CN106616900A - Preparation method of composite natural antioxidant - Google Patents
Preparation method of composite natural antioxidant Download PDFInfo
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- CN106616900A CN106616900A CN201611262804.4A CN201611262804A CN106616900A CN 106616900 A CN106616900 A CN 106616900A CN 201611262804 A CN201611262804 A CN 201611262804A CN 106616900 A CN106616900 A CN 106616900A
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- peel
- antioxidant
- natural antioxidant
- dried orange
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- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 120
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002131 composite material Substances 0.000 title abstract description 12
- 235000010837 Echinocereus enneacanthus subsp brevispinus Nutrition 0.000 claims abstract description 42
- 235000006850 Echinocereus enneacanthus var dubius Nutrition 0.000 claims abstract description 42
- 238000000605 extraction Methods 0.000 claims abstract description 42
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- 238000005507 spraying Methods 0.000 claims abstract 2
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
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- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Anti-Oxidant Or Stabilizer Compositions (AREA)
Abstract
A preparation method of a composite natural antioxidant comprises the following steps: (1) after pretreating dried orange peel, shaddock peel and pitaya peel respectively, and carrying out microwave synergistic extraction to obtain crude extracts of the dried orange peel, the shaddock peel and the pitaya peel respectively; (2) carrying out separation and purification on the crude extracts by using large-aperture resin, and respectively refining the crude extracts to obtain extraction concentrated solutions of the dried orange peel, the shaddock peel and the pitaya peel; (3) compounding the extraction concentrated solutions and auxiliaries in proportion to obtain antioxidant composite liquid; and (4) carrying out spraying drying or vacuum drying on the antioxidant composite liquid to obtain the composite natural antioxidant. The preparation method of the composite natural antioxidant is simple to operate, high in extraction rate and low in cost. The composite natural antioxidant which has the characteristics of high efficiency, safety, good stability and wide running range can be obtained.
Description
Technical field
The present invention relates to technical field of food additives, more particularly to a kind of preparation method of complex natural antioxidant.
Background technology
Food additives industry constantly development, has promoted developing rapidly for food antioxidant industry, is made by people always
Synthetized oxidation preventive agent is gradually treated coldly due to there is safety problem by people, and the synthetized oxidation preventive agent that such as early stage is applied is such as
BHT (dibutyl hydroxy toluene), BHA and TBHQ (TBHQ) etc. due to yield it is big, price is low, it is anti-oxidant compared with
Strong advantage, monopolizes always for a long time the market of food antioxidant.However, constantly someone is to artificial synthesized anti-oxidant
The security of agent is queried, and has carried out a series of research to its toxicity that may be present, is as a result shown, artificial synthesized
Antioxidant has certain toxicity and carcinogenesis, therefore natural is gradually occurred in the life of people.
Almost have half to be natural in current health food, such as vitamin E, vitamin C, vitamin A, β-
Carrotene, SOD enzymes etc., but the cost of these naturals is too high, antioxygenic property is not ideal enough, therefore study weight
Point is but the animals and plants extract complicated component of natural source in the extraction of antioxidant, and antioxidant effect is many kinds of substance
Collective effect, effective antioxidant content often do not know, and its antioxidant effect is also not easy to compare on quantitative, to power
Learn and structure activity study brings difficulty.Some natural antioxidants engender commercially, such as rosemary, many distiller's yeasts of tea,
OPC, propolis etc., but there is that antioxidant content is single, and non-oxidizability is low, and extraction cost is high, expensive, city
Field occupation rate is low to be obtained final products and there is easily moisture absorption with the narrow deficiency of use range, and traditional extraction process, no
It is easy to maintain, the problems such as transporting and collect inconvenience.
The content of the invention
It is an object of the invention to propose a kind of preparation method of complex natural antioxidant, its is simple to operate, recovery rate
High, low cost, can obtain the complex natural antioxidant with the wide feature of highly effective and safe, good stability and operation strategies.
It is that, up to this purpose, the present invention is employed the following technical solutions：
A kind of preparation method of complex natural antioxidant, comprises the steps：
(1) it is thick to extract：After pre-processing to dried orange peel, pomelo peel and pitaya peel respectively, by microwave synergistic extraction mode point
Do not obtain the crude extract of dried orange peel, pomelo peel and pitaya peel；
(2) refine：The crude extract of step (1) is isolated and purified using large aperture resin, is refining to obtain respectively
To the extraction concentrate of dried orange peel, pomelo peel and pitaya peel；
(3) compound：The extraction concentrate is proportionally compounded with adjuvant, antioxidant compositional liquor is obtained；
(4) it is dried：By the antioxidant compositional liquor by being spray-dried or being vacuum dried, composite natral is obtained anti-oxidant
Agent.
Further illustrate, pretreatment described in step (1) includes cleaning, is dried and crushes, wherein baking temperature for 50～
65 DEG C, drying time is 4～6h, and smashing fineness is 40～60 mesh.
Further illustrate, the microwave synergistic extraction comprises the steps：
(1) dried orange peel for having pre-processed, pomelo peel and pitaya peel be respectively placed in three extractors respectively；
(2) different concentration ethanol solution is added by the solid-liquid ratio of each setting：Dried orange peel is according to 1:4 solid-liquid ratio is adding 73%
Ethanol solution；Pomelo peel is according to 1:3 solid-liquid ratio is adding 55% ethanol solution；Pitaya peel is according to 1:3 solid-liquid ratio is adding
Plus 60% ethanol solution；
(3) ethanol solution of 5ml is first respectively added in the extractor, Jing after microwave irradiation is extracted, then 25ml is respectively added
Ethanol solution, at 70 DEG C distinguish constant temperature stirring 30min, be filtrated to get crude extract.
Further illustrate, the condition of the microwave irradiation is：Dried orange peel irradiation 80s under 640W microwave powers；It is described
Pomelo peel irradiation 90s under 640W microwave powers；Pitaya peel irradiation 80s under 480W microwave powers.
