CN107897629A - A kind of antiseptics for natural food extracted from shaddock leaf and extracting method - Google Patents
A kind of antiseptics for natural food extracted from shaddock leaf and extracting method Download PDFInfo
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
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Abstract
The invention belongs to the technical field of preservative extraction, there is provided a kind of method that antiseptics for natural food is extracted from shaddock leaf.This method is using shaddock leaf as raw material, crushed first and immersion treatment, then calcium lactate and white fungus dry powder is aided in carry out rotary evaporation after vacuum film concentrates, ultrasonic wave extraction is carried out again, the compound containing flavonoids can be extracted after filtered and dry, a kind of pure natural, safe and efficient natural plant preservative is made.Compared with conventional method, extraction efficiency of the present invention is higher, and gained preservative is safe and healthy and long shelf-life; has a broad antifungal spectrum, additive amount are small, belong to pure natural addictive and clarification type preservative, and raw material is easy to get; extraction process is easily controllable, and energy consumption is relatively low, it can be achieved that scale application.
Description
Technical field
The invention belongs to the technical field of preservative extraction, there is provided a kind of wholefood anti-corrosion extracted from shaddock leaf
Agent and extracting method.
Background technology
In modern food processing, be only possible to adapt to consumer demand with suitable preserved food ability.
The food decay as caused by microorganism goes bad not only causes very big influence to the production and living of the mankind, causes huge waste,
And directly affect the life and health of consumer.According to statistics, the food loss that China there are about 20 ~ 30% every year is all by various
Caused by corruption.Therefore, appropriate food antiseptic technology is become as major issue urgently to be resolved hurrily in food security.And add anti-
Rotten agent is easy to use as one kind, and effective anti-corrosion supplementary means, increasingly receives the favor of people.
Food preservative by sources divides at present, there is two major class of chemical preservative and natural antiseptic agent.Chemical preservative is to make
With widest food preservative, but due to there is certain toxic action to human body, unfavorable shadow is will also result in ecological environment
Ring, must strictly limit in use.In contrast, antiseptics for natural food generally refers to straight from plant, animal, microorganism
Separation and Extraction is connect, a kind of material with antisepsis, it is with aboundresources, strong, the safe and non-toxic, has a broad antifungal spectrum of antibiotic property etc.
Advantage increasingly causes concern and attention in food industry.
Antiseptics for natural food is one of Main way of food preservative exploitation, can be divided into 3 types according to source：
（1）Animal sources natural antiseptic agent, refers to the preservative extracted from the relevant material of animal, such as lysozyme, insect antibacterial
Peptide, propolis, nucleoprotamine etc.；（2）Natural antiseptic agent of plant source, which refers to, to be naturally occurring in plant, by it is manually modified, decompose,
The methods of distillation is obtained to have antisepsis product, such as pectin decomposer, spice extract, tea polyphenols, marine algae extract；
（3）Microbial source natural antiseptic agent, refers to the antibacterial produced by microbial metabolism, antibacterial substance, is that food preservative is opened in recent years
One hot spot of hair, such as nisin, natamycin, kojic acid.
Antiseptics for natural food degradable normal components for food in human body alimentary canal, do not influence archenteric flora,
The use of medicinal antibiotic is not influenced, but also there is certain nutritive value.Its mechanism of action is the same as general food preservative phase
Seemingly, it directly can promptly destroy by acting on cell membrane and cell membrane system and carry out material dependent on membrane structure integrality
With the cell and organelle of energetic supersession, and the rupture inducing microbial self-dissolving of intracellular lysosome membrane can be caused；It can also pass through
The change for acting on inhereditary material or hereditary particle structure causes bacteriostasis；More also it is by acting on enzyme or function egg
In vain, the change of their functions is made to play sterilizing antisepsis.
