
Sterilize 30min at 65~85 DEG C, obtains to fermentation liquid；
Step 4, inclined-plane saccharomyces cerevisiae is accessed in Saccharomyces protein peptone dextrose broth, in 25 DEG C of condition constant temperature
Activated within shaking table culture 48 hours, and by activated fermentation by saccharomyces cerevisiae agent by 5% inoculum concentration access in fermentation liquid,
Sealed fermenting 6 days are stood in 30 DEG C of conditions, obtains alcohol fermentation liquid；
Step 5, the acetic acid bacteria of slant preservation is accessed into acetic acid bacteria fluid nutrient medium, in 30 DEG C of condition constant-temperature table cultures 48
Hour is activated, and activated acetic acid bacterium leavening agent is accessed alcohol fermentation liquid obtained above according to 10% inoculum concentration
In, the liquid amount of alcohol fermentation liquid is the 40% of acetic fermentation tank volume, and fermentation temperature is 33 DEG C, fermentation number of days is 12 days, into
Then row acetic fermentation carries out semicontinuous acetic fermentation；
Step 6, the fermentation liquid of Dichlorodiphenyl Acetate after fermentation is filtered, and the vinegar liquid being obtained by filtration is heated to 80~85 DEG C
And 15~30min is kept, obtain apple Hawthorn Vinegar；
Step 7, acetic fermentation will be terminated in apple Hawthorn Vinegar and the production of sorghum mature vinegar and just through the smoked unstrained spirits smoked,
Vinegar liquid is filtered out after impregnating 1.5 hours according to 80~90 DEG C of heat preservation of the ratio mixing that mass ratio is 1.5:1, controlling pH exists
5.0g/100mL or more carries out ageing to vinegar liquid, sterilization, canned obtains compound vinegar of fruit and grain.
Optionally, the hawthorn fourth after the diced apple and immersion color protection after immersion color protection is respectively placed in the step 2 and is beaten
When being beaten in pulp grinder, the material-water ratio of diced apple and water is 1:1/2, and the material-water ratio of hawthorn fourth and water is 1:1.
Optionally, when cider and haw juice being mixed in proportion in the step 3, the matter between cider and haw juice
Amount ratio is 3:1.
Optionally, the step 3 is to produce 1 ° of alcohol according to theoretically 2g/100mL sugar when sugar addition is 12%
It is realized by adding cotton white sugar.
It optionally, is using eight layers of gauze in the step 6 when the fermentation liquid of Dichlorodiphenyl Acetate after fermentation is filtered
It is filtered.
Optionally, the process of the semicontinuous acetic fermentation process are as follows: when the fermentation liquid total acid content in apparatus for acetic acid fermentation tank
When reaching 3.8g/100mL, according to 2/3 segmentation amount of apparatus for acetic acid fermentation tank liquid amount, 2/3 vinegar is released by apparatus for acetic acid fermentation tank lower part
Acid fermentation liquid then squeezes into the alcohol fermentation liquid that same volume alcohol content is 4.5% from apparatus for acetic acid fermentation tank top and carries out feed supplement
Continue acetic fermentation, ferments number of days about 4~5 days, when the fermentation liquid total acid content in tank reaches 3.8g/100mL, again
According to 2/3 segmentation amount of apparatus for acetic acid fermentation tank liquid amount, 2/3 acetic acid fermentation liquid is released by apparatus for acetic acid fermentation tank lower part, then from vinegar
Acid fermentation tank top squeezes into the alcohol fermentation liquid progress feed supplement that same volume alcohol content is 4.5% and continues acetic fermentation,
Fermentation about 4~5 days, such continuous circulating fermentation.
Optionally, the preparation method of the Saccharomyces protein peptone glucose slant medium are as follows: by 2g glucose, 2g albumen
Peptone, 1g yeast extract and 1.8-2.0g agar are dissolved in 100mL distilled water, and are sterilized 15 minutes in 0.10MPa；
The preparation method of the Saccharomyces protein peptone dextrose broth are as follows: by 2g glucose, 2g peptone and 1g
Yeast extract is dissolved in 100mL distilled water, and is sterilized 15 minutes in 0.10MPa.
Optionally, the preparation method of the acetic acid bacteria slant medium are as follows: by 2mL95% ethyl alcohol, 1g glucose, 1g yeast
Cream, 1.8-2.0g agar and 1.5g dissolution of calcium carbonate sterilize 15 minutes in 100mL distilled water in 0.10MPa；When preparation first not
Add ethyl alcohol, adds ethyl alcohol after sterilizing.
The preparation method of the acetic acid bacteria fluid nutrient medium are as follows: by 2mL95% ethyl alcohol, 1g glucose, 1g yeast extract, 1.5g
Dissolution of calcium carbonate sterilizes 15 minutes in 100mL distilled water in 0.10MPa；Ethyl alcohol is first not added when preparation, adds second after sterilizing
Alcohol.
Optionally, the saccharomyces cerevisiae is CICC1001, and the acetic acid bacteria is that Shanghai makes 1.01.