Further illustrate, the large aperture resin carries out isolating and purifying comprising the steps to the crude extract：
(1) large aperture resin treatment：Large aperture resin absolute ethyl alcohol is fully soaked, then uses water, 0.1mol/ successively
LNaCl and Na2CO3Solution is rinsed, finally with distillation water washing；Take large aperture resin and filter off moisture, post, post are filled using drainage
Diameter 1.0cm, the large aperture resin height of filling is 3.0cm；
(2) by the crude extract using Jing dress post after large aperture resin isolated and purified, adsorption time be 120～
150min, using 0.2%HCl-40% ethanol solutions as eluant, eluent, sample introduction speed is 1.5mL/min, and elution speed is
1.0mL/min。
Further illustrate, the adjuvant includes lecithin, vitamin C and citric acid；The dried orange peel, pomelo peel and flue
Pericarp extract concentrate be with the compound proportion of lecithin, vitamin C and citric acid：3:6:6:0.2:0.1:0.2.
Further illustrate, the Parameter Conditions of the spray drying include that the homogenization pressure of emulsion is 35～40MPa, air intake
Temperature is 170 DEG C, and leaving air temp is 60 DEG C, and feeding temperature is 50 DEG C.
Beneficial effects of the present invention：(1) choose that yield is big, be easy to get and dried orange peel with low cost, pomelo peel and pitaya peel
Raw material, be combined various antioxidant contents, low cost；And by the absorption of microwave synergistic extraction and large aperture resin to anti-oxidant
Effective extraction of composition, can pass through control extraction conditions to improve the anti-oxidant work of purity and unit product of antioxidant composition
Property, simple to operate, recovery rate is high；
(2) will extract concentrate carries out the antioxidant compositional liquor that compounding obtains efficient safety with adjuvant, and its is anti-oxidant
Ability is mainly embodied in and have preferable Scavenging activity to DPPH free radicals, ultra-oxygen anion free radical, hydroxyl radical free radical and go back
Proper energy power, and as the rising of antioxidant compositional liquor concentration, oxidation resistance strengthen, it is more suitable for lipid anti-oxidant
Agent, and to antioxidant effect that linoleic acid, lard, vegetable oil, grease and cake are done well；
(3) the good complex natural antioxidant product of covered effect is obtained by being spray-dried or being vacuum dried, is difficult to inhale
It is wet, it is easy to preservation, the characteristics of there is no potential safety hazard, its range of application can be expanded, it is widely used in food antioxidant, health care
The field such as product and cosmetics.
Description of the drawings
Fig. 1 is the influence curve figure that the microwave power of one embodiment of the invention is extracted to pitaya peel；
Fig. 2 is the influence curve figure that the Microwave Extraction time of one embodiment of the invention extracts to antioxidant；
Fig. 3 is the influence curve figure that the solid-liquid ratio of one embodiment of the invention is extracted to antioxidant；
Fig. 4 is the static adsorption curve map of 5 kinds of resins of one embodiment of the invention；
Fig. 5 is the leakage plot figure under the different sample introduction speed of one embodiment of the invention；
Fig. 6 is the elution curve of the different acid concentrations of one embodiment of the invention；
Fig. 7 is the visible absorption spectra figure that the concentrate of one embodiment of the invention places 7d；
Fig. 8 is the Scavenging activity curve map of the compositional liquor to DPPH free radicals of one embodiment of the invention；
Fig. 9 is 3 kinds of compositional liquors of one embodiment of the invention to 02 -Elimination effect curve map；
Figure 10 is elimination effect curve map of the 3 kinds of compositional liquors of one embodiment of the invention to ultra-oxygen anion free radical；
Figure 11 is the reducing power curve map of 3 kinds of compositional liquors of one embodiment of the invention.
Specific embodiment
Further illustrate technical scheme below in conjunction with the accompanying drawings and by specific embodiment.
A kind of preparation method of complex natural antioxidant, comprises the steps：
(1) it is thick to extract：After pre-processing to dried orange peel, pomelo peel and pitaya peel respectively, by microwave synergistic extraction mode point
Do not obtain the crude extract of dried orange peel, pomelo peel and pitaya peel；
(2) refine：The crude extract of step (1) is isolated and purified using large aperture resin, is refining to obtain respectively
To the extraction concentrate of dried orange peel, pomelo peel and pitaya peel；
(3) compound：The extraction concentrate is proportionally compounded with adjuvant, antioxidant compositional liquor is obtained；
(4) it is dried：By the antioxidant compositional liquor by being spray-dried or being vacuum dried, composite natral is obtained anti-oxidant
Agent.
The present invention is carried with dried orange peel, pomelo peel and pitaya peel as primary raw material respectively through pretreatment, antioxidant content
After taking the refining and concentrating with antioxidant content, spray drying is compounded and carried out with adjuvant and obtains a kind of efficient, safety non-toxic
Complex natural antioxidant；Realize microwave synergistic extraction technique, large aperture resin purification technique and be spray-dried work
Effective combination of skill, obtains the technological parameter and analysis method system of more optimal complex natural antioxidant, can extensively transport
For having technology in enterprise, to producing the food antioxidant of high-quality, health, environmental protection.
