CN105124716B - The method for preparing food preservative using Chinese cassia tree oil extract waste liquid - Google Patents
The method for preparing food preservative using Chinese cassia tree oil extract waste liquid Download PDFInfo
- Publication number
- CN105124716B CN105124716B CN201510439512.2A CN201510439512A CN105124716B CN 105124716 B CN105124716 B CN 105124716B CN 201510439512 A CN201510439512 A CN 201510439512A CN 105124716 B CN105124716 B CN 105124716B
- Authority
- CN
- China
- Prior art keywords
- chinese cassia
- cassia tree
- trans
- water phase
- waste liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/006—Refining fats or fatty oils by extraction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
Abstract
A method of preparing food preservative using Chinese cassia tree oil extract waste liquid, it is related to a kind of method preparing food preservative, the present invention utilizes the water phase distillate that will be collected from the water phase distillate flowed out in the oil water separator of Chinese cassia tree oil extractor or after the brownish black muddiness waste liquid re-distillation in extractor, by the way that sodium chloride or potassium chloride is added, trans-cinnamic aldehyde and cinnamic acid in water phase distillate is set to be precipitated, organic solvent is added to be extracted, then organic solvent is evaporated under reduced pressure, obtain brown oil liquid, this brown oil liquid cryogen is freezed, crystallization is precipitated, fast filtering obtains trans-cinnamic aldehyde and Chinese cassia tree acid blend.Trans-cinnamic aldehyde and Chinese cassia tree acid blend have bacteriostatic activity to staphylococcus aureus, Escherichia coli, hay bacillus, aspergillus niger, aspergillus flavus and Penicillium citrinum, have scavenging effect to DPPH free radicals, can be used as food preservative.This method is easy to operate, it is environmentally friendly, at low cost, convenient for promoting the use of.
Description
Technical field
The present invention relates to a kind of method preparing preservative, especially a kind of method preparing food preservative.
Background technology
The alias jade osmanthus Chinese cassia tree (Cinnamomum cassia Presl), is Lauraceae Cinnamomum, is mainly distributed on the torrid zone, South Asia
Torrid areas.China is the main place of production of Chinese cassia tree, is mainly distributed on Guangxi, Guangdong, followed by Hainan, Yunnan, good fortune at home
It builds, the essential oil product made of Chinese cassia tree has very extensive purposes in the industries such as essence and flavoring agent and food.
The production of domestic cinnamon oil is all to use traditional steam distillation technique.General in steam distillation technique
It collects oil phase part in distillate to be allocated as cinnamon essential oil product, the water phase flowed out from the oil water separator of Chinese cassia tree oil extractor evaporates
The brownish black muddiness waste liquid gone out in liquid and Chinese cassia tree oil extractor is usually expelled directly out, but when extracting cinnamon essential oil since water dissipates
Often some volatile ingredient is dissolved in (or being slightly soluble in) water and stays in slops for effect, hydrolysis and thermodynamic activity
In.Retain in this some volatile compounds in Chinese cassia tree oil extract waste liquid, the mainly containing oxygen derivative of terpene substances, these objects
Matter gives off a strong fragrance, and represents the distinctive fragrance of essential oil, is the part of most worthy in essential oil, and due to the oil-water ratio of distillate
Small, this Some essential oils ratio shared in entirely distillating essential oil is considerable.
Food preservative is generally divided into chemical synthesis preservative and natural antiseptic agent.The still benzene that China largely uses at present
The chemical syntheses preservatives such as formic acid and its salt, sorbic acid and its salt, parabens.Through long-term application and research hair
The problems such as some existing synthetic preservatives lure carcinous, teratogenesis and easily cause food poisoning.Long-term consumption or the excessive appearance of amount
Easily in people's internal deposition, therefore there is carcinogenic possibility.And in the production process of synthetic preservative, poison gas is will produce
Body has certain harm to the working environment of people, and be easy to cause environmental pollution.A large amount of result of study shows one in recent years
A little natural plants and its extract have certain antiseptic and inhibiting bacteria function effect.Natural antiseptic agent is harmful to human health, the peace used
Full property has also fully been confirmed.
Invention content
The object of the present invention is to provide it is a kind of it is environmentally friendly, at low cost, there is antibacterial antioxidation, convenient for promoting the use of and pure
The preparation method of natural food preservative.