Achieved both at home and abroad in terms of antiseptics for natural food, especially natural food preservatives from plant materials at present certain
Effect.Wherein Lee builds sweet smell et al. and has invented a kind of method, its product and application that middle extraction flavonoids plant antiseptic agent is done from bamboo
（Chinese invention patent application number 201510454741.1）, from bamboo do in the quaternary system of ethanol, acetic acid, ethyl acetate and water
Mixed solvent is extracted, and isolates and purifies to obtain food preservative with macroporous absorbent resin, but the preservative that this method obtains is protected
The matter phase is shorter, and narrow antimicrobial spectrum.A kind of vegetable source natural preservation and antisepsis using myrica rubra leaf as raw material in addition, Wang Xiaowei invention is known clearly
Agent（Chinese invention patent application number 201510829593.7）, include following raw material：Waxberry leaf extract, tea polyphenol extract thing,
Ethanol extract, Isosorbide-5-Nitrae-two (methylol) -2,5- piperazinediones, forsythia suspense extraction, the salt of cloves, but this method process is more
Complicated and raw material is too many.
The content of the invention
Technical research at present without shaddock leaf extraction antiseptics for natural food, fails to efficiently use shaddock leaf itself superior
Disinfecting detoxifying performance.For such case, it is proposed that a kind of method that antiseptics for natural food is extracted from shaddock leaf, it is special
Point is using shaddock leaf as raw material, then carries out crushing immersion treatment, and calcium lactate and white fungus are aided in after being concentrated by vacuum film
Dry powder carries out rotary evaporation, finally carries out ultrasonic wave extraction, obtains the efficient natural plant anti-corrosion containing flavone compound
Agent.
A kind of antiseptics for natural food extracted from shaddock leaf is further provided for, general wholefood anti-corrosion can be solved
The problems such as agent narrow antimicrobial spectrum, antibacterial effect are poor, the shelf-life is shorter.
To achieve the above object, the concrete technical scheme used for：
A kind of method that antiseptics for natural food is extracted from shaddock leaf, using shaddock leaf as raw material, is crushed and is soaked first
Processing, then aids in calcium lactate and white fungus dry powder after vacuum film concentrates, and carries out rotary evaporation, then carry out ultrasonic wave and carry
Take, the antiseptics for natural food containing flavone compound can be extracted after filtered and dry, the specific steps of preparation are such as
Under：
（1）Selection is grown fine, emerald shaddock leaf, is first cleaned twice with clear water, and naturally dry to moisture content is not higher than
15%, then crushed through pulverizer, then be placed in certain density ethanol solution, filter is obtained by filtration in immersion treatment after a certain period of time
Liquid；
（2）The water-bath switch of Reduced Pressure Concentration Device, and set temperature are opened, is then shut off screw clamp and piston, and beat
Vacuum pump is opened, condensed water is opened after system forms negative pressure, then by step（1）Filtrate from feed inlet add, film steam
Send out and form liquid lamella on the tube wall of pipe, and uniformly moved under the promotion of suction function, the ethanol of liquid and gasification enters gas
In liquid/gas separator, the condensed pipe of ethanol enters in receiving bottle, and concentrate enters in receiving flask from separator lower end；
（3）Connect Rotary Evaporators cooling water pipe and vacuum adapter, by speed governing knob it is left-handed to minimum, press power supply start,
After indicator light is bright slowly then step is added to feed inlet to right rotation speed governing knob to required rotating speed（2）The concentrate of gained,
Auxiliary calcium lactate and white fungus dry powder are added, concentrate enters evaporation flask, by water-bath constant temperature while rotation forms film
Heating, and evaporation is diffused under negative pressure state, realize further concentration；
（4）To step（3）The concentrate of gained carries out water bath with thermostatic control heating, is handled using ultrasonic wave, certain time is laggard
Row filtering and drying, you can obtain the antiseptics for natural food containing flavone compound.
Preferably, step（1）The shaddock leaf is shatian pomelo, pomelo, Pingshan shaddock, golden fragrant shaddock, Jin Lanyou, mulberry fiber crops shaddock, four
The leaf of at least one of season throwing, crack in beam or Wanbai pummelo.
Preferably, step（1）Size after the shaddock leaf crushes should be not more than 3mm × 3mm.