The present invention by choose that yield is big, be easy to get and dried orange peel with low cost, pomelo peel and pitaya peel raw material, be combined
Various antioxidant contents, low cost；And by the absorption of microwave synergistic extraction and large aperture resin to the effective of antioxidant content
Extract, control extraction conditions can be passed through to improve the purity and unit product antioxidation activity of antioxidant composition, it is simple to operate,
Recovery rate is high；
Using the method for compounding, concentrate and adjuvant will be extracted carry out compounding the antioxidant for obtaining efficiently, safe and answer
With liquid, by having carried out anti-oxidant experiment to the antioxidant compositional liquor, its oxidation resistance is mainly embodied in DPPH
Free radical, ultra-oxygen anion free radical, hydroxyl radical free radical have preferable Scavenging activity and reducing power, and with antioxidant
The rising of compositional liquor concentration, oxidation resistance strengthens, and is more suitable for lipid antioxidant, and to linoleic acid, lard, plant
The antioxidant effect that oil, grease and cake are done well；
For the unstability to complex natural antioxidant, it is spray-dried or is vacuum dried to finally give covered effect
Good complex natural antioxidant product, it not only has and is difficult moisture absorption, it is easy to preservation, the characteristics of there is no potential safety hazard, can
Its range of application is expanded significantly, is widely used in the fields such as food antioxidant, health products and cosmetics.
Further illustrate, pretreatment described in step (1) includes cleaning, is dried and crushes, wherein baking temperature for 50～
65 DEG C, drying time is 4～6h, and smashing fineness is 40～60 mesh.
Further illustrate, the microwave synergistic extraction comprises the steps：
(1) dried orange peel for having pre-processed, pomelo peel and pitaya peel be respectively placed in three extractors respectively；
(2) different concentration ethanol solution is added by the solid-liquid ratio of each setting：Dried orange peel is according to 1:4 solid-liquid ratio is adding 73%
Ethanol solution；Pomelo peel is according to 1:3 solid-liquid ratio is adding 55% ethanol solution；Pitaya peel is according to 1:3 solid-liquid ratio is adding
Plus 60% ethanol solution；
(3) ethanol solution of 5ml is first respectively added in the extractor, Jing after microwave irradiation is extracted, then 25ml is respectively added
Ethanol solution, at 70 DEG C distinguish constant temperature stirring 30min, be filtrated to get crude extract.
By adopt 95% edible ethanol to be each configured to volume fraction for 55%, 60% and 73% three kinds of ethanol waters
Solution, is respectively intended to the extractant as pomelo peel, pitaya peel and dried orange peel, and extractant can be recycled, cost-effective, and
And according to the characteristics of different raw materials setting certain solid-liquid ratio, so as to realize more preferable microwave synergistic extraction effect, effectively
Composition in protection plant, rate of extraction is fast, improves yield and extraction of substance purity, reduces extractant consumption and waste is produced
Amount, meets environmental protection theory.
Further illustrate, the condition of the microwave irradiation is：Dried orange peel irradiation 80s under 640W microwave powers；It is described
Pomelo peel irradiation 90s under 640W microwave powers；Pitaya peel irradiation 80s under 480W microwave powers.
Because microwave power and irradiation (extraction) time effects the extraction effect of antioxidant composition, therefore for difference
The condition of microwave irradiation of raw material carry out testing preferably, it is preferred so as to obtain dried orange peel, pomelo peel and pitaya peel respectively
Microwave condition.
Further illustrate, the large aperture resin carries out isolating and purifying comprising the steps to the crude extract：
(1) large aperture resin treatment：Large aperture resin absolute ethyl alcohol is fully soaked, then uses water, 0.1mol/ successively
LNaCl and Na2CO3Solution is rinsed, finally with distillation water washing；Take large aperture resin and filter off moisture, post, post are filled using drainage
Diameter 1.0cm, the large aperture resin height of filling is 3.0cm；
(2) by the crude extract using Jing dress post after large aperture resin isolated and purified, adsorption time be 120～
150min, using 0.2%HCl-40% ethanol solutions as eluant, eluent, sample introduction speed is 1.5mL/min, and elution speed is
1.0mL/min。
The crude extract is isolated and purified by the suction-operated of large aperture resin, and during the preferred absorption
Between, the parameter such as the concentration of eluant, eluent and eluant, eluent, sample introduction speed and elution speed, so as to further improve the recovery of antioxidant
Rate, cycles of concentration, it is not only capable of reducing energy consumption, and while avoid the degraded and denaturation of the antioxidant in concentration process.
Further illustrate, the adjuvant includes lecithin, vitamin C and citric acid；The dried orange peel, pomelo peel and flue
Pericarp extract concentrate be with the compound proportion of lecithin, vitamin C and citric acid：3:6:6:0.2:0.1:0.2.
The extraction concentrate is compounded with the lecithin, vitamin C and citric acid, preferably its compounded formula,
So as to optimize the oxidation resistance of the antioxidant compositional liquor, its color is light brown, can adopt paper bag packing and paper web
Packaging, antioxidation activity is suitable with same dosage, and safety and Health, applicability is wide.
Further illustrate, the Parameter Conditions of the spray drying include that the homogenization pressure of emulsion is 35～40MPa, air intake
Temperature is 170 DEG C, and leaving air temp is 60 DEG C, and feeding temperature is 50 DEG C.
When being spray-dried, the EAT, leaving air temp, the homogenization pressure of emulsion and feeding temperature for
The stability of the granular size, rate of drying and moisture and product of spray drying has a large effect, therefore preferably
The homogenization pressure of emulsion is 35～40MPa, and EAT is 170 DEG C, and at 60 DEG C, feeding temperature is 50 DEG C to leaving air temp.
A kind of embodiment-preparation technology of natural composite antioxidant
1st, it is thick to extract
(1) pre-process：
A. the pretreatment of dried orange peel：
Dried orange peel is put into baking oven, 4h is dried at 65 DEG C, crushed, cross 40 mesh hoof, petroleum ether soak degreasing, by the thing after degreasing
Material drying, places standby.
B. the pretreatment of pomelo peel：
Shaddock is gone after pulp, pomelo peel to be cleaned, is dried, shredded, be put into baking oven, 4h is dried at 40 DEG C, crushed, cross 60
Mesh hoof, places standby.
C. the pretreatment of pitaya peel：
Dragon fruit fleshing, pitaya peel are cleaned, dried, shredded, baking oven is put into, 6h is dried at 50 DEG C, crushed, cross 40 mesh
Hoof, places standby.