Solving above-mentioned technical problem the technical solution adopted by the present invention is：It is a kind of to prepare food using Chinese cassia tree oil extract waste liquid
The method of preservative, it is characterised in that：Include the following steps：
A. trans-cinnamaldehyde and Chinese cassia tree acid blend are extracted from Chinese cassia tree oil extract waste liquid：
(1) water phase distillate is collected, water phase distillate is the water phase flowed out from the oil water separator of Chinese cassia tree oil extractor
Distillate, or water phase distillate that will be collected after the brownish black muddiness waste liquid re-distillation in Chinese cassia tree oil extractor；
(2) sodium chloride or potassium chloride are added into above-mentioned acquired water phase distillate, make in water phase distillate it is trans--
Cinnamic acid and cinnamic acid are precipitated；
(3) organic solvent is added into the water phase distillate after step (2) to be extracted, the organic solvent of addition is
N-hexane or acetone or ethyl acetate, organic solvent and the water phase distillate volume ratio taken are 1/6, are taken after extraction organic molten
Agent phase；
(4) organic solvent acquired by step (3) is mutually evaporated under reduced pressure, obtains brown oil liquid；
(5) cryogenic freezing is carried out to the brown oil liquid acquired by step (4), wait that crystallization is precipitated, rapid filtration under suction to obtain the final product
To trans-cinnamaldehyde and Chinese cassia tree acid blend, the content of trans-cinnamaldehyde is the content of 75~90%, cinnamic acid in mixture
It is 10~25%；
B. the prepared trans-cinnamaldehydes obtained of above-mentioned steps a and Chinese cassia tree acid blend, have the anti-oxidant work of stronger antibacterial
Property, make food preservative using the trans-cinnamaldehyde and Chinese cassia tree acid blend that are obtained prepared by above-mentioned steps a.
The further technical solution that the present invention uses is：It is flowed out in the oil water separator of Chinese cassia tree oil extractor in step (1)
Water phase distillate be colourless transparent liquid, to isolate the remaining distilled water after cinnamon oil, dissolved with Chinese cassia tree in this water
Volatile ingredient, main component are trans-cinnamic aldehyde and cinnamic acid.
The further technical solution that the present invention uses is：The brownish black muddiness in Chinese cassia tree oil extractor is given up in step (1)
The water phase distillate collected after liquid re-distillation is colourless or micro-strip light brown liquid, in this water the volatility dissolved with Chinese cassia tree at
Point, main component is trans-cinnamaldehyde and cinnamic acid.
The further technical solution that the present invention uses is：Sodium chloride is added in the step (2) or the amount of potassium chloride is：Make
The 50% of concentration when a concentration of saturation solubility of sodium chloride or Klorvess Liquid.
The further technical solution that the present invention uses is：Vacuum distillation in the step (4) is：In temperature be 55 DEG C~
It is evaporated under reduced pressure by Rotary Evaporators under conditions of 65 DEG C.
The further technical solution that the present invention uses is：The temperature of cryogenic freezing in the step (5) be -8 DEG C~-
25 DEG C, cooling time is 3~10 hours.
The further technical solution that the present invention uses is：Trans-cinnamaldehyde and Chinese cassia tree acid blend are to Staphylococcus aureus
Bacterium, Escherichia coli, hay bacillus, aspergillus niger, aspergillus flavus and Penicillium citrinum have bacteriostatic activity, have to DPPH free radicals and remove
Effect, can be used as food preservative.
Due to the adoption of the above technical scheme, the present invention using Chinese cassia tree oil extract waste liquid prepare the method for food preservative with
The prior art is compared, and is had the advantages that：
1. reducing environmental pollution：
Since the present invention is to extract trans-cinnamaldehyde and Chinese cassia tree acid blend from Chinese cassia tree oil extract waste liquid, it is used to prepare
Food preservative.Chinese cassia tree oil extract waste liquid is typically all to be discharged as waste liquid, and the present invention is useless to the Chinese cassia tree oil extract
Liquid is recycled, and the utility value of Chinese cassia tree oil extract waste liquid is not only increased, and also greatly reduces its discharge to environment
Caused by pollute.
2. having antisepsis：
The present invention is the trans-cinnamaldehyde extracted from Chinese cassia tree oil extract waste liquid and Chinese cassia tree acid blend, tool using raw material
There are certain fragrance and good antisepsis, to Escherichia coli, hay bacillus, staphylococcus aureus, aspergillus niger, aspergillus flavus
There is bacteriostatic activity with Penicillium citrinum, there is scavenging effect to DPPH free radicals.
3. reducing cost, small to human body toxic side effect：
And main material used in the present invention is the trans-cinnamaldehyde and cinnamic acid extracted from Chinese cassia tree oil extract waste liquid
Mixture belongs to natural antiseptic agent of plant source.Compared with potassium sorbate, the artificial preservative that sodium benzoate is representative, to people
The toxic side effect of body is small.
4. method is simple and convenient to operate：
Main material used in the present invention is not only to flow out from the oil water separator of Chinese cassia tree oil extractor colourless
Prescribed liquid water phase distillate isolates the remaining distilled water after cinnamon oil, can also be and collect in Chinese cassia tree oil extractor
Brownish black muddiness vinasse, then by this vinasse re-distillation, distillate is collected, other raw material are also existing in the market
Material, and the present invention use mainly comprise the following steps some simpleization such as solution modeling, extraction, vacuum distillation and mixed dissolution
Method, method is simple and convenient to operate, convenient for promoting the use of.
Description of the drawings
Fig. 1 be trans-cinnamaldehyde and Chinese cassia tree acid blend to the scavenging effect of DPPH with concentration situation of change；
Fig. 2 is for cinnamon essential oil to the scavenging effect of DPPH with concentration situation of change；
Fig. 3 is for trans-cinnamaldehyde to the scavenging effect of DPPH with concentration situation of change；
Fig. 4 is for cinnamic acid to the scavenging effect of DPPH with concentration situation of change.