The technical solution that the embodiment of the present invention provides can include the following benefits:
By first preparing apple Hawthorn Vinegar, and acetic fermentation will be terminated in apple Hawthorn Vinegar and the production of sorghum mature vinegar and just passed through
It crosses the smoked unstrained spirits smoked, keeps the temperature and impregnate according to the ratio mixing that mass ratio is 1.5:1 and filter out vinegar liquid and produce composite fruit
Grain vinegar provides a kind of production work of the fermented type fruit grain vinegar joint product of alimentary health-care function for having both mature vinegar and fruit vinegar
Skill, its development are not only that society provides novel foodstuff, can also save food, open up fruit market, promoting employment.By
The alcoholic fermentation stage is using liquid fruit vinegar alcohol and acetic fermentation process and combines to greatest extent to a certain extent traditional old
Mature vinegar technique and quality and quality, as much as possible raising ordinary liquid fruit vinegar quality, shorten the ordinary liquid fruit vinegar production cycle, mention
High utilization rate of equipment and installations reduces equipment investment cost, it is ensured that final products have fine qualities quality and functional characteristic, realize effect
Benefit maximizes.
Detailed description of the invention
The drawings herein are incorporated into the specification and forms part of this specification, and shows and meets implementation of the invention
Example, and be used to explain the principle of the present invention together with specification.
Fig. 1 is the flow chart of the preparation method of compound vinegar of fruit and grain provided in an embodiment of the present invention.
Fig. 2 apple pulp material-water ratio and the relation schematic diagram of soluble solid (pol), reduced sugar and alcohol content are.
Fig. 3 is the relation schematic diagram of hawthorn slurry water ratio Yu soluble solid (pol), reduced sugar and alcohol content.
Fig. 4 is the influence schematic diagram of the different quality comparison acetic fermentation between cider and haw juice.
Fig. 5 is the influence schematic diagram of different acetic acid bacteria inoculum concentration Dichlorodiphenyl Acetate fermentations.
Fig. 6 is the influence schematic diagram of different temperatures Dichlorodiphenyl Acetate fermentation.
Fig. 7 is the influence schematic diagram of different fermentations number of days Dichlorodiphenyl Acetate fermentation.
Fig. 8 is the influence schematic diagram of different initial pH Dichlorodiphenyl Acetate fermentations.
Fig. 9 is the influence schematic diagram of different liquid amount Dichlorodiphenyl Acetate fermentations.
Figure 10 is the response surface figure (left side) and contour of the influence of the reciprocation Dichlorodiphenyl Acetate fermentation of liquid amount, fermentation temperature
Scheme on (right side).
Figure 11 is the response surface figure (left side) of influence of reciprocation Dichlorodiphenyl Acetate fermentation of number of days, fermentation temperature and contour of fermenting
Line chart (right side).
Figure 12 is the response surface figure (left side) and contour of the influence of the reciprocation Dichlorodiphenyl Acetate fermentation of liquid amount, the number of days that ferments
Scheme on (right side).
Specific embodiment
With reference to the accompanying drawings and examples, specific embodiments of the present invention will be described in further detail.
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention
Formula is described in further detail.
As shown in Figure 1, the preparation method of compound vinegar of fruit and grain provided in an embodiment of the present invention comprising following steps 1 to step
Rapid 7.
Step 1, no disease and pests harm, mature apple and hawthorn are selected；Apple is cut into the diced apple of 10-30mm after cleaning, put
In the mixing colour protecting liquid for entering the citric acid that concentration is 0.10% and the NaCl that concentration is 0.1%, the liquid level covering of colour protecting liquid is mixed
Diced apple impregnates 10min and carries out color protection, can 3~5 batches of diced apples of continuous dipping with the mixing colour protecting liquid once prepared；Hawthorn is cut into
The hawthorn fourth of 10-20mm is placed in the Sodium Metabisulfite solution that concentration is 40mg/L, the liquid level of Sodium Metabisulfite solution
It covers hawthorn fourth and impregnates 5min progress color protection, it can 3~5 batches of hawthorn fourths of continuous dipping with the colour protecting liquid once prepared.
Wherein, the configuration proportion of colour protecting liquid is mixed are as follows: 0.10g citric acid, 0.1gNaCl and 100ml water, i.e., by 0.10g lemon
Lemon acid and 0.1gNaCl are dissolved in 100ml water and stir evenly.Mix the colour protecting liquid that colour protecting liquid is diced apple.Lay particular stress on sulfurous acid
The preparation method of sodium solution are as follows: 40mg Sodium Metabisulfite is dissolved in 1000ml water and stirs evenly.Sodium Metabisulfite is molten
Liquid is the colour protecting liquid of hawthorn fourth.
Step 2, the hawthorn fourth after the diced apple and immersion color protection after immersion color protection is taken out from corresponding colour protecting liquid, point
It is not placed in beater, and pectase 30g is added altogether in two times by every 100kg fruit fourth and is beaten (first i.e. among mashing
Remaining 1/2 pectase is added in 1/2 pectase of secondary addition before mashing terminates), and digested two hours at 35~50 DEG C.