(2) microwave synergistic extraction
A. operating procedure：
(1) each 5.0g of the dried orange peel for having pre-processed, pomelo peel and pitaya peel is respectively placed in three extractors respectively；
(2) different concentration ethanol solution is added by the solid-liquid ratio of each setting：Dried orange peel adds 73% ethanol solution；Pomelo peel adds
Plus 55% ethanol solution；Pitaya peel adds 60% ethanol solution；
(3) ethanol solution of 5ml is first respectively added in the extractor, Jing after microwave irradiation is extracted, then 25ml is respectively added
Ethanol solution, at 70 DEG C distinguish constant temperature stirring 30min, be filtrated to get crude extract.
B. the Optimum Experiment and Study on influencing factors of extraction process:
Each crude extract is measured using AAS, measures the measurement point of dried orange peel crude extract in 632nm, shaddock
At 513nm, the measurement point of pitaya peel crude extract is at 535nm for the measurement point of sub- skin crude extract；Using OD632, OD513
And OD535The judgement of experiment is optimized respectively as the index of each crude extract.
3 factors of main research include microwave power, irradiation (extraction) time and solid-liquid ratio (g:Ml), fixed wherein two
Individual factor carries out the parallel test of the 3rd factor, and each process counterpoise is multiple 3 times.
1. microwave power：Many parts of the pitaya peel that 10.0g cuts accurately is weighed, in being respectively placed in triangular flask, and thereto
According to solid-liquid ratio (g:Ml it is) 1:3 add 60% ethanol solution 30ml, micro-wave oven peak power 800W, respectively using its 20%,
40%, 60%, 80%, 80s is extracted in the state of 100% peak power, determine the overall OD of final extract535, as a result see figure
1, microwave power shows the impact that pitaya peel is extracted, with the raising of microwave power, OD535It is consequently increased, power is
Highest is reached when 60%, therefore selects Microwave Extraction power to be 60% (480W).
2. irradiation (extraction) time：Many parts of 10.0g pitaya peels are accurately weighed, in being respectively placed in triangular flask, according to 1:3
Solid-liquid ratio (g:Ml) add certain volume pure water, under 60% microwave irradiation power (i.e. 480W), respectively extract 60,
70th, 80,90,100,110,120 and 130s, extract OD535 is determined, as shown in Fig. 2 the Microwave Extraction time carries to antioxidant
The impact for taking, as a result understands, between 60-80s, dragon fruit Fruit peel extract yield is significantly increased with the increase of time.When
When microwave heating time reaches 110s, preferably, prolongation over time afterwards, change is little for extraction effect；In view of anti-oxidant
The heat endurance and efficiency of agent, the OD of 80-100s535It is very nearly the same, therefore optimal selection is 80s.
3. system solid-liquid ratio is extracted：Many parts of 10.0g pitaya peels are accurately weighed, in being respectively placed in triangular flask, and thereto
60% ethanol of different volumes is separately added into, respectively 1:2、1:3、1:4、1:5、1:It is 6 solid-liquid ratio, microwave power 480W, micro-
Extract under conditions of ripple extraction time 80s.Solid-liquid ratio is shown in Fig. 3 to the impact that dragon fruit pericarp antioxidant is extracted, and shows when material
Liquor ratio (g:Ml 1) is reached:When 3, OD535Maximum, afterwards as quantity of solvent increases, declines on the contrary.Dried orange peel and pomelo peel extract
Optimal extraction technology is identical with dragon fruit.Finally giving optimal microwave synergistic extraction condition is：The solid-liquid ratio of pitaya peel
For 1:3, microwave power 480W, microwave irradiation time is 80s；The solid-liquid ratio of dried orange peel is 1:4, microwave power 640W, microwave irradiation
Time is 80s；The solid-liquid ratio of pomelo peel is 1:3, microwave power 640W, microwave irradiation time is 90s.
2nd, refine：
A. experimental procedure：
(1) large aperture resin treatment：Large aperture resin absolute ethyl alcohol is fully soaked, then uses water, 0.1mol/ successively
LNaCl and Na2CO3Solution is rinsed, finally with distillation water washing；Take large aperture resin and filter off moisture, post, post are filled using drainage
Diameter 1.0cm, the large aperture resin height of filling is 3.0cm；
(2) crude extract is isolated and purified using the large aperture resin Jing after dress post, adsorption time is
150min, using 0.2%HCl-40% ethanol solutions as eluant, eluent, sample introduction speed is 1.5mL/min, and elution speed is
1.0mL/min；It is refining to obtain the extraction concentrate of dried orange peel, pomelo peel and pitaya peel；
B. the Optimum Experiment research of dragon fruit antioxidant process for refining:
Dried orange peel extract, pomelo peel extract and dragon fruit Fruit peel extract assay adopt in 632nm, 513nm and
OD value at 535nm, the dry product with respective purifying is drawn calibration curve and is converted as reference.
1. adsorption time：Certain density extract is configured to water, 200mL is respectively taken in 5 conical flasks, is separately added into
The pretreated 5 kinds of macroreticular resins of 0.8g：(Chemical Plant of Nankai Univ. produces for S-8 types, AB-8 types, NKA-9 types, D3520 types, X-5 types
Product), it is placed on shaking table and vibrates, rotating speed is 100r/min, pipettes a small amount of liquid from supernatant liquor respectively per 30min and surveys it
OD535 values, Fig. 4 is Static Adsorption curve of the dragon fruit antioxidant on different resins, as seen from Figure 4, the absorption of S-8 resins
Ability is all stronger than AB-8, NKA-9, D3520, X-5, and as adsorption time extends, supernatant oxidation preventive content exponentially declines,
When adsorption time reaches 150min, adsorption rate is up to 81.9%, and the absorption affinity of other 4 kinds of resins, all very weak, adsorption rate only has
6.7%.