Preferably, step（1）In the ethanol solution, the volumetric concentration of ethanol is 60 ~ 80%.
Preferably, step（1）The mass ratio of the shaddock leaf and ethanol solution is 1:15~1:12, soaking time is 2 ~ 3h.
Preferably, step（2）The heating-up temperature of the water-bath is 50 ~ 60 DEG C.
Preferably, step（3）The Rotary Evaporators by rotation motor, evaporation flask, vacuum system, thermostat water bath,
Condenser pipe and receiving flask composition, rotary power is 150 ~ 180W, and heating power is 1000 ~ 1200W.
Preferably, step（3）The water-bath heating-up temperature of the Rotary Evaporators is 60 ~ 70 DEG C, the rotation of evaporation flask
Rotating speed is 80 ~ 150r/min, and liquid amount is not more than the 50% of evaporation flask capacity.
Preferably, step（3）The concentrate, calcium lactate, the quality mixture ratio of white fungus dry powder are 100:1-2:1-3.Breast
Sour calcium make it that the stability of extract is protected with white fungus dry powder, when not only extending the anti-corrosion time, and storing preservative
Between it is long, prevent from going bad.
Preferably, step（4）The heating-up temperature of the ultrasonication is 50 ~ 60 DEG C, and processing time is 40 ~ 60min.
The principle of vacuum film concentration is at reduced pressure conditions, treatment fluid to be concentrated is continuously flowed into certain speed thin
Uniform liquid lamella is formed in film evaporation tube, after heating, boiling point relatively low solvent in part is gasified in the process, and with it is dense
Contracting liquid enters in gas-liquid separator together, and concentrate is entered in receiving flask by the lower end of separator, is separated from system.And
Vaporized solvent then enters condenser pipe from the upper end of separator, is separated after cooling into returnable bottle from system.
Vacuum film concentration can be repeated, until being concentrated into required volume.In the present invention, processing is gone out using vacuum film concentrating and separating
Ethanol and part water in liquid.The key of the concentration process is the control of feed speed, if feed speed is too low, film by
Hot overlong time, be easy to cause film and is adhered on tube wall and be difficult to move, also result in solution some components in long-time plus
Hanker chemical change occurs.If feed speed is too fast, fluid heating time is short, and heating surface (area) (HS is small, it is difficult to uniform thin layer is formed,
Solvent has little time to volatilize, and causes thickening efficiency to reduce.Therefore, should neither be filled up with fluid in evaporation tube, but will not be evaporated for
Preferably, film thickness is uniform, and can uniformly be moved under suction function.
Rotary Evaporators are exactly using the principle of vacuum distillation, realize the continuous steaming to easy volatile solvent at reduced pressure conditions
Evaporate.By electronic control, evaporation flask is rotated under most suitable rotating speed, concentrate is formed film to increase evaporating surface
Product, while evaporation flask is in negative pressure state, be conducive to the volatilization of solvent.Evaporation flask is placed in thermostatted water while rotating
Heated in bath, concentrate heated diffusive evaporation under negative pressure.Heating-up temperature is close to the boiling point of solvent.Efficiently cooling down
Steam liquefies rapidly under the action of device, and pressure of the inside of a bottle, which reduces, can accelerate evaporation rate.
The extracting method of the present invention is added into calcium lactate and white fungus dry powder when Rotary Evaporators are evaporated under reduced pressure so that extraction
The flavonoids thing of thing is obtained good and protected, and not only extends the anti-corrosion time, and grows preservative storage time.
A kind of antiseptics for natural food extracted from shaddock leaf, is prepared by the above method.
The present invention provides it is a kind of from shaddock leaf extract antiseptics for natural food method, compared with prior art, its
The characteristics of prominent and excellent effect are：
1. the present invention uses vacuum film concentration technique can be so that the preservative in sample is rapidly dissolved in solvent, Ran Houli
With Rotary Evaporators heating evaporation, extraction efficiency is improved.