Specific implementation mode
A kind of method preparing food preservative using Chinese cassia tree oil extract waste liquid of the present invention, includes the following steps：
A. trans-cinnamaldehyde and Chinese cassia tree acid blend are extracted from Chinese cassia tree oil extract waste liquid：
(1) water phase distillate is collected, water phase distillate is the water phase flowed out from the oil water separator of Chinese cassia tree oil extractor
Distillate, or water phase distillate that will be collected after the brownish black muddiness waste liquid re-distillation in Chinese cassia tree oil extractor；Wherein meat
The water phase distillate flowed out in the oil water separator of oil of bay extractor is colourless transparent liquid, to isolate the residue after cinnamon oil
Distilled water, the volatile ingredient of Chinese cassia tree is dissolved in this water, main component is trans-cinnamic aldehyde and cinnamic acid；By cinnamon oil
The water phase distillate collected after brownish black muddiness waste liquid re-distillation in extractor is colourless or micro-strip light brown liquid color, this water
In be dissolved with Chinese cassia tree volatile ingredient, main component also be trans-cinnamaldehyde and cinnamic acid；
(2) sodium chloride or potassium chloride are added into above-mentioned acquired water phase distillate, wherein sodium chloride or chlorination is added
The amount of potassium is：The 50% of concentration when making a concentration of saturation solubility of sodium chloride or Klorvess Liquid；Make in water phase distillate
Trans-cinnamaldehyde and cinnamic acid are precipitated；
(3) organic solvent is added into the water phase distillate after step (2) to be extracted, the organic solvent of addition is
N-hexane or acetone or ethyl acetate, organic solvent and the water phase distillate volume ratio taken are 1/6, are taken after extraction organic molten
Agent phase；
(4) organic solvent acquired by step (3) is mutually evaporated under reduced pressure, vacuum distillation is specially：In temperature be 55
DEG C~65 DEG C under conditions of be evaporated under reduced pressure by Rotary Evaporators；Brown oil liquid is obtained after vacuum distillation；
(5) cryogenic freezing is carried out to the brown oil liquid acquired by step (4), the temperature of cryogenic freezing is -8 DEG C
~-25 DEG C, cooling time be 3~10 hours, waited after cryogenic freezing be precipitated crystallization, rapid filtration under suction i.e. obtain trans-cinnamaldehyde and
Chinese cassia tree acid blend, the content of trans-cinnamaldehyde is 75~90% in mixture, the content of cinnamic acid is 10~25%；
B. the preparation-obtained trans-cinnamaldehydes of above-mentioned steps a and Chinese cassia tree acid blend have stronger antibacterial anti-oxidant
Activity, it was proved that trans-cinnamaldehyde and Chinese cassia tree acid blend to staphylococcus aureus, Escherichia coli, hay bacillus,
Aspergillus niger, aspergillus flavus and Penicillium citrinum have bacteriostatic activity, have scavenging effect to DPPH free radicals, use above-mentioned steps a institutes
The trans-cinnamaldehyde and Chinese cassia tree acid blend being prepared into make food preservative.
1. carrying the bacteriostatic experiment of the trans-cinnamaldehyde extracted in oily waste liquid and Chinese cassia tree acid blend from cinnamon oil
1.1 experimental method
1.1.1 for trying strain
Aspergillus flavus (Aspergillus flavus), aspergillus niger (Aspergillus niger), Penicillium citrinum
(Penicillium citrinum), Escherichia coli (Escherichia coli), staphylococcus aureus
(Staphylococus aureus), bacillus subtilis (Bacillus subtilis).
1.1.2 culture medium
PDA culture medium (mould use) (g/L)：Peeled potatoes 200g, glucose 20g, agar 15g, natural ph.Nutrition
Agar medium (bacterium use) (g/L)：Peptone 10g, beef extract powder 3g, sodium chloride 5g, agar powder 15g, pH7.3 ± 0.1.
Nutrient broth medium (bacterial liquid culture use) (g/L)：Peptone 10g, beef extract powder 3g, sodium chloride 5g,
pH7.3±0.1。
Culture medium containing candidate drug (bacterium, mould use)：Nutrient agar (bacterium) or PDA culture medium (mould),
Tween 80, candidate drug.
1.1.3 related solution
Physiological saline, streptomycin sulphate for injection solution (1.35mg/mL), clotrimazole solution (3mg/mL).
1.1.4 the preparation of culture medium
First, 50 bottles of nutrient agar is done, 2% Tween-80 is added, shakes up, is wrapped up, moist heat sterilization at 121 DEG C
20min；Then, on superclean bench, trans-cinnamaldehyde and Chinese cassia tree acid blend (or Chinese cassia tree is added by the concentration gradient of table 1
Essential oil, streptomycin sulphate, clotrimazole), for jog to being down flat plate after even, every bottle is fallen 3 wares, and corresponding label is sticked on tablet, is put down
It puts and waits coagulating.Three groups are finished to doing three groups of antibacterial tests to mould after the antibacterial tests of bacterium again.Nutrient agar is PDA culture medium
Substitution, the moist heat sterilization 30min at 115 DEG C.