2. in eluant, eluent concentration of alcohol selection：0.20g is taken respectively has adsorbed the wet of dragon fruit pericarp antioxidant
Resin, it is each to add the ethanol water that 50mL concentration is 20%, 40%, 60%, 80%, wherein shaking containing 0.2% hydrochloric acid
10min is vibrated on bed, rotating speed is 100r/min, antioxidant is desorbed from resin, and stripping liquid is diluted to 0.2%HCl
Concentration of alcohol is 20%, measurement, the results are shown in Table 1.
The impact OD535 values that the different ethanol concentration of table 1 is desorbed to antioxidant
The OD value of stripping liquid is higher, illustrates that desorption effect is better.As it can be seen from table 1 when concentration of alcohol is 40%
When, the OD535 value highests of stripping liquid, desorption effect is best；Concentration of alcohol is too high or too low, is all unfavorable for that antioxidant is desorbed.
3. sample introduction speed：Leakage of the dragon fruit pericarp antioxidant on S-8 type macroporous absorption posts under different sample introduction speed
Curve such as Fig. 5, its center line 1～4 is respectively 0.4,1.0,1.5 and 2.0mL/min；As a result show, adsorption flow rate increase, macropore tree
Fat work adsorbance declines, and antioxidant can not fully adsorb just flow out resin bed, and antioxidant is fully absorbed during low flow velocity,
But sample injection time is long；Therefore sample introduction speed is selected to be that 1.5mL/min is more suitable.
4. different acid concentrations：Carried with pitaya peel of the ethanol solution hydrochloride of variable concentrations to absorption on S-8 resin columns
Take liquid to be eluted, elution speed is 1.0mL/min, as a result such as the elution curve of Fig. 6 difference acid concentrations, use 0.2%HCl-
, used as eluant, eluent, peak shape is narrower, and peak value is higher for 40% ethanol solution, and the concentrated effect of antioxidant is good.
5. cycles of concentration and the rate of recovery：Merge the antioxidant peak of the wash-out of 0.2%HCl-40% ethanol solutions, determine anti-
Oxidant concentration is 37.81mg/mL, and the cycles of concentration of sample is 17.7 times, and the rate of recovery is up to 93.4%.
6. in concentrate antioxidant stability：Antioxidant liquid after concentration is placed in 4 DEG C of refrigerators and is preserved, every
1d takes out 1.0mL concentrates, determines the change of absorption spectrum afterwards with 100 times of distilled water diluting, observes Antioxidant Concentrate liquid
Steadiness.Fig. 7 is the visible absorption spectra figure that concentrate places 7d, and as can be seen from Figure within 1 week antioxidant is maximum inhales
Receive value changes slowly, and have no the change that matter occurs, preservation requirement before spray drying can be met.
The experiment more than can be seen that and use large aperture resin S-8 refining and concentrating dragon fruit antioxidants, with 0.2%HCl-
40% ethanol solution reaches 93.4% as eluent, the rate of recovery of antioxidant, and cycles of concentration reaches more than 17 times.
3rd, compounding and anti-oxidant experiment：
A. compound：By the extraction concentrate with lecithin, vitamin C and citric acid according to 3:6:6:0.2:0.1:0.2
Ratio compounded, obtain antioxidant compositional liquor；
B. anti-oxidant experiment：
1. to ultra-oxygen anion free radical O2 -Removing：Concentration is 1.5 × 10-3The luminol solution pH=of mol/L
10.20 0.05mol/LNa2CO3-NaHCO3Buffer preparation, concentration for 0.1mol/L pyrogallol storing solution with 1 ×
10-3The hydrochloric acid of mol/L is prepared, and using front deionized water 1 × 10 is diluted to-4mol/L.Using buffer solution as solvent, prepare not
With the sample solution of concentration.With sample solution of the Flow Injection Analysis/Chemiluminescence instrument sequentially determining from dilute to dense, peak face is read
Product.
Clearance rate=(A0-Ai)/A0× 100%.Wherein A0For blank solution peak area；AiFor sample solution peak area.Jing
SOD, catalase and mannitol detect that the free radical that the system is produced is superoxide anion O2-。
2. to the removing of hydroxyl radical free radical OH：Concentration is 6.4 × 10-4The luminol solution of mol/L, 0.012mol/
LH2O2Matched somebody with somebody respectively with the 0.05mol/L KH2PO4-NaOH cushioning liquid of pH=7.40 with 0.8mg/mL potassium ferrocyanide solutions
System.Using buffer solution as solvent, the sample solution of serial variable concentrations is configured to.According to above-mentioned Flow Injection Analysis/Chemiluminescence side
Method determines and calculates the activity that sample removes hydroxyl radical free radical.
3. to the removing of DPPH free radicals：The sample solution 2.0mL of variable concentrations is taken, is separately added into and is being equipped with 2.0mL's
Concentration is 1 × 10-4In the colorimetric cylinder of mol/L DPP ethanol solutions, lucifuge stands half an hour under room temperature, surveys at 517nm
Amount absorbance Ai.Deionized water replaces sample solution, obtains absorbance A0, absolute ethyl alcohol replace DPPH, obtain absorbance Aj。
Clearance rate=[1- (Ai-Aj)/A0] × 100%.
4. the measure of reducing power：The sample of 2.0mL variable concentrations is taken, the 0.2mol/L phosphoric acid buffers of pH=6.60 are added
The each 2.5mL of the potassium ferricyanide solution of liquid 1% is mixed.Cool down rapidly after 50 DEG C of water-bath 20min, add 2.5mL10% trichloroacetic acids molten
Liquid, 10min is centrifuged after mixing under 3000r/min, takes supernatant 2.0mL, addition 2.5mL deionized waters and 0.5mL0.1%
Liquor ferri trichloridi, standing mensuration absorbance at 700nm after ten minutes.