2. the preservative that the present invention extracts can be widely used in fruits and vegetables, food, beverage, extend the shelf life, and be good for safely
Health, belongs to pure natural addictive.
3. present invention extraction preservative adds calcium lactate and white fungus dry powder when Rotary Evaporators are evaporated under reduced pressure so that extraction
The flavonoids thing of thing is obtained good and protected, and not only extends the anti-corrosion time, and grows preservative storage time, has antibacterial
Wide spectrum, additive amount are small, belong to clarification type preservative, color and luster, the flavor and taste of product are not interfered with after addition, for beverage system
Have a clear superiority in product.
4. present invention extraction preservative uses pomelo peel to be derived from a wealth of sources for raw material, of low cost, extraction process is easy to control
System, energy consumption are relatively low, it can be achieved that scale application.
Embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the model of the present invention
Enclose and be only limitted to following example.Without departing from the idea of the above method of the present invention, according to ordinary skill knowledge
The various replacements or change made with customary means, should be included in the scope of the present invention.
Embodiment 1
A kind of method that antiseptics for natural food is extracted from shaddock leaf, it is as follows that it extracts the detailed process of preservative：
Selection is grown fine, the shaddock leaf 10kg of emerald shatian pomelo, is first cleaned twice with clear water, naturally dry to moisture content
Not higher than 15%, then particle diameter is crushed to through leaf pulverizer and is no more than 3mm × 3mm, then it is 80% to be placed in 13kg volumetric concentrations
In ethanol solution, immersion treatment 2h；The water-bath switch of Reduced Pressure Concentration Device is opened, and it is 60 DEG C to set heating-up temperature,
Be then shut off screw clamp and piston, and open vacuum pump, after system formed negative pressure after open condensed water, then by treatment fluid from into
Material mouth adds, and treatment fluid forms liquid lamella on the tube wall of thin film evaporation pipe, and is uniformly moved under the promotion of suction function,
Liquid and the ethanol of gasification enter in gas-liquid separator, and the condensed pipe of ethanol enters in receiving bottle, and concentrate is from separator lower end
Into in receiving flask；The cooling water pipe and vacuum adapter of Rotary Evaporators are connected, speed governing knob is left-handed to minimum, press power supply
Then start, slowly adds concentrate to feed inlet to right rotation speed governing knob after indicator light is bright, adds auxiliary calcium lactate and silver
Ear dry powder, concentrate, calcium lactate, the quality mixture ratio of white fungus dry powder are 100:1:3, concentrate enters evaporation flask, is rotating
By water-bath heated at constant temperature while forming film, and evaporation is diffused under negative pressure state, realizes further concentration；Rotation
The rotary power of evaporimeter is 180W, and heating power 1000, water-bath heating-up temperature is 60 DEG C, and negative pressure pressure is 600mmHg,
The rotary rpm of evaporation flask is 150r/min, liquid amount 40%；Carry out 50 DEG C of water bath with thermostatic control to concentrate to heat, at the same time
Use frequency to be handled for the ultrasonic wave of 80Hz, filtered and dried after 40min, you can obtain containing flavone compound
Antiseptics for natural food.
To the extracting method of embodiment 1, it extracts anti-corrosion effect of the obtained preservative after storing 6 months and 12 months
Rate, as shown in table 1.