Wherein, the quality of fruit and the ratio for adding water quality when material-water ratio refers to mashing.Since material-water ratio can influence slurries
Middle soluble solid content, so that wine out how many, clarifying effect, alcoholic strength and aesthetic quality etc. are influenced, therefore, in mashing
Suitable material-water ratio is chosen to be crucial subsequent each process flow.
To determine suitable material-water ratio when mashing, the embodiment of the present invention is by apple according to 1:2,1:1,1:1/2,1:1/4,1:
1/8 is beaten, and hawthorn is beaten according to 1:1/2,1:1,1:2,1:3,1:4 respectively.It as shown in table 1, is apple material
Water ratio and state schematic table is slurried.Fig. 2 is apple pulp material-water ratio and soluble solid (pol), reduced sugar and alcohol content
Relation schematic diagram.
Table 1
As it can be seen from table 1 apple material-water ratio is slurried when being 1:1/2, difficulty is moderate, and feed liquid viscosity is suitable for.
As shown in Figure 2, as the ratio of apple and water is smaller and smaller, though soluble solid content integrally becomes in decline
Gesture, but when material-water ratio is 1:1/4,1:1/2,1:1, soluble solid content decline is gentle.This is because amount of water can when few
Dissolubility solid content does not dissolve out completely, as the soluble solid that increases of amount of water leaches on one side, is diluted on one side, or less
Drop trend is more gentle；When continuing growing the ratio of water, the water that soluble solid is added into after leaching completely is further dilute
It releases.Therefore, when material-water ratio is greater than 1:1/2, soluble solid declines rapidly.In conclusion the step 2 of the embodiment of the present invention
Middle to impregnate the diced apple after color protection and be placed in when being beaten in beater, the material-water ratio of diced apple and water is 1:1/2.
Suitable material-water ratio when to determine mashing, the embodiment of the present invention by hawthorn respectively according to 1:1/2,1:1,1:2,1:3,
1:4 is beaten.As shown in table 2, hawthorn material-water ratio and state schematic table to be slurried.Fig. 3 be hawthorn slurry water ratio with it is solvable
The relation schematic diagram of property solid content (pol), reduced sugar and alcohol content.
Table 2
As shown in Table 2, it when material-water ratio is 1:1, is slurried generally, and feed liquid is fine and smooth uniformly, it is dilute thick suitable.As shown in figure 3,
When material-water ratio is 1:1, soluble solid content and alcohol content are all moderate.Therefore, in step 2 of the embodiment of the present invention preferably
The hawthorn fourth after color protection will be impregnated to be placed in when being beaten in beater, the material-water ratio that hawthorn fourth and water is arranged is 1:1.
Step 3, by after enzymatic hydrolysis cider and haw juice mix in proportion after immediately sugar addition be 12%, and
Sterilize 30min at 65~85 DEG C, obtains to fermentation liquid.
Mass values and subsequent alcoholic fermentation when due to mixing cider and haw juice, between cider and haw juice
The factors such as the alcoholic strength in technique are related, therefore, the mass ratio when embodiment of the present invention also mixes cider and haw juice into
Research is gone.As shown in figure 4, its different quality between cider and haw juice compares the influence schematic diagram of acetic fermentation.
As shown in Figure 4, although pol is (actually soluble solid herein when the mass ratio between cider and haw juice is 2 ︰ 1
Shape object content) highest, but this due to haw juice large percentage, pectic substance content is higher, and content of reducing sugar is not high, because
And the alcoholic strength generated that ferments is not high.The alcoholic strength to be formed is fermented most when the mass ratio between cider and haw juice is 3 ︰ 1
Height, so that it is guaranteed that acetic fermentation has enough substrate contents.Therefore, in step 3 described in the embodiment of the present invention by cider and
When haw juice mixes, the mass values between cider and haw juice are 3 ︰ 1.
In order to ensure apple Hawthorn Vinegar obtained acidity close to 4%, the step 3 is when sugar addition is 12%
Generate what 1 ° of alcohol was realized by adding cotton white sugar according to 2g/100mL sugar, to guarantee alcohol content at the end of alcoholic fermentation
It can be close to 5%.
Step 4, inclined-plane saccharomyces cerevisiae is accessed in Saccharomyces protein peptone dextrose broth, in 25 DEG C of condition constant temperature
Shaking table (160r/min) is cultivated 48 hours and is activated, and (i.e. yeast count reaches 1 by activated fermentation by saccharomyces cerevisiae agent
× 108/ml) it accesses by 5% inoculum concentration to (wait for accessing 5ml leavening in fermentation liquid by every 100ml) in fermentation liquid,
Sealed fermenting 6 days are stood in 30 DEG C of conditions, obtains alcohol fermentation liquid.
The step of step is alcoholic fermentation.Preferably, the saccharomyces cerevisiae is CICC1001.
Wherein, the preparation method of the Saccharomyces protein peptone glucose slant medium are as follows: by 2g glucose, 2g albumen
Peptone, 1g yeast extract and 1.8-2.0g agar are dissolved in 100mL distilled water, and are sterilized 15 minutes in 0.10MPa.The saccharomycete
The preparation method of peptone dextrose fluid nutrient medium are as follows: 2g glucose, 2g peptone and 1g yeast extract are dissolved in 100mL and steamed
In distilled water, and sterilize 15 minutes in 0.10MPa.