5. the measure of bacteriostasis：Four kinds are inoculated in respectively in liquid nutrient broth culture medium for examination bacterium, in 37 DEG C, rotating speed
To activate 24h in the shaking table of 100r/min, bacterium solution is set to reach finite concentration.The culture medium for preparing, sterilize 15min in 121 DEG C.
Can be poured into flat board when agar medium is cooled to 45 DEG C or so and shake up, thickness is 1/2 flat board depth.Treat that culture medium coagulates
Gu after add 0.1mL bacteria suspensions, with it is aseptic coating rod coating it is uniform.A moment is stood, is punched (a diameter of 6mm) in flat board, chosen
Go out unnecessary culture medium, in the hole that the injection of 0.1mL sterile solutions has been accomplished fluently, 24h is cultivated at being placed in 37 DEG C, determine inhibition zone straight
Footpath.
6. the measure of minimum inhibitory concentration：Prepare pancreas peptone soybean broth culture medium, 121 DEG C of autoclavings.Using pancreas
Tryptone soya broth carries out test tube serial dilution and obtains the concentration of Tea Polyphenols being respectively 0.01%, 0.02%, 0.03%, 0.04%
And 0.05%；Bamboo vinegar concentration is respectively 0.5%, 1.0%, 1.5%, 2.0% and 2.5%.Connect in each serial culture base
Kind a kind of bacterium, each concentration three is managed parallel, and 18h is cultivated at being placed in 37 DEG C, and growing state is observed afterwards.By each pipe using line
Method inoculation, culture, observe each growing state for examination bacterium, are with the least concentration without bacteria growing in flat board minimum antibacterial dense
Degree MIC.
Dried orange peel, pomelo peel and pitaya peel are extracted into concentrate and lecithin, vitamin C, citric acid enter in the following proportions
Row compounding：A3:6:6:0.2:0.1:0.2；B 3:6:3:0.2:0.1:0.2；C 6:3:3:0.2:0.1:0.2；Will be 3 to more than
The antioxygenic property of formula carries out contrast experiment.
7. to the removing of DPPH free radicals：It is free in liquid system with compounding to the elimination effect of DPPH in from Fig. 8
Base removes the rising of agent content, the Scavenging activity of DPPH is risen, half removing of all free radical scavengers to DPPH free radicals
Rate IC50It is about the same, it is 236.7mL/L, it is all higher than the IC in single product50(208.0m L/L), (206.7mL/L) and
(196.9mL/L).Organic material component containing antioxidation activity in dried orange peel extract and pomelo peel extract, there is removing DPPH
Effect, the active amino of pitaya peel extract, using the teaching of the invention it is possible to provide go back protohydrogen, it may have good DPPH elimination effects.It is multiple
There is synergistic effect after matching somebody with somebody, and the effect of the A that fills a prescription is better than other 2 formulas.
8. to the removing of ultra-oxygen anion free radical：Fig. 9 is 3 kinds of compositional liquors to 02 -Elimination effect.With the increasing of content
Height, compositional liquor is to 02 -Scavenging activity strengthen, comparatively, fill a prescription C effect it is preferable.
9. to the removing of ultra-oxygen anion free radical：Figure 10 represents removing of 3 kinds of compositional liquors to ultra-oxygen anion free radical
Effect.Effect after compounding substantially improves many than the clearance rate of single product, illustrates there is synergistic effect after compounding, especially matches somebody with somebody
The effect of square A is better than other formulas.
10. reducing power：Reducing power is to represent that polyphenoils provides the important indicator of electronic capability, by providing electricity
Son, blocks Fe2+To Fe3+Transformation, so as to show certain reducing power.Figure 11 is the reducing power of 3 kinds of compositional liquors, with
The rising of compositional liquor concentration, absorbance gradually increases, reducing power strengthens, i.e., oxidation resistance strengthens.Compositional liquor is also
In substance system, when absorbance is up to 0.4, corresponding compositional liquor concentration is 80mg/mL, and Tea Polyphenols is corresponding dense in same system
Spend for 65 μ g/mL.
(11) fungistatic effect：
The compositional liquor of table 2 is to for the inhibition (antibacterial circle diameter MM) of examination bacterium
Table 2 is 3 kinds of compositional liquors to four kinds of inhibitions for examination bacterium, it is known that bamboo vinegar is to Escherichia coli, golden yellow grape
Coccus, pseudomonas aeruginosa and vibrio parahemolyticus have different degrees of inhibitory action, wherein the effect of formula A is best.
For complex natural antioxidant oxidation resistance and to for examination bacterium inhibition, as a result show, compound
The oxidation resistance of liquid is mainly embodied in be had preferably clearly to DPPH free radicals, ultra-oxygen anion free radical, hydroxyl radical free radical
Removing solid capacity and reducing power.As the rising of compositional liquor concentration, oxidation resistance strengthen, lipid antioxidant is more suitable for.
Meanwhile, the compositional liquor food-borne pathogens common to four kinds have preferable inhibition, are also the liters with compositional liquor liquid concentration
High and strengthen, when being diluted to 10% concentration, bacteriostasis are greatly lowered.
4th, it is dried：
A. experimental procedure：By the antioxidant compositional liquor by be spray-dried or be vacuum dried, wherein, emulsion it is equal
Matter pressure is 35MPa, and EAT is 170 DEG C, and leaving air temp is 60 DEG C, and feeding temperature is 50 DEG C, and composite natral antioxygen is obtained
Agent.
Application study
1st, to linoleic antioxidation
The size of antioxidant oxidation resistance is evaluated, the present invention is using using wider thiobarbituricacidα- method (TBA
Method).As can be seen from Table 3,0.02% complex natural antioxidant and the Linoleic Acid solution of TBHQ are with the addition of in an experiment, its
Light absorption value rises slowly, and the light absorption value of blank starts rapidly to rise after the cultivation time is 12h.Add i.e. in sample
Complex natural antioxidant as TBHQ to the interception of the very strong row of linoleic lipid peroxidation tool.This experiment
In, complex natural antioxidant is slightly better than the effect of TBHQ to the interception of linoleic lipid peroxidation.