The concentration of contained trans-cinnamaldehyde and Chinese cassia tree acid blend, cinnamon essential oil and positive reference substance in 1 culture medium of table
1.1.5 the preparation of bacteria suspension
(1) preparation of bacterium bacteria suspension
A. the preparation of liquid is planted
Strain distinguishes one ring lawn of picking in nutrient broth medium after slant activation 2~3 times, with oese, mixes
Even (each strain prepares 3 bottles) is placed in shaking table, and 37 DEG C, rotating speed 130rpm of temperature control is cultivated for 24 hours, spare as strain liquid.
B. the extension rate of strain liquid is determined
9mL physiological saline is accurately drawn respectively with 10mL pipettes in numbered sterile test tube.It first shakes to be diluted
Meat soup bacterium solution to uniform, then with 1 sterile pipette pipe, for several times, then the accurate 1mL that draws is in 10 for pressure-vaccum back and forth in bacterium solution-1Examination
(note in pipe：The tip of pipette cannot contact 10-1Bacterium solution) concussion is uniform.The another sterile pipette pipe for taking 1 1mL, with same
Mode, 10-1Bacterium solution in purge back and forth for several times, accurate 1mL bacterium solutions of drawing are to 10-2Guan Zhong, and so on.10 are taken respectively-5、10-6、10-7、10-8Bacteria suspension 0.1mL is coated in 37 DEG C of cultures for 24 hours.It is dense that original bacteria liquid is calculated according to flat-plate bacterial colony number
Degree[134]。
Total bacteria count cfu/mL=average colony numbers × extension rate × 10
According to count of bacteria as a result, dilute the strain liquid of each bacterium, it is made into final concentration of 108The Escherichia coli of cfu/mL,
Staphylococcus aureus suspension and 106The hay bacillus suspension of cfu/mL.
C. bacteria suspension is prepared
9mL physiological saline is accurately drawn respectively with 10mL pipettes in numbered sterile test tube.It first shakes to be diluted
Bacterium solution to uniform, then with 1 sterile pipette pipe, for several times, then the accurate 1mL that draws is in 10 for pressure-vaccum back and forth in bacterium solution-1In test tube
(note：The tip of pipette cannot contact 10-1Bacterium solution).The another sterile pipette pipe for taking 1 1mL, in the same way, 10-1
Bacterium solution in purge back and forth for several times, accurate 1mL bacterium solutions of drawing are to 10-2Guan Zhong, and so on, until the dilution determined in (2)
Until.
(2) preparation of mycotic spore suspension
After strain progress slant activation 2~3 times, 48h is cultivated, it is spare.
The mycotic spore on inclined-plane is eluted with physiological saline, after oscillation is so that spore is fully dispersed, as mould
The spore suspension of bacterium.The counting of spore suspension is carried out with blood counting chamber[133].Take spore suspension, the appropriate dilution of progress.It takes dry
The blood counting chamber covered of dry cleaning, spore suspension is dripped a droplet with sterile dropper by coverslip edge (should not mistake
It is more), it allows spore suspension voluntarily to penetrate into, pays attention to cannot thering is bubble generation.5min is stood, blood counting chamber, which is placed in microscope, to be carried
On object platform, into line number bacterium.The specification for the blood counting chamber that this experiment uses is 25 × 16, and total bacteria count is in every milliliter of bacterium solution：
Note：X indicates the spore count per small lattice
According to mycotic spore count as a result, dilute the strain liquid of each mould, be made into final concentration of 106The spore of cfu/mL
Suspension.
1.1.6 the measurement of inhibition zone
Using filter paper enzyme measure trans-cinnamaldehyde and Chinese cassia tree acid blend inhibition zone, and with cinnamon essential oil, it is trans--
Cinnamic acid, cinnamic acid experimental result compared, made with streptomycin sulphate for injection (to bacterium) and clotrimazole (to mould)
Positive control, process are as follows：
Prepare filter paper：With the stronger and homogeneous double-layer filter paper of water absorbing force, the circle of a diameter of 6mm is broken into card punch
Shape filter paper, sets in the culture dish of clean dried, 1~2h of hot air sterilization at 150~170 DEG C.
Culture medium：Bacterium uses nutrient agar, mould to use PDA culture medium.
Specific experiment process：The concussion of prepared bacteria suspension is uniform, on ultrapurification aseptic working platform, with sterile liquid relief
Rifle draw bacterium solution 0.1mL, it is equably coated on to planar surface, just setting incubator 1h (37 DEG C of bacteriological incubator temperature, it is mould
28 DEG C of bacterium incubator temperature).It is got after 1h on ultrapurification aseptic working platform, 3 filter papers is put into positive triangle in each plate,
Then various sample to be tested 10ul are drawn with sterile liquid-transfering gun again to be vertically added drop-wise on filter paper.Bacterium is just setting training in 37 DEG C of constant temperature
It is inverted culture for 24 hours after supporting 1h, mould is inverted culture 48h after 28 DEG C of constant temperature are just setting culture 1h, observes antibacterial situation, and measure suppression
Bacterium loop diameter, is averaged, its fungistatic effect is evaluated with this.