Step 5, the acetic acid bacteria of slant preservation is accessed into acetic acid bacteria fluid nutrient medium, in 30 DEG C of condition constant-temperature table (160r/
Min it) cultivates 48 hours and is activated, and (i.e. acetic acid bacteria cell number reaches 1.8 × 10 by activated acetic acid bacterium leavening agent8/ml
) access in alcohol fermentation liquid obtained above according to 10% inoculum concentration (i.e. by being accessed in every 100ml alcohol fermentation liquid
10ml acetic acid bacterium leavening agent), the liquid amount of alcohol fermentation liquid is the 40% of acetic fermentation tank volume, and fermentation temperature is 33 DEG C, hair
Ferment number of days is 12 days, carries out acetic fermentation, then carries out semicontinuous acetic fermentation.
The step of step is acetic fermentation.Preferably, the acetic acid bacteria is that Shanghai makes 1.01.
Wherein, the preparation method of the acetic acid bacteria slant medium are as follows: by 2mL95% ethyl alcohol, 1g glucose, 1g yeast
Cream, 1.8-2.0g agar and 1.5g dissolution of calcium carbonate sterilize 15 minutes in 100mL distilled water in 0.10MPa；When preparation first not
Add ethyl alcohol, adds ethyl alcohol after sterilizing.The preparation method of the acetic acid bacteria fluid nutrient medium are as follows: by 2mL95% ethyl alcohol, 1g grape
Sugar, 1g yeast extract, 1.5g dissolution of calcium carbonate sterilize 15 minutes in 100mL distilled water in 0.10MPa；Second is first not added when preparation
Alcohol adds ethyl alcohol after sterilizing.Due to ethyl alcohol sterilizing when can a large amount of evaporation losses, so the embodiment of the present invention preparation acetic acid
It is first to sterilize that ethyl alcohol is added afterwards when bacterium slant medium and acetic acid bacteria fluid nutrient medium.
In the embodiment of the present invention after alcoholic strength reaches 4.5%, into acetic fermentation.When due to acetic fermentation, acetic acid bacteria
Inoculum concentration, fermentation temperature, alcohol fermentation liquid liquid amount and fermentation number of days can Dichlorodiphenyl Acetate fermentation result have an impact, for protect
Card acetic fermentation effect is best, and the embodiment of the present invention respectively researchs and analyses the different factors for influencing acetic fermentation, point
Analysis process and result are as follows:
The influence of 5.1 different acetic acid bacteria inoculum concentration Dichlorodiphenyl Acetate fermentations.
Influence using acetic acid bacteria inoculum concentration to fermentation ends total acid content selects acetic acid bacteria inoculum concentration difference as research object
It is 6%, 8%, 10%, 12%, 14%, fermentation temperature is 33 DEG C, and liquid amount is the 40% of acetic fermentation tank volume, fermentation 12
It, carries out acetic fermentation.Measure the total acid content generated.
As shown in figure 5, it is the influence schematic diagram of different acetic acid bacteria inoculum concentration Dichlorodiphenyl Acetates fermentation.As shown in Figure 5, it is fermenting
Temperature is 33 DEG C, and liquid amount is the 40% of acetic fermentation tank volume, and fermentation number of days is under the conditions of 12 days, with acetic acid bacteria inoculum concentration
Increase, the total acid content of fruit vinegar is gradually increased, when acetic acid bacteria inoculum concentration is 10%, total acid content highest；When acetic acid bacteria connects
When kind amount is greater than 10%, total acid content is gradually reduced.This is because in the certain fermentation liquid of nutriment, acetic acid bacteria inoculum concentration
Excessive, acetic acid bacterial content is bigger in fermentation liquid, and the nutrition of consumption is also more, and the substrate for generating acetic acid is less, to make
Acid amount must be produced to be relatively low.In conclusion the inoculum concentration for the most suitable acetic acid bacteria that the embodiment of the present invention determines is 10%.
The influence of 5.2 different fermentations temperature Dichlorodiphenyl Acetates fermentation.
Influence using fermentation temperature to fermentation ends total acid content as research object, to select temperature be respectively 20 DEG C, 25 DEG C,
30 DEG C, 33 DEG C, 37 DEG C, acetic acid bacteria inoculum concentration are 10%, and liquid amount is the 40% of fermenter volume, and fermentation time is 12 days, into
Row acetic fermentation.Measure the total acid content generated.
Fig. 6 is the influence schematic diagram of different temperatures Dichlorodiphenyl Acetate fermentation.As shown in fig. 6, the inoculum concentration in acetic acid bacteria is 10%,
Liquid amount is the 40% of acetic fermentation tank volume, and under the conditions of fermentation 12 days, fermentation temperature is too low, is unfavorable for the growth of acetic acid bacteria,
It is also low to produce acid, fermentation temperature is excessively high to will cause thallus aging quickening, and fermentation liquid total acid content is caused to decline.It will be appreciated from fig. 6 that with
Temperature gradually rises, and total acid content also rises with it, but temperature be higher than 33 DEG C when, total acid content gradually decreases, therefore of the invention
The most suitable fermentation temperature that embodiment determines is 33 DEG C.