Embodiment 2
A kind of method that antiseptics for natural food is extracted from shaddock leaf, it is as follows that it extracts the detailed process of preservative：
Selection is grown fine, the shaddock leaf 10kg of emerald Pingshan shaddock, is first cleaned twice with clear water, naturally dry to moisture content
Not higher than 15%, then particle diameter is crushed to through leaf pulverizer and is no more than 3mm × 3mm, then it is 60% to be placed in 11kg volumetric concentrations
In ethanol solution, immersion treatment 3h；The water-bath switch of Reduced Pressure Concentration Device is opened, and it is 50 DEG C to set heating-up temperature,
Be then shut off screw clamp and piston, and open vacuum pump, after system formed negative pressure after open condensed water, then by treatment fluid from into
Material mouth adds, and treatment fluid forms liquid lamella on the tube wall of thin film evaporation pipe, and is uniformly moved under the promotion of suction function,
Liquid and the ethanol of gasification enter in gas-liquid separator, and the condensed pipe of ethanol enters in receiving bottle, and concentrate is from separator lower end
Into in receiving flask；The cooling water pipe and vacuum adapter of Rotary Evaporators are connected, speed governing knob is left-handed to minimum, press power supply
Then start, slowly adds concentrate to feed inlet to right rotation speed governing knob after indicator light is bright, adds auxiliary calcium lactate and silver
Ear dry powder, concentrate, calcium lactate, the quality mixture ratio of white fungus dry powder are 100:2:3, concentrate enters evaporation flask, is rotating
By water-bath heated at constant temperature while forming film, and evaporation is diffused under negative pressure state, realizes further concentration；Rotation
The rotary power of evaporimeter is 160W, and heating power 1100W, water-bath heating-up temperature is 70 DEG C, and negative pressure pressure is
500mmHg, the rotary rpm of evaporation flask are 110r/min, liquid amount 40%；50 DEG C of water bath with thermostatic control is carried out to concentrate to add
Heat, while use frequency to be handled for the ultrasonic wave of 60Hz, filtered and dried after 50min, you can obtained containing flavones
The antiseptics for natural food of class compound.
To the extracting method of embodiment 2, it extracts anti-corrosion effect of the obtained preservative after storing 6 months and 12 months
Rate, as shown in table 1.
Embodiment 3
A kind of method that antiseptics for natural food is extracted from shaddock leaf, it is as follows that it extracts the detailed process of preservative：
Selection is grown fine, the shaddock leaf 10kg of emerald golden fragrant shaddock, is first cleaned twice with clear water, naturally dry to moisture content
Not higher than 15%, then particle diameter is crushed to through leaf pulverizer and is no more than 3mm × 3mm, then it is 70% to be placed in 14kg volumetric concentrations
In ethanol solution, immersion treatment 3h；The water-bath switch of Reduced Pressure Concentration Device is opened, and it is 58 DEG C to set heating-up temperature,
Be then shut off screw clamp and piston, and open vacuum pump, after system formed negative pressure after open condensed water, then by treatment fluid from into
Material mouth adds, and treatment fluid forms liquid lamella on the tube wall of thin film evaporation pipe, and is uniformly moved under the promotion of suction function,
Liquid and the ethanol of gasification enter in gas-liquid separator, and the condensed pipe of ethanol enters in receiving bottle, and concentrate is from separator lower end
Into in receiving flask；The cooling water pipe and vacuum adapter of Rotary Evaporators are connected, speed governing knob is left-handed to minimum, press power supply
Then start, slowly adds concentrate to feed inlet to right rotation speed governing knob after indicator light is bright, adds auxiliary calcium lactate and silver
Ear dry powder, concentrate, calcium lactate, the quality mixture ratio of white fungus dry powder are 100:1:1, concentrate enters evaporation flask, is rotating
By water-bath heated at constant temperature while forming film, and evaporation is diffused under negative pressure state, realizes further concentration；Rotation
The rotary power of evaporimeter is 160W, and heating power 1000W, water-bath heating-up temperature is 62 DEG C, and negative pressure pressure is
500mmHg, the rotary rpm of evaporation flask are 120r/min, liquid amount 40%；57 DEG C of water bath with thermostatic control is carried out to concentrate to add
Heat, while use frequency to be handled for the ultrasonic wave of 60Hz, filtered and dried after 55min, you can obtained containing flavones
The antiseptics for natural food of class compound.
To the extracting method of embodiment 3, it extracts anti-corrosion effect of the obtained preservative after storing 6 months and 12 months
Rate, as shown in table 1.