1.1.7 the measurement of minimal inhibitory concentration (MIC)
Using the minimal inhibitory concentration (MIC) of plate dilution assay method trans-cinnamaldehyde and Chinese cassia tree acid blend, and and meat
Osmanthus essential oil, trans-cinnamaldehyde, cinnamic acid experimental result compared, experimental method is as follows：
On clean work station, bacterium bacteria suspension or spore suspension 0.1mL are drawn with sterile liquid-transfering gun, is injected according to label
In the culture medium containing candidate drug solidified, it is equably coated on planar surface, it is (37 DEG C of bacterium, mould to set certain temperature
28 DEG C of bacterium) under, after culture certain time (Bacteria Culture for 24 hours, mycotic culture 48h), the growing state of observation test bacterium.With complete
There is no minimal inhibitory concentration MIC of the Cmin that bacterium grows as each medicine to different bacterium.Blank pair is set up during experiment
According to.
1.1.8 the measurement of minimum bactericidal concentration (MBC)
Anti-microbial property is studied, it is also necessary to which bactericidal properties size is judged by the minimum bactericidal concentration (MBC) of measurement.Its
Process is：Not having the tablet of long bacterium to continue to cultivate in 1.7, bacterium is further cultured for for 24 hours, and mould is further cultured for 48h, takes out observation result.
Originally there may be long bacterium phenomenon without the tablet of long bacterium, and be minimum bactericidal concentration with the minimum concentration completely without bacterium growth
MBC。
1.2 experimental result
1.2.1 the trans-cinnamaldehyde and Chinese cassia tree acid blend Antibacterial Activity extracted from Chinese cassia tree oil extract waste liquid
Using filter paper enzyme determine the trans-cinnamaldehyde extracted from Chinese cassia tree oil extract waste liquid and Chinese cassia tree acid blend,
Cinnamon essential oil and trans-cinnamaldehyde, Chinese cassia tree acid monomers are to for examination bacterium staphylococcus aureus, Escherichia coli, hay bacillus, black song
The bacteriostatic activity of mould, aspergillus flavus and Penicillium citrinum, and sun is made with streptomycin sulphate for injection (to bacterium) and clotrimazole (to mould)
Property control, the results are shown in Table 2.
Fungistatic effect (the unit of 2 trans-cinnamaldehyde of table and Chinese cassia tree acid blend：Millimeter)
Note:Corresponding experiment, no data are not done in expression.
From table 2 it can be seen that trans-cinnamaldehyde and Chinese cassia tree acid blend are to golden yellow grape bacillus, Escherichia coli, withered grass
Bacillus, aspergillus niger, Penicillium citrinum, aspergillus flavus have stronger inhibiting effect.Trans-cinnamaldehyde and Chinese cassia tree acid blend are to golden yellow
Grape bacillus, Escherichia coli, hay bacillus, aspergillus niger, Penicillium citrinum, aspergillus flavus the size of antibacterial circle diameter respectively be
37.8mm、32.0mm、43.2mm、39.3mm、33.0mm、34.8mm；Cinnamon essential oil is to above-mentioned for the big of examination bacterium antibacterial circle diameter
It is small respectively to be 30.8mm, 24.2mm, 37.3mm, 35.0mm, 28.0mm, 30.2mm.
Trans-cinnamaldehyde and Chinese cassia tree acid blend are both greater than cinnamon essential oil to each antibacterial circle diameter for trying bacterium, illustrate from
The trans-cinnamaldehyde and Chinese cassia tree acid blend extracted in cinnamon essential oil extraction waste liquid is obviously high to all fungistatic effects for trying bacterium
In cinnamon essential oil.
Trans-cinnamaldehyde and Chinese cassia tree acid blend are both greater than trans-cinnamaldehyde, Chinese cassia tree to each antibacterial circle diameter for trying bacterium
Acid monomers illustrate to extract the trans-cinnamaldehyde extracted in waste liquid and Chinese cassia tree acid blend to all for trying bacterium from cinnamon essential oil
Fungistatic effect is apparently higher than trans-cinnamyl aldehyde monomer and Chinese cassia tree acid monomers.
1.1.2 the minimal inhibitory concentration of the trans-cinnamaldehyde and Chinese cassia tree acid blend that are extracted from Chinese cassia tree oil extract waste liquid
Using trans-cinnamaldehyde and the cinnamic acid mixing extracted from Chinese cassia tree oil extract waste liquid with plate dilution assay method
Object, cinnamon essential oil and trans-cinnamaldehyde, Chinese cassia tree acid monomers to staphylococcus aureus, Escherichia coli, hay bacillus, aspergillus niger,
The minimal inhibitory concentration of aspergillus flavus and Penicillium citrinum, the results are shown in Table 3.