The influence of 5.3 different fermentations number of days Dichlorodiphenyl Acetates fermentation.
Using influence of the number of days to fermentation ends total acid content of fermenting as research object, acetic acid bacteria inoculum concentration is 10%, fills liquid
Amount is the 40% of fermenter volume, and fermentation temperature is 33 DEG C, carries out acetic fermentation.Every other day measure total acid content.
Fig. 7 is the influence schematic diagram of different fermentations number of days Dichlorodiphenyl Acetate fermentation.It as shown in Figure 7, is 33 DEG C in fermentation temperature, dress
Liquid measure is that the 40% of acetic fermentation tank volume ferments initial stage under conditions of inoculum concentration is 10%, and total acid content increases very fast；When
When fermentation time is 12 days, total acid content reaches maximum value, so the number of days that the embodiment of the present invention chooses acetic fermentation is 12 days.
The influence of 5.4 different initial pH Dichlorodiphenyl Acetate fermentations.
Influence using the initial pH of fermentation liquid to fermentation ends total acid content as research object, select initial pH for 3.0,3.8,
4.5,5.0,5.5, acetic acid bacteria inoculum concentration is 10%, and fermentation temperature is 33 DEG C, and liquid amount is the 40% of fermentation flask volume, when fermentation
Between be 12 days, carry out acetic fermentation.Measure the total acid content generated.
Fig. 8 is the influence schematic diagram of different initial pH Dichlorodiphenyl Acetate fermentations.It as seen from Figure 8, is 33 DEG C in fermentation temperature,
Liquid amount is the 40% of acetic fermentation tank volume, and acetic acid bacteria inoculum concentration is 10%, under the conditions of fermentation 12 days, when pH is 4.5, always
Acid content highest, so, the pH that the embodiment of the present invention determines is 4.5.
The influence of 5.5 different liquid amount Dichlorodiphenyl Acetate fermentations
Influence using liquid amount to fermentation ends total acid content selects liquid amount for fermentation flask volume as research object
24%, 32%, 40%, 48%, 56%, inoculum concentration 10%, fermentation temperature is 33 DEG C, pH 4.5, and fermentation time is 12 days,
Carry out acetic fermentation.Measure the total acid content generated.
Fig. 9 is the influence schematic diagram of different liquid amount Dichlorodiphenyl Acetates fermentation.It as shown in Figure 9, is 33 DEG C in fermentation temperature, inoculation
Amount is 10%, pH 4.5, and under the conditions of fermentation 12 days, with the increase of liquid amount, total acid content, which is presented, first increases becoming of reducing afterwards
Gesture, the total acid content highest when liquid amount is 40%, declines later.So the most suitable liquid amount that the embodiment of the present invention determines
It is the 40% of acetic fermentation bottle volume.
In order to more scientifically select the principal element for influencing acetic fermentation effect from above-mentioned all single factor tests, it is necessary to logical
The screening that factor screening (Plackett-Burman, PB) test carries out significant factor is crossed, then carries out response surface experiments optimization most
Whole design scheme.Firstly, 12 groups are taken, the experimental design that level is 2, to fermentation temperature (A), liquid amount (B), fermentation number of days
(C), 5 factors such as initial pH (D), inoculum concentration (E) are investigated, and experimental design and the results are shown in Table 3.
Table 3
According to test data, the equation that is fitted are as follows: total acid=2.4187-0.0069A+0.0636B-0.3362C+
0.7191D+0.4016E.Through the progress variance analysis of Minitab17 software it is found that in the entire regression region of research, the mould
Type fitness is preferable, coefficient of determination R2=95.92%, illustrate to influence in the principal element screening test of acetic fermentation,
95.92% data can thus model explanation, test result be more accurate.
As shown in table 4, analysis of variance table is tested for PB.
Table 4
By table 4 according to the variance analysis of test result it is found that three factor P (C)=0.004, P (D)=0.000, P (E)
=0.002 its P value is respectively less than 0.05.Therefore, following the description selection liquid amount, temperature, fermentation time continue response interview
It tests.
Response surface experiments design is the design scheme that further assay optimization is carried out using the result of factor screening, according to
PB tests three significant factors obtained, i.e. fermentation temperature (A), liquid amount (B), fermentation number of days (C), see the table below the response in 5
Response surface experiments variance analysis in face experimental design and result and table 6.
Table 5
Table 6
By 6 variance analysis of table can perception model to lose quasi- item not significant (P=0.0602 > 0.05), it is quasi- to illustrate that equation does not lose, returns
Model is extremely significant (P=0.0022 < 0.01), the coefficient R of model2It is 93.48%, illustrates that the model can be preferably fitted
Test result, therefore regression equation provides a suitable model to the acetic fermentation of this apple Hawthorn Vinegar.From variance analysis
It can also be seen that A- fermentation temperature in the first order of equation (0.0083 < 0.01 influence is extremely significant), C- fermentation time in table
(0.0129 < 0.05) is all the factor for needing mainly to control during the fermentation.Model interacts item C2(< 0.01) it influences extremely aobvious
It writes, AB, A2、B2(< 0.05) is more significant.Illustrate there is apparent reciprocation between three factors of influence acetic fermentation.