Embodiment 4
A kind of method that antiseptics for natural food is extracted from shaddock leaf, it is as follows that it extracts the detailed process of preservative：
Selection is grown fine, the shaddock leaf 10kg of emerald mulberry fiber crops shaddock, is first cleaned twice with clear water, naturally dry to moisture content
Not higher than 15%, then particle diameter is crushed to through leaf pulverizer and is no more than 3mm × 3mm, then it is 70% to be placed in 15kg volumetric concentrations
In ethanol solution, immersion treatment 2h；The water-bath switch of Reduced Pressure Concentration Device is opened, and it is 52 DEG C to set heating-up temperature,
Be then shut off screw clamp and piston, and open vacuum pump, after system formed negative pressure after open condensed water, then by treatment fluid from into
Material mouth adds, and treatment fluid forms liquid lamella on the tube wall of thin film evaporation pipe, and is uniformly moved under the promotion of suction function,
Liquid and the ethanol of gasification enter in gas-liquid separator, and the condensed pipe of ethanol enters in receiving bottle, and concentrate is from separator lower end
Into in receiving flask；The cooling water pipe and vacuum adapter of Rotary Evaporators are connected, speed governing knob is left-handed to minimum, press power supply
Then start, slowly adds concentrate to feed inlet to right rotation speed governing knob after indicator light is bright, adds auxiliary calcium lactate and silver
Ear dry powder, concentrate, calcium lactate, the quality mixture ratio of white fungus dry powder are 100:2:3, concentrate enters evaporation flask, is rotating
By water-bath heated at constant temperature while forming film, and evaporation is diffused under negative pressure state, realizes further concentration；Rotation
The rotary power of evaporimeter is 160W, and heating power 1200W, water-bath heating-up temperature is 68 DEG C, and negative pressure pressure is
550mmHg, the rotary rpm of evaporation flask are 90r/min, liquid amount 40%；55 DEG C of water bath with thermostatic control is carried out to concentrate to add
Heat, while use frequency to be handled for the ultrasonic wave of 70Hz, filtered and dried after 45min, you can obtained containing flavones
The antiseptics for natural food of class compound.
To the extracting method of embodiment 4, it extracts anti-corrosion effect of the obtained preservative after storing 6 months and 12 months
Rate, as shown in table 1.
Embodiment 5
A kind of method that antiseptics for natural food is extracted from shaddock leaf, it is as follows that it extracts the detailed process of preservative：
Selection is grown fine, the shaddock leaf 10kg of emerald pomelo shaddock, is first cleaned twice with clear water, naturally dry to moisture content
Not higher than 15%, then particle diameter is crushed to through leaf pulverizer and is no more than 3mm × 3mm, then it is 75% to be placed in 13kg volumetric concentrations
In ethanol solution, immersion treatment 2h；The water-bath switch of Reduced Pressure Concentration Device is opened, and it is 56 DEG C to set heating-up temperature,
Be then shut off screw clamp and piston, and open vacuum pump, after system formed negative pressure after open condensed water, then by treatment fluid from into
Material mouth adds, and treatment fluid forms liquid lamella on the tube wall of thin film evaporation pipe, and is uniformly moved under the promotion of suction function,
Liquid and the ethanol of gasification enter in gas-liquid separator, and the condensed pipe of ethanol enters in receiving bottle, and concentrate is from separator lower end
Into in receiving flask；The cooling water pipe and vacuum adapter of Rotary Evaporators are connected, speed governing knob is left-handed to minimum, press power supply
Then start, slowly adds concentrate to feed inlet to right rotation speed governing knob after indicator light is bright, adds auxiliary calcium lactate and silver
Ear dry powder, concentrate, calcium lactate, the quality mixture ratio of white fungus dry powder are 100:1:1, concentrate enters evaporation flask, is rotating
By water-bath heated at constant temperature while forming film, and evaporation is diffused under negative pressure state, realizes further concentration；Rotation
The rotary power of evaporimeter is 175W, and heating power 1150W, water-bath heating-up temperature is 65 DEG C, and negative pressure pressure is
450mmHg, the rotary rpm of evaporation flask are 100r/min, liquid amount 40%；55 DEG C of water bath with thermostatic control is carried out to concentrate to add
Heat, while use frequency to be handled for the ultrasonic wave of 70Hz, filtered and dried after 50min, you can obtained containing flavones
The antiseptics for natural food of class compound.