3 trans-cinnamaldehyde of table and Chinese cassia tree acid blend and cinnamon essential oil are to the various minimal inhibitory concentrations (MIC) for trying bacterium
Note：：Indicate not long bacterium；+：Indicate that thalline dotted (bulk) is grown；++：It is small that thalli growth area accounts for platen area
In 25%；+++：Thalli growth area accounts for platen area 25%~50%；++++：Thalli growth area account for platen area 50%~
75%；+++++：Thalli growth area accounts for platen area 75%~100%
From table 3 it can be seen that trans-cinnamaldehyde and Chinese cassia tree acid blend are to Escherichia coli, staphylococcus aureus, withered grass
Bacillus, Penicillium citrinum, aspergillus niger, aspergillus flavus have certain inhibiting effect, to Escherichia coli, staphylococcus aureus, withered grass bar
Minimal inhibitory concentration of three kinds of the bacterium for trying bacterium is 0.312~1.25ml/L, wherein the inhibiting effect to hay bacillus is most strong most
Small Mlc is 0.312ml/L；It is for the minimal inhibitory concentration for trying mould to three kinds of Penicillium citrinum, aspergillus niger and aspergillus flavus
0.312~0.625ml/L, wherein being 0.312ml/L to the most strong minimal inhibitory concentration of the inhibiting effect of aspergillus niger.
The minimal inhibitory concentration of the test bacterium of trans-cinnamaldehyde and Chinese cassia tree acid blend is below cinnamon essential oil, trans--meat
Cinnamic aldehyde monomer, Chinese cassia tree acid monomers are to the minimal inhibitory concentration of test bacterium, the bacteriostatic activity of trans-cinnamaldehyde and Chinese cassia tree acid blend
It is better than cinnamon essential oil, trans-cinnamyl aldehyde monomer, Chinese cassia tree acid monomers.
1.2.3 the minimum bactericidal concentration of the trans-cinnamaldehyde and Chinese cassia tree acid blend that are extracted from Chinese cassia tree oil extract waste liquid
(MBC)
Minimum bactericidal concentration can accurately reflect the anti-microbial property of bacteriostatic agent, not have long bacterium after measuring minimal inhibitory concentration
Tablet continue to cultivate the corresponding time (bacterium is further cultured for for 24 hours, and mould is further cultured for 48h), record from Chinese cassia tree oil extract waste liquid
The minimum bactericidal concentration of the trans-cinnamaldehyde and Chinese cassia tree acid blend of extraction, is as a result listed in table 4.
4 trans-cinnamaldehyde of table and Chinese cassia tree acid blend are to the various minimum bactericidal concentrations (MBC) for trying bacterium
From table 4, it can be seen that trans-cinnamaldehyde and Chinese cassia tree acid blend are to Escherichia coli, staphylococcus aureus, withered grass
Bacillus, Penicillium citrinum, aspergillus niger and aspergillus flavus bacteriocidal concentration be respectively 2.5ml/L, 1.25ml/L, 0.625ml/L, 0.625ml/
L、0.625ml/L、0.625ml/L；Trans-cinnamaldehyde and Chinese cassia tree acid blend for the bactericidal activity for trying bacterium to being more than cinnamon spirit
Oil, trans-cinnamyl aldehyde monomer, Chinese cassia tree acid monomers.
2. cinnamon oil proposes the anti-oxidant experiment of the trans-cinnamaldehyde extracted in oily waste liquid and Chinese cassia tree acid blend
The antioxygenic property that method evaluates trans-cinnamaldehyde and Chinese cassia tree acid blend, and and cinnamon spirit are removed using DPPH
The antioxygenic property of oil is compared.
2.1 experimental method
Cinnamon oil is carried into the trans-cinnamaldehyde extracted in oily waste liquid and Chinese cassia tree acid blend, cinnamon essential oil, trans--meat
Cinnamic aldehyde monomer, Chinese cassia tree acid monomers, are configured to the solution of various concentration (20~800mg/mL) using absolute ethyl alcohol as solvent respectively.It is accurate
DPPH solids are really weighed, and are made into a concentration of 2 × 10-2The ethanol solution of mg/mL pays attention to being kept in dark place.It is past
2mLDPPH solution is sequentially added in 5.0mL tool plug test tubes, the sample of a certain amount of different volumes is added, with absolute ethyl alcohol
It adds to 4.0mL scales, is sufficiently mixed uniformly.Timing is started simultaneously at, reference is made with absolute ethyl alcohol, (the absorption maximum at 517nm
At wavelength) different sample solutions are measured in the absorbance of Each point in time, it is that can preferably reflect variation tendency experimental selection
Concentration is determined substantially according to double dilution method, and absorbance is surveyed 3 times and is averaged, and determines that the hybrid reaction time is 1h.
It is to be to the clearance rate of DPPH free radicals to define sample antioxidant：
S%=[1- (Ai-Aj)/Ac] × 100
Wherein：The absorbance of Ai=2mLDPPH solution+each sample；
Aj=each sample solution does not add background absorbance when DPPH solution in system；
The absorbance of Ac=2mLDPPH solution+2mL absolute ethyl alcohols.
This experiment makees positive control with tert-butyl hydroquinone (TBHQ) and butylated hydroxy anisole (BHA).