Multiple regression Fitting Analysis is carried out using Design Expert8.0.6 software, obtains each variable factors of zymotechnique
Quadratic equation model are as follows: total acid=+ 3.74+0.29*A+0.021*B+0.27*C-0.30*A*B-0.22*A*C+0.070*B*
C-0.27*A2-0.36*B2-0.73*C2。
Response surface figure can intuitively reflect each factor and influence of the reciprocation to response between them, utilize
Design Expert8.0.6 software carries out secondary multiple regression fitting, the response surface figure of obtained quadratic regression equation and its
Contour is shown in Figure 10, Figure 11, Figure 12.Figure 10 is the response of the influence of the reciprocation Dichlorodiphenyl Acetate fermentation of liquid amount, fermentation temperature
Face figure (left side) and contour map (right side).Figure 11 is the sound of the influence of the reciprocation Dichlorodiphenyl Acetate fermentation of fermentation number of days, fermentation temperature
Answer face figure (left side) and contour map (right side).Figure 12 is the sound of the influence of the reciprocation Dichlorodiphenyl Acetate fermentation of liquid amount, the number of days that ferments
Answer face figure (left side) and contour map (right side).
From the response surface figure to interact two-by-two between each factor, there is stronger reciprocation between each factor, sends out
Now wherein curve tendency is steeper, influences more significant；Curve tendency is more smooth, influences smaller.Curved surface variation is accordingly shown as
The size of response variation.By Figure 10-Figure 12 it is found that three response factors all have extreme value in selected range, by sound
Thin-skinned part is answered to analyze the result optimized are as follows: liquid amount 38.17%, fermentation temperature are 34.92 DEG C, and fermentation number of days is
12.08 days, obtained total acid content was 3.85g/100mL.
For the accuracy of testing model prediction, fermentation verifying is carried out at optimum conditions.It is tested by repeatability three times
Confirmatory test, measuring average value is 3.83g/100mL, is coincide with model, illustrates that the model can preferably predict fermentation situation, tool
There is actual application value.
Preferably, the acetic fermentation in the step 5 uses semicontinuous acetic fermentation process.Wherein, the semicontinuous vinegar
The process of acid fermentation technique are as follows: when the fermentation liquid total acid content in apparatus for acetic acid fermentation tank reaches 3.8g/100mL, sent out according to acetic acid
2/3 segmentation amount of fermentation tank liquid amount releases acetic acid fermentation liquid (vinegar liquid smokes unstrained spirits for drenching sorghum vinegar) by apparatus for acetic acid fermentation tank lower part,
The alcohol fermentation liquid progress feed supplement that same volume alcohol content is 4.5% is then squeezed into apparatus for acetic acid fermentation tank continues acetic acid
Fermentation is fermented number of days about 4~5 days, when the fermentation liquid total acid content in tank reaches 3.8g/100mL, again according to acetic fermentation
2/3 segmentation amount of canned liquid measure is released 2/3 acetic acid fermentation liquid by apparatus for acetic acid fermentation tank lower part, then from apparatus for acetic acid fermentation tank top
It squeezes into the alcohol fermentation liquid progress feed supplement that same volume alcohol content is 4.5% and continues acetic fermentation, ferment about 4~5 days,
Such continuous circulating fermentation.Test result shows that when segmentation amount is 2/3, the short acetic fermentation period is only the 1/ of former batch fermentation
3~1/2, production efficiency significantly improves, and shortens the common standing liquid state fermentation fruit vinegar production cycle, improves utilization rate of equipment and installations,
Ensure that final products have fine qualities quality and functional characteristic, realize maximizing the benefits.
Step 6, the fermentation liquid of Dichlorodiphenyl Acetate after fermentation is filtered, and the vinegar liquid being obtained by filtration is heated to 80~85 DEG C
And 15~30min is kept, obtain apple Hawthorn Vinegar；
It preferably, is using eight layers of gauze in the step 6 when the fermentation liquid of Dichlorodiphenyl Acetate after fermentation is filtered
It is filtered.
Step 7, acetic fermentation will be terminated in apple Hawthorn Vinegar and the production of sorghum mature vinegar and just through the smoked unstrained spirits smoked,
Vinegar liquid is filtered out after impregnating 1.5 hours according to 80~90 DEG C of heat preservation of the ratio mixing that mass ratio is 1.5:1, controlling pH exists
5.0g/100mL or more carries out ageing to vinegar liquid, sterilization, canned obtains compound vinegar of fruit and grain.
The product quality for the compound vinegar of fruit and grain being prepared through the above steps is as follows:
1, subjective appreciation and physical and chemical index
Compound vinegar of fruit and grain is dark brown, glossy, mellow delicious, and no suspended substance, free from admixture has microprecipitation.
The total acid 5.02g/100mL of compound vinegar of fruit and grain, total ester be 2.8g/100mL, content of reducing sugar 1.75g/100mL,
Soluble solid is 11%, pH 3.65.