To the extracting method of embodiment 5, it extracts anti-corrosion effect of the obtained preservative after storing 6 months and 12 months
Rate, as shown in table 1.
Comparative example 1
A kind of method that antiseptics for natural food is extracted from shaddock leaf, it is as follows that it extracts the detailed process of preservative：
Selection is grown fine, the shaddock leaf 10kg of emerald pomelo shaddock, is first cleaned twice with clear water, naturally dry to moisture content
Not higher than 15%, then particle diameter is crushed to through leaf pulverizer and is no more than 3mm × 3mm, then it is 75% to be placed in 13kg volumetric concentrations
In ethanol solution, immersion treatment 2h；The water-bath switch of Reduced Pressure Concentration Device is opened, and it is 56 DEG C to set heating-up temperature,
Be then shut off screw clamp and piston, and open vacuum pump, after system formed negative pressure after open condensed water, then by treatment fluid from into
Material mouth adds, and treatment fluid forms liquid lamella on the tube wall of thin film evaporation pipe, and is uniformly moved under the promotion of suction function,
Liquid and the ethanol of gasification enter in gas-liquid separator, and the condensed pipe of ethanol enters in receiving bottle, and concentrate is from separator lower end
Into in receiving flask；The cooling water pipe and vacuum adapter of Rotary Evaporators are connected, speed governing knob is left-handed to minimum, press power supply
Then start, slowly adds concentrate, concentrate enters evaporation and burns to right rotation speed governing knob after indicator light is bright to feed inlet
Bottle, by water-bath heated at constant temperature while rotation forms film, and is diffused evaporation under negative pressure state, realizes further
Concentration；The rotary power of Rotary Evaporators is 175W, and heating power 1150W, water-bath heating-up temperature is 65 DEG C, negative pressure pressure
For 450mmHg, the rotary rpm of evaporation flask is 100r/min, liquid amount 40%；55 DEG C of water bath with thermostatic control is carried out to concentrate
Heating, while use frequency to be handled for the ultrasonic wave of 70Hz, filtered and dried after 50min, you can obtained containing Huang
The antiseptics for natural food of ketone compounds.
1 extracting method of comparative example, it extracts preservative efficiency of the obtained preservative after storing 6 months and 12 months, such as
Shown in table 1.
Comparative example 2
A kind of method that antiseptics for natural food is extracted from shaddock leaf, it is as follows that it extracts the detailed process of preservative：
Selection is grown fine, the shaddock leaf 10kg of emerald pomelo shaddock, is first cleaned twice with clear water, naturally dry to moisture content
Not higher than 15%, then particle diameter is crushed to through leaf pulverizer and is no more than 3mm × 3mm, then it is 75% to be placed in 13kg volumetric concentrations
In ethanol solution, immersion treatment 2h；The water-bath switch of Reduced Pressure Concentration Device is opened, and it is 56 DEG C to set heating-up temperature,
Be then shut off screw clamp and piston, and open vacuum pump, after system formed negative pressure after open condensed water, then by treatment fluid from into
Material mouth adds, and treatment fluid forms liquid lamella on the tube wall of thin film evaporation pipe, and is uniformly moved under the promotion of suction function,
Liquid and the ethanol of gasification enter in gas-liquid separator, and the condensed pipe of ethanol enters in receiving bottle, and concentrate is from separator lower end
Into in receiving flask；By concentrate, calcium lactate and white fungus dry powder, using quality mixture ratio as 100:1:1 is uniformly mixed, at 110 DEG C
Convection drying, obtains the antiseptics for natural food containing flavone compound.
2 extracting method of comparative example, it extracts preservative efficiency of the obtained preservative after storing 6 months and 12 months, such as
Shown in table 1.
Table 1：
By test, the comparative example 1 do not protected with calcium lactate and white fungus dry powder and without the contrast using rotary evaporation protection
Example 2, there is obvious decline in its anti-corrosion effect after preservative storage.