Table 3 is to linoleic antioxidation
2nd, on the snperoxiaized impact of lard lipid
After blank lard sample is placed 18 days in 60 DEG C of constant incubators, the light absorption value under its 532nm is rapidly raised,
Show that now lard autoxidation is fast, MDA (MDA) content produced in sample is entered and increases the phase rapidly；Add anti-oxidant
Light absorption value in each process of agent is constantly in reduced levels, shows the MDA that its oxidation rate is slow, produces in its sample
(MDA) seldom, antioxidant complex natural antioxidant and TBHQ have played antioxidation to content in lard, and pig has been delayed in resistance
The oxydative spoilage of oil.
Antioxidant effect (absorbance) of the sample of the different purity of table 4 to lard
Note：Sample 1,2,3 is respectively the complex natural antioxidant that purity is 60%, 80% and 90%
As can be seen from Table 4, its oxidation resistance of the complex natural antioxidant of different purity has certain difference, and purity is got over
Height, antioxidant effect is better；In the case of equal addition, purity is 60%, 80%, 90% complex natural antioxidant
The lard sample of process is that mda content is low compared with TBHQ in different its light absorption value of detection period, shows that composite natral is anti-oxidant
Agent delays the effect that lard is aoxidized more than TBHQ, and each antioxidant effect for processing is followed successively by 90% α-HT>80% α-HT>60% α-
HT>TBHQ。
Table 5 is to the snperoxiaized inhibiting rate of lard (%)
By watch 5 it can also be seen that antioxidation rate of release is faster than TBHQ, antioxidant capacity in 30 days is processed TBHQ is compared
Greatly.At 10 days, when TBHQ is to the snperoxiaized inhibiting rate of lard only 25%, the suppression of the complex natural antioxidant of different purity
Rate has respectively reached 32.14%, 35.71% and 57.14%, during by 30 days, its antioxygen inhibiting rate still remain in 95% with
On.
Simultaneously it can also be seen that anti-oxidant inhibiting rate is in positive dependence with purity, its inhibiting rate size order is：90%
>α-HT>80% α-HT>60% complex natural antioxidant>TBHQ.
3rd, on the snperoxiaized impact of vegetable oil lipid
Antioxidant effect (absorbance) of the sample of the different purity of table 6 to vegetable oil
Found out by table 6, check plant oil samples started its light absorption value from the 14th day i.e. into the stage is steeply risen, to the 31st
It when its light absorption value up to very high；Each light absorption value for processing is in whole process significantly lower than control.Before 20 days, purity
Light absorption value for 90% complex natural antioxidant is minimum, and purity is 60% and the light absorption value of 80%, TBHQ is close.20 days
Afterwards, the light absorption value of TBHQ belongs to minimum in but processing at four, is secondly 90%, 80%, 60%.Test result indicate that, to planting
For thing oil, complex natural antioxidant is better than TBHQ in the antioxidant effect of early stage, and anaphase effect is slightly worse compared with TBHQ；But it resists
As the antioxidant effect in lard, i.e., in the case of equal addition, antioxidant effect is with purity liter for oxidation effectiveness
It is high and strengthen.
Inhibiting rate of each sample of table 7 to vegetable oil being oxygenized
As shown in Table 7：Each sample is all higher to the peroxidating inhibiting rate of vegetable oil, but it suppresses the snperoxiaized feelings of vegetable oil
Condition is complicated compared with lard.At the 10th day and the 20th day, purity was the inhibiting rate highest that 90% complex natural antioxidant is processed,
Respectively up to 56.82%, 94.49%；And be 92.7% with the inhibiting rate highest of TBHQ during by 30 days.Experiment shows, is combined day
So antioxidant is better than vegetable oil to the antioxidant effect of lard.
4th, the application in pastry product
Complex natural antioxidant is being carried out to grease, in the anti-oxidant experiment of cake, complex natural antioxidant performance
Good antioxidant effect.As a result such as table 8, when complex natural antioxidant addition is 0.04%, rape oil, lard, the moon
The peroxide value time up to standard is respectively blank 2,2.4,3.2 and 5.5 times in cake, walnut shortbread；Work as complex natural antioxidant
When addition is 0.06%, in rape oil, lard, moon cake, walnut shortbread the peroxide value time up to standard be respectively blank 2.3,
3.4th, 4,7.2 times.Show complex natural antioxidant anti-oxidant application effect well.
The oxidation resistant application effect of the complex natural antioxidant of table 8
The know-why of the present invention is described above in association with specific embodiment.These descriptions are intended merely to explain the present invention's
Principle, and can not by any way be construed to limiting the scope of the invention.Based on explanation herein, the technology of this area
Personnel associate other specific embodiments of the present invention by need not paying performing creative labour, these modes fall within
Within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of complex natural antioxidant, it is characterised in that：Comprise the steps：
(1) it is thick to extract：After pre-processing to dried orange peel, pomelo peel and pitaya peel respectively, obtained respectively by microwave synergistic extraction mode
To the crude extract of dried orange peel, pomelo peel and pitaya peel；
(2) refine：The crude extract of step (1) is isolated and purified using large aperture resin, is refining to obtain respectively old
The extraction concentrate of skin, pomelo peel and pitaya peel；
(3) compound：The extraction concentrate is proportionally compounded with adjuvant, antioxidant compositional liquor is obtained；
(4) it is dried：By the antioxidant compositional liquor by being spray-dried or being vacuum dried, complex natural antioxidant is obtained.
2. the preparation method of a kind of complex natural antioxidant according to claim 1, it is characterised in that：In step (1)
It is described pretreatment include cleaning, be dried and crush, wherein baking temperature be 50～65 DEG C, drying time be 4～6h, smashing fineness
For 40～60 mesh.