2, aroma volatile
Using gas chromatograph-mass spectrometer (GC-MS) measurement analysis shows: with vinegar characteristic flavor in compound vinegar of fruit and grain
Substance has benzyl carbinol, phenylacetaldehyde, 2-Methyl Butyric Acid, ethyl acetate, phenethyl acetate, ethyl palmitate, wherein ethyl acetate
Content has reached 15.30%, higher than single apple vinegar, Hawthorn Vinegar and sorghum vinegar.
Alcohols is another major class volatile component in vinegar, up to 14 kinds of the alcohols material in compound vinegar of fruit and grain, than single original
Expect that vinegar is abundant.
Aldehydes has irritation, and majority is harmful to the human body, as the acetaldehyde of denier can form pungent, compound vinegar of fruit and grain
In the content of aldehyde material substantially reduced compared with the content of aldehyde material in sorghum vinegar.
Ligustrazine has platelet aggregation-against and depolymerization, expands parteriole, improves microcirculation, increases brain blood flow and promoting blood circulationization
Silt effect, ligustrazine content is higher than the single raw material middle content that makes vinegar in compound vinegar of fruit and grain.
3, functional component
3.1, flavones content:
Flavone compound has the function of the medicine healthy sofas such as anti-oxidant, anti-aging, heat-clearing, reducing blood lipid, and being that one kind is great opens
The natural of hair prospect.Measurement result shows that the flavones content in compound vinegar of fruit and grain has reached 450.74mg/100mL,
Respectively higher than 2 times of 8 times of apple vinegar and sorghum vinegar.
3.2, polyphenol content:
Phenolic substances has very strong inoxidizability, and very important antioxidation is played in food, and total phenol content is got over
Height, oxidation resistance are stronger.Measurement result shows that the total phenol content in compound vinegar of fruit and grain up to 464.73mg/100mL, is shown
Write the apple vinegar or Hawthorn Vinegar for being higher than single raw material.
4, organic acid content
It as shown in Table 9, is four kinds of vinegar organic acid content testing result schematic tables.As shown in Table 9, compound vinegar of fruit and grain is not only
Malic acid and pyruvic acid rich in fruit vinegar, but also there is high level lactic acid, lactic acid has faint fragrance.Compound vinegar of fruit and grain is very
The composition for improving single raw material vinegar organic acid well, alleviates the irritation of acetic acid, improves tart flavour quality.
Table 9
It can to sum up obtain, the single raw material vinegar of flavor substance kind analogy of the compound vinegar of fruit and grain of production of the embodiment of the present invention is abundant,
Flavones, the content of polyphenol are high, and contained organic acid not only includes the kinds of organic acids in the fruit vinegar and sorghum vinegar of single raw material, but also
Main organic acid content obviously increases.
Compound vinegar of fruit and grain can be used as flavouring as a kind of novel product, it can also be used to prepare new beverage, be apple
The development and utilization of fruit and haw raw material, dosage of saving food and increase orchard worker's income open a new way.
All the above alternatives can any combination, the present invention not to one by one combine after structure carry out specifically
It is bright.
The above embodiments are only used to illustrate the present invention, and not limitation of the present invention, in relation to the common of technical field
Technical staff can also make a variety of changes and modification without departing from the spirit and scope of the present invention, therefore all
Equivalent technical solution also belongs to scope of the invention, and scope of patent protection of the invention should be defined by the claims.
Claims (9)
1. a kind of preparation method of compound vinegar of fruit and grain, which comprises the steps of:
Step 1, no disease and pests harm, mature apple and hawthorn are selected；Apple is cut into the diced apple of 10-30mm after cleaning, be put into dense
In the mixing colour protecting liquid for the NaCl that the citric acid and concentration that degree is 0.10% are 0.1%, the liquid level covering apple of colour protecting liquid is mixed
Fourth impregnates 10min and carries out color protection, can 3~5 batches of diced apples of continuous dipping with the mixing colour protecting liquid once prepared；Hawthorn is cut into 10-
The hawthorn fourth of 20mm is placed in the Sodium Metabisulfite solution that concentration is 40mg/L, and the liquid level of Sodium Metabisulfite solution covers
Hawthorn fourth impregnates 5min and carries out color protection, can 3~5 batches of hawthorn fourths of continuous dipping with the colour protecting liquid once prepared；
Step 2, the hawthorn fourth after the diced apple and immersion color protection after immersion color protection is taken out from corresponding colour protecting liquid, sets respectively
In beater, and pectase 30g is added altogether in two times by every 100kg fruit fourth and is beaten, and is small in 35~50 DEG C of enzymatic hydrolysis two
When；
Step 3, by after enzymatic hydrolysis cider and haw juice mix in proportion after immediately sugar addition be 12%, and 65~
Sterilize 30min at 85 DEG C, obtains to fermentation liquid；
Step 4, inclined-plane saccharomyces cerevisiae is accessed in Saccharomyces protein peptone dextrose broth, in 25 DEG C of condition constant-temperature tables
Culture is activated for 48 hours, and by activated fermentation by saccharomyces cerevisiae agent by 5% inoculum concentration access in fermentation liquid, 30
DEG C condition stand sealed fermenting 6 days, obtain alcohol fermentation liquid；
Step 5, the acetic acid bacteria of slant preservation is accessed into acetic acid bacteria fluid nutrient medium, 30 DEG C the culture of condition constant-temperature table 48 hours
It is activated, and activated acetic acid bacterium leavening agent is accessed in alcohol fermentation liquid obtained above according to 10% inoculum concentration,
The liquid amount of alcohol fermentation liquid is the 40% of acetic fermentation tank volume, and fermentation temperature is 33 DEG C, fermentation number of days is 12 days, carries out vinegar
Then acid fermentation carries out semicontinuous acetic fermentation；
Step 6, the fermentation liquid of Dichlorodiphenyl Acetate after fermentation is filtered, and the vinegar liquid being obtained by filtration is heated to 80~85 DEG C and is protected
15~30min is held, apple Hawthorn Vinegar is obtained；
Step 7, acetic fermentation will be terminated in apple Hawthorn Vinegar and the production of sorghum mature vinegar and just through the smoked unstrained spirits smoked, according to
80~90 DEG C of heat preservation of the ratio mixing that mass ratio is 1.5:1 filters out vinegar liquid after impregnating 1.5 hours, and controlling pH is in 5.0g/
100mL or more carries out ageing to vinegar liquid, sterilization, canned obtains compound vinegar of fruit and grain.