Claims (9)
1. a kind of method that antiseptics for natural food is extracted from shaddock leaf, using shaddock leaf as raw material, is crushed and is soaked first
Bubble processing, then aids in calcium lactate and white fungus dry powder after vacuum film concentrates, and carries out rotary evaporation, then carry out ultrasonic wave and carry
Take, the antiseptics for natural food containing flavone compound can be extracted after filtered and dry, the specific steps of preparation are such as
Under：
（1）Selection is grown fine, emerald shaddock leaf, is first cleaned twice with clear water, and naturally dry to moisture content is not higher than
15%, then crushed through pulverizer, then be placed in certain density ethanol solution, filter is obtained by filtration in immersion treatment after a certain period of time
Liquid；
（2）The water-bath switch of Reduced Pressure Concentration Device, and set temperature are opened, is then shut off screw clamp and piston, and beat
Vacuum pump is opened, condensed water is opened after system forms negative pressure, then by step（1）Filtrate from feed inlet add, film steam
Send out and form liquid lamella on the tube wall of pipe, and uniformly moved under the promotion of suction function, the ethanol of liquid and gasification enters gas
In liquid/gas separator, the condensed pipe of ethanol enters in receiving bottle, and concentrate enters in receiving flask from separator lower end；
（3）Connect Rotary Evaporators cooling water pipe and vacuum adapter, by speed governing knob it is left-handed to minimum, press power supply start,
After indicator light is bright slowly then step is added to feed inlet to right rotation speed governing knob to required rotating speed（2）The concentrate of gained,
Auxiliary calcium lactate and white fungus dry powder are added, concentrate enters evaporation flask, by water-bath constant temperature while rotation forms film
Heating, and evaporation is diffused under negative pressure state, realize further concentration；
（4）To step（3）The concentrate of gained carries out water bath with thermostatic control heating, is handled using ultrasonic wave, certain time is laggard
Row filtering and drying, you can obtain the antiseptics for natural food containing flavone compound.
A kind of 2. method that antiseptics for natural food is extracted from shaddock leaf according to claim 1, it is characterised in that：Step
（1）The shaddock leaf is shatian pomelo, pomelo, Pingshan shaddock, golden fragrant shaddock, Jin Lanyou, mulberry fiber crops shaddock, four seasons throwing, crack in beam or Wanbai pummelo
At least one of leaf.
A kind of 3. method that antiseptics for natural food is extracted from shaddock leaf according to claim 1, it is characterised in that：Step
（1）Size after the shaddock leaf crushes should be not more than 3mm × 3mm.
A kind of 4. method that antiseptics for natural food is extracted from shaddock leaf according to claim 1, it is characterised in that：Step
（1）In the ethanol solution, the volumetric concentration of ethanol is 60 ~ 80%.
A kind of 5. method that antiseptics for natural food is extracted from shaddock leaf according to claim 1, it is characterised in that：Step
（1）The mass ratio of the shaddock leaf and ethanol solution is 1:15~1:12, soaking time is 2 ~ 3h.
A kind of 6. method that antiseptics for natural food is extracted from shaddock leaf according to claim 1, it is characterised in that：Step
（2）The heating-up temperature of the water-bath is 50 ~ 60 DEG C.
A kind of 7. method that antiseptics for natural food is extracted from shaddock leaf according to claim 1, it is characterised in that：Step
（3）The water-bath heating-up temperature of the Rotary Evaporators is 60 ~ 70 DEG C, and the rotary rpm of evaporation flask is 80 ~ 150r/min, dress
Liquid measure is not more than the 50% of evaporation flask capacity.
A kind of 8. method that antiseptics for natural food is extracted from shaddock leaf according to claim 1, it is characterised in that：Step
（3）The concentrate, calcium lactate, the quality mixture ratio of white fungus dry powder are 100:1-2:1-3.
A kind of 9. antiseptics for natural food extracted by any one of claim 1-8 the method from shaddock leaf.
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