3. the preparation method of a kind of complex natural antioxidant according to claim 1, it is characterised in that：The microwave association
Comprise the steps with extraction：
(1) dried orange peel for having pre-processed, pomelo peel and pitaya peel be respectively placed in three extractors respectively；
(2) different concentration ethanol solution is added by the solid-liquid ratio of each setting：Dried orange peel is according to 1:4 solid-liquid ratio is adding 73% ethanol
Solution；Pomelo peel is according to 1:3 solid-liquid ratio is adding 55% ethanol solution；Pitaya peel is according to 1:3 solid-liquid ratio is adding
60% ethanol solution；
(3) ethanol solution of 5ml is first respectively added in the extractor, Jing after microwave irradiation is extracted, then the second for respectively adding 25ml
Alcoholic solution, distinguishes constant temperature stirring 30min at 70 DEG C, is filtrated to get crude extract.
4. the preparation method of a kind of complex natural antioxidant according to claim 3, it is characterised in that：The microwave spoke
According to condition be：Dried orange peel irradiation 80s under 640W microwave powers；Pomelo peel irradiation 90s under 640W microwave powers；
Pitaya peel irradiation 80s under 480W microwave powers.
5. the preparation method of a kind of complex natural antioxidant according to claim 1, it is characterised in that：The large aperture
Resin carries out isolating and purifying comprising the steps to the crude extract：
(1) large aperture resin treatment：Large aperture resin absolute ethyl alcohol is fully soaked, then uses water, 0.1mol/LNaCl successively
And Na2CO3Solution is rinsed, finally with distillation water washing；Take large aperture resin and filter off moisture, post, column diameter are filled using drainage
1.0cm, the large aperture resin height of filling is 3.0cm；
(2) by the crude extract using Jing dress post after large aperture resin isolated and purified, adsorption time be 120～
150min, using 0.2%HCl-40% ethanol solutions as eluant, eluent, sample introduction speed is 1.5mL/min, and elution speed is
1.0mL/min。
6. the preparation method of a kind of complex natural antioxidant according to claim 1, it is characterised in that：The adjuvant
Including lecithin, vitamin C and citric acid；The extraction concentrate of the dried orange peel, pomelo peel and pitaya peel and lecithin, dimension life
The compound proportion of plain C and citric acid is：3:6:6:0.2:0.1:0.2.
7. the preparation method of a kind of complex natural antioxidant according to claim 1, it is characterised in that：The spraying is dry
Dry Parameter Conditions include that the homogenization pressure of emulsion is 35～40MPa, and EAT is 170 DEG C, and leaving air temp is 60 DEG C, is entered
Material temperature degree is 50 DEG C.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286395A (en) * | 2017-06-26 | 2017-10-24 | 佛山市凡卡家具有限公司 | A kind of manufacture craft of the natural emulsion mattress of mold-proof oxidation-resistant |
| CN107279668A (en) * | 2017-06-29 | 2017-10-24 | 南通泰和食品有限公司 | A kind of food antioxidant and preparation method thereof |
| CN107836626A (en) * | 2017-09-22 | 2018-03-27 | 安徽丹研食品有限公司 | A kind of highly efficiency compositional food antioxidant and preparation method thereof |
| CN108186804A (en) * | 2018-01-24 | 2018-06-22 | 合肥华盖生物科技有限公司 | A kind of preparation method of complex natural antioxidant |
| CN108244455A (en) * | 2017-12-19 | 2018-07-06 | 安徽强旺生物工程有限公司 | A kind of high efficiency extraction technique of natural flavor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102450726A (en) * | 2011-11-11 | 2012-05-16 | 河南工业大学 | Natural composite antioxidant and preparation method thereof |
| KR20140120069A (en) * | 2013-04-02 | 2014-10-13 | 김영남 | Feed for abalon |
| CN104397826A (en) * | 2014-12-04 | 2015-03-11 | 梁亨 | Preparation method for natural food antioxidant |
| CN105831549A (en) * | 2016-03-30 | 2016-08-10 | 嘉兴市真真老老食品有限公司 | Soybean dreg extract natural composite anti-oxidant and preparation method thereof |
-
2016
- 2016-12-30 CN CN201611262804.4A patent/CN106616900A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102450726A (en) * | 2011-11-11 | 2012-05-16 | 河南工业大学 | Natural composite antioxidant and preparation method thereof |
| KR20140120069A (en) * | 2013-04-02 | 2014-10-13 | 김영남 | Feed for abalon |
| CN104397826A (en) * | 2014-12-04 | 2015-03-11 | 梁亨 | Preparation method for natural food antioxidant |
| CN105831549A (en) * | 2016-03-30 | 2016-08-10 | 嘉兴市真真老老食品有限公司 | Soybean dreg extract natural composite anti-oxidant and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 齐明: "一种新型复合天然抗氧化剂的抗氧化性能研究", 《健康食品与功能性食品配料学术研讨会暨2016年广东省食品学会年会论文集》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286395A (en) * | 2017-06-26 | 2017-10-24 | 佛山市凡卡家具有限公司 | A kind of manufacture craft of the natural emulsion mattress of mold-proof oxidation-resistant |
| CN107279668A (en) * | 2017-06-29 | 2017-10-24 | 南通泰和食品有限公司 | A kind of food antioxidant and preparation method thereof |
| CN107836626A (en) * | 2017-09-22 | 2018-03-27 | 安徽丹研食品有限公司 | A kind of highly efficiency compositional food antioxidant and preparation method thereof |
| CN108244455A (en) * | 2017-12-19 | 2018-07-06 | 安徽强旺生物工程有限公司 | A kind of high efficiency extraction technique of natural flavor |
| CN108186804A (en) * | 2018-01-24 | 2018-06-22 | 合肥华盖生物科技有限公司 | A kind of preparation method of complex natural antioxidant |
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