2. the preparation method of compound vinegar of fruit and grain according to claim 1, which is characterized in that will impregnate and protect in the step 2
It diced apple after color and impregnates the hawthorn fourth after color protection and is respectively placed in when being beaten in beater, the material-water ratio of diced apple and water
For 1:1/2, the material-water ratio of hawthorn fourth and water is 1:1.
3. the preparation method of compound vinegar of fruit and grain according to claim 1, which is characterized in that by cider in the step 3
When mixing in proportion with haw juice, the mass values between cider and haw juice are 3:1.
4. the preparation method of compound vinegar of fruit and grain according to claim 1, which is characterized in that the step 3 is in sugar addition
When being 12%, 1 ° of alcohol is produced according to theoretically 2g/100mL sugar and is realized by adding cotton white sugar.
5. the preparation method of compound vinegar of fruit and grain according to claim 1, which is characterized in that in Dichlorodiphenyl Acetate in the step 6
When fermentation liquid after fermentation is filtered, it is filtered using eight layers of gauze.
6. the preparation method of compound vinegar of fruit and grain according to claim 1, which is characterized in that the semicontinuous acetic fermentation work
The process of skill are as follows: when the fermentation liquid total acid content in apparatus for acetic acid fermentation tank reaches 3.8g/100mL, according to the canned liquid of acetic fermentation
2/3 segmentation amount of amount is released 2/3 acetic acid fermentation liquid by apparatus for acetic acid fermentation tank lower part, then squeezed into together from apparatus for acetic acid fermentation tank top
The alcohol fermentation liquid that sample volume alcohol content is 4.5% carries out feed supplement and continues acetic fermentation, ferments number of days about 4~5 days, to
When fermentation liquid total acid content in tank reaches 3.8g/100mL, again according to 2/3 segmentation amount of apparatus for acetic acid fermentation tank liquid amount, by vinegar
Acid fermentation tank lower part releases 2/3 acetic acid fermentation liquid, and then squeezing into same volume alcohol content from apparatus for acetic acid fermentation tank top is
4.5% alcohol fermentation liquid carries out feed supplement and continues acetic fermentation, ferments about 4~5 days, such continuous circulating fermentation.
7. the preparation method of compound vinegar of fruit and grain according to claim 1, which is characterized in that
The preparation method of the Saccharomyces protein peptone glucose slant medium are as follows: by 2g glucose, 2g peptone, 1g yeast extract
It is dissolved in 100mL distilled water with 1.8-2.0g agar, and sterilizes 15 minutes in 0.10MPa；
The preparation method of the Saccharomyces protein peptone dextrose broth are as follows: by 2g glucose, 2g peptone and 1g yeast
Cream is dissolved in 100mL distilled water, and is sterilized 15 minutes in 0.10MPa.
8. the preparation method of compound vinegar of fruit and grain according to claim 1, which is characterized in that
The preparation method of the acetic acid bacteria slant medium are as follows: by 2mL95% ethyl alcohol, 1g glucose, 1g yeast extract, 1.8-2.0g
Agar and 1.5g dissolution of calcium carbonate sterilize 15 minutes in 100mL distilled water in 0.10MPa；Ethyl alcohol is first not added when preparation, sterilizes
After add ethyl alcohol.
The preparation method of the acetic acid bacteria fluid nutrient medium are as follows: by 2mL95% ethyl alcohol, 1g glucose, 1g yeast extract, 1.5g carbonic acid
Calcium is dissolved in 100mL distilled water, is sterilized 15 minutes in 0.10MPa；Ethyl alcohol is first not added when preparation, adds ethyl alcohol after sterilizing.
9. the preparation method of compound vinegar of fruit and grain according to claim 1, which is characterized in that the saccharomyces cerevisiae is
CICC1001, the acetic acid bacteria are that Shanghai makes 1.01.
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