2.2 experimental result
Fig. 1 be trans-cinnamaldehyde and Chinese cassia tree acid blend to the scavenging effect of DPPH with concentration situation of change, Fig. 2 is
Cinnamon essential oil to the scavenging effect of DPPH with concentration situation of change, Fig. 3 be trans-cinnamaldehyde to the scavenging effect of DPPH with
Concentration situation of change, Fig. 4 be cinnamic acid to the scavenging effect of DPPH with concentration situation of change, can be clearly seen that and testing
Under the conditions of, trans-cinnamaldehyde and Chinese cassia tree acid blend, cinnamon essential oil, trans-cinnamyl aldehyde monomer, Chinese cassia tree acid monomers are to DPPH
Free radical all has certain Scavenging activity, and with the increase of concentration, and clearance rate gradually increases.
Trans-cinnamaldehyde and Chinese cassia tree acid blend, cinnamon essential oil, trans-cinnamyl aldehyde monomer, Chinese cassia tree acid monomers are to DPPH
Clearance rate and concentration between have a certain amount imitate relationship, when usually with the clearance rate of DPPH up to 50%, antioxidant sample
Concentration (IC50) weigh Scavenging activity of the sample to DPPH, IC50It is worth smaller, shows that it gets over the Scavenging activity of DPPH
By force.Trans-cinnamaldehyde and Chinese cassia tree acid blend, cinnamon essential oil, trans-cinnamyl aldehyde monomer, Chinese cassia tree can be obtained from Fig. 1~Fig. 4
The IC of acid monomers50Value, is listed in Table 5 below.
5 trans-cinnamaldehyde of table and Chinese cassia tree acid blend remove the ability (IC of DPPH50)
As can be seen from Table 5, the antioxidant activity of trans-cinnamaldehyde and Chinese cassia tree acid blend be better than cinnamon essential oil, it is trans--
Chinese cassia tree aldehyde monomer, Chinese cassia tree acid monomers.
Claims (4)
1. a kind of method preparing food preservative using Chinese cassia tree oil extract waste liquid, it is characterised in that：Include the following steps：
A. trans-cinnamaldehyde and Chinese cassia tree acid blend are extracted from Chinese cassia tree oil extract waste liquid：
（1）Water phase distillate is collected, water phase distillate is that the water phase flowed out from the oil water separator of Chinese cassia tree oil extractor distillates
Liquid, or water phase distillate that will be collected after the brownish black muddiness waste liquid re-distillation in Chinese cassia tree oil extractor；
（2）Sodium chloride or potassium chloride are added into above-mentioned acquired water phase distillate, makes the trans-cinnamyl in water phase distillate
Aldehyde and cinnamic acid are precipitated；
（3）To by step（2）Organic solvent is added in water phase distillate afterwards to be extracted, the organic solvent of addition be just oneself
Alkane or acetone or ethyl acetate, organic solvent and the water phase distillate volume ratio taken are 1/6, and organic solvent is taken after extraction
Phase；
（4）To step（3）Acquired organic solvent is mutually evaporated under reduced pressure, and brown oil liquid is obtained；
（5）To step（4）Acquired brown oil liquid carries out cryogenic freezing, waits that crystallization is precipitated, rapid filtration under suction obtains anti-
Formula-cinnamic acid and Chinese cassia tree acid blend, in mixture the content of trans-cinnamaldehyde be the content of 75 ~ 90%, cinnamic acid be 10 ~
25%；
B. the preparation-obtained trans-cinnamaldehydes of above-mentioned steps a and Chinese cassia tree acid blend have the anti-oxidant work of stronger antibacterial
Property, make food preservative using the preparation-obtained trans-cinnamaldehydes of above-mentioned steps a and Chinese cassia tree acid blend.
2. the method according to claim 1 for preparing food preservative using Chinese cassia tree oil extract waste liquid, it is characterised in that：Institute
State step（2）The middle amount that sodium chloride or potassium chloride is added is：When making a concentration of saturation solubility of sodium chloride or Klorvess Liquid
The 50% of concentration.
3. the method according to claim 1 for preparing food preservative using Chinese cassia tree oil extract waste liquid, it is characterised in that：Institute
State step（4）In vacuum distillation be：It is evaporated under reduced pressure by Rotary Evaporators under conditions of being 55 DEG C ~ 65 DEG C in temperature.
4. the method according to claim 1 for preparing food preservative using Chinese cassia tree oil extract waste liquid, it is characterised in that：Institute
State step（5）In cryogenic freezing temperature be -8 DEG C ~ -25 DEG C, cooling time be 3~10 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510439512.2A CN105124716B (en) | 2015-07-23 | 2015-07-23 | The method for preparing food preservative using Chinese cassia tree oil extract waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510439512.2A CN105124716B (en) | 2015-07-23 | 2015-07-23 | The method for preparing food preservative using Chinese cassia tree oil extract waste liquid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105124716A CN105124716A (en) | 2015-12-09 |
| CN105124716B true CN105124716B (en) | 2018-07-17 |
Family
ID=54710590
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510439512.2A Active CN105124716B (en) | 2015-07-23 | 2015-07-23 | The method for preparing food preservative using Chinese cassia tree oil extract waste liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105124716B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110250395A (en) * | 2019-07-16 | 2019-09-20 | 广西科技大学 | The method for preparing food preservative using husky ginger oil extract waste liquid |
| CN110301572A (en) * | 2019-07-16 | 2019-10-08 | 广西科技大学 | The method for preparing food preservative using Chinese anise oil extract waste liquid |
| CN113143994B (en) * | 2021-01-08 | 2022-07-12 | 广东药科大学 | Water extract of cinnamon oil production residue and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1347971A (en) * | 2001-09-18 | 2002-05-08 | 沈雪荣 | Cassia oil extracting process from cassia twig and leaf |
| CN102952629A (en) * | 2012-12-06 | 2013-03-06 | 广西京桂香料有限公司 | Technological method for extracting natural cinnamon oil |
| CN104003839A (en) * | 2014-06-05 | 2014-08-27 | 褚朝森 | Preparation method of cinnamic acid or derivatives thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ATE350123T1 (en) * | 2001-06-06 | 2007-01-15 | Naturel Corp Llc | LOW TEMPERATURE PROCESS FOR EXTRACTING THE MAIN COMPONENTS FROM PLANTS |
-
2015
- 2015-07-23 CN CN201510439512.2A patent/CN105124716B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1347971A (en) * | 2001-09-18 | 2002-05-08 | 沈雪荣 | Cassia oil extracting process from cassia twig and leaf |
| CN102952629A (en) * | 2012-12-06 | 2013-03-06 | 广西京桂香料有限公司 | Technological method for extracting natural cinnamon oil |
| CN104003839A (en) * | 2014-06-05 | 2014-08-27 | 褚朝森 | Preparation method of cinnamic acid or derivatives thereof |
Non-Patent Citations (1)
| Title |
|---|
| 肉桂醛的研究进展;周明等;《经济动物学报》;20141225;1-5、15 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105124716A (en) | 2015-12-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105124716B (en) | The method for preparing food preservative using Chinese cassia tree oil extract waste liquid | |
| CN104798824A (en) | Botanical fungicide as well as preparation, use and storage methods thereof | |
| CN101708289B (en) | Preparation method for bamboo vinegar antibacterial liquid | |
| CN101049176B (en) | Extractive from bamboo vinegar liquid, preparation method and application | |
| CN109673682B (en) | Preparation method of natural antibacterial mite-killing agent | |
| CN105002251A (en) | Sesame antimicrobial peptide preparation method | |
| CN103210921B (en) | The application of Tea Polyphenols in the biological prevention and control of aflatoxin | |
| CN101223891A (en) | Aniseed essential oil for inhibiting plant pathogenic fungi and preparing method thereof | |
| CN101695301B (en) | Micro-emulsion for killing Monilinia fructicola and preparation method thereof | |
| CN110250395A (en) | The method for preparing food preservative using husky ginger oil extract waste liquid | |
| CN103584253A (en) | Natural preservative with leaf mustard leaves and camphor tree leaves used as raw materials, as well as preparation method and application of natural preservative | |
| CN108208137A (en) | Antimicrobial antistaling agent for fresh-keeping of vegetables and its preparation method and application | |
| CN101612175B (en) | Separation and identification of syringa amurensis rupr. bark volatile oil components and novel application | |
| CN102618386A (en) | Method for preparing chenopodium vulvaria volatile oil and application of chenopodium vulvaria volatile oil | |
| CN110169422A (en) | A kind of combined dosage form bactericide and its preparation method and application | |
| CN103120200A (en) | Preparation method of water-soluble olive polyphenol with bacteriostatic and preserved activity on meat products | |
| CN109350570A (en) | A kind of cosmetics preservative and its application based on natural plant composition | |
| CN102763662B (en) | Medium for separating Peronophythora Litchi Chen ex Ko et al | |
| CN110301572A (en) | The method for preparing food preservative using Chinese anise oil extract waste liquid | |
| CN107502450A (en) | Wooden grape essential oil and its application | |
| CN106306979A (en) | Application of spice extract to inhibition and removal of food-borne pathogenic bacterium biological membrane | |
| CN103610209B (en) | Natural plant preservative taking rape seed cakes and folium ginkgo as raw materials as well as preparation method and application thereof | |
| CN103548884B (en) | Chinese pistache kills Tetranychus cinnabarinus agent and preparation method thereof | |
| CN106472572A (en) | A kind of microbial bactericide and preparation method and application | |
| CN111956672A (en) | Extraction and application of cordyceps militaris antibacterial active substance |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210604 Address after: 311100 No.74 Xingqiao North Road, Xingqiao street, Yuhang District, Hangzhou City, Zhejiang Province Patentee after: Hangzhou Huaweiheng Food Co.,Ltd. Address before: 545006 No. 268 East Ring Road, the Guangxi Zhuang Autonomous Region, Liuzhou Patentee before: GUANGXI University OF SCIENCE AND TECHNOLOGY |
|
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 310000 No. 74, Xingqiao North Road, Xingqiao street, Linping District, Hangzhou City, Zhejiang Province Patentee after: Hangzhou huaweiheng Biotechnology Co.,Ltd. Address before: 311100 No.74 Xingqiao North Road, Xingqiao street, Yuhang District, Hangzhou City, Zhejiang Province Patentee before: Hangzhou Huaweiheng Food Co.,Ltd. |