CN113176129B - Method for verifying regeneration effect between antioxidants by constructing solid-liquid two-phase separable regeneration system - Google Patents
Method for verifying regeneration effect between antioxidants by constructing solid-liquid two-phase separable regeneration system Download PDFInfo
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
Abstract
The invention discloses a method for verifying the regeneration effect among antioxidants by constructing a solid-liquid two-phase separable regeneration system, belonging to the field of the regeneration effect of the antioxidants. The method comprises the steps of dissolving a fat-soluble antioxidant in methanol according to different solubilities of the antioxidants, and performing inclusion on a water-soluble antioxidant and beta-cyclodextrin to form a solid-phase inclusion compound, so that a solid-liquid two-phase separable regeneration system with the antioxidants mutually contacted but not mutually soluble is constructed, and when the water-soluble antioxidant exists or not, the change of the antioxidant capacity in a liquid-phase solution is compared by a DPPH (dehydroepiandrosterone) free radical scavenging method, so that whether the added water-soluble antioxidant has a regeneration effect on the fat-soluble antioxidant is judged. The invention realizes effective verification of the regeneration action between antioxidants, and has the advantages of simple method, less influencing factors and lower cost.
Description
Technical Field
The invention relates to a method for verifying the regeneration effect among antioxidants by constructing a solid-liquid two-phase separable regeneration system, belonging to the field of the regeneration effect of the antioxidants.
Background
Antioxidants are classified according to their source, and antioxidants can be classified into industrial synthetic antioxidants and natural antioxidants. The common synthetic antioxidants are mainly three of tert-butylhydroquinone (TBHQ), 2, 6-di-tert-butyl-4-methylphenol (BHT) and Butylated Hydroxyanisole (BHA). Has long been widely used in industrial production due to the advantages of low price, simple process and strong antioxidant effect. The natural antioxidant is used as a natural green safe antioxidant, and has a wide variety of types, such as vitamin C, E and the like, and is widely applied to the fields of oil, cosmetics and the like. However, compared with natural antioxidants, synthetic antioxidants are often selected as the main antioxidants of foods containing lipids in food enterprises because of their high extraction cost and unsatisfactory antioxidant effect.
Antioxidants can be classified into water-soluble antioxidants and oil-soluble antioxidants and compatible antioxidants according to solubility classification. Fat-soluble antioxidants such as TBHQ and alpha-tocopherol, which are often used in lipid-containing foods to retard the oxidation of fats leading to changes in the flavor of the foods; water-soluble antioxidants such as tea polyphenols, vitamin C, sodium erythorbate and phytic acid are used for slowing down oxidation during processing and storage of fruits and vegetables to ensure food quality.
Food spoilage is primarily caused by oxidation, especially lipid oxidation. The addition of antioxidants is currently the most common method of delaying lipid oxidation and extending the shelf life of foods. In view of the potential toxicity and carcinogenicity of synthetic antioxidants, it is imperative to find alternatives to human health and economic benefits. Natural antioxidants are receiving wide attention because of their abundant resources and their health and high efficiency. The natural antioxidant and the synthetic antioxidant are combined to generate a synergistic antioxidant effect, so that the using amount of the synthetic antioxidant is reduced, and the antioxidant effect is not influenced or even better.
In the practical application process, the use of a single antioxidant often cannot meet the requirements of practical production, so that many researches are carried out to compound two or more antioxidants of different types so as to realize better antioxidant effect. After different antioxidants are compounded, the antioxidant capacity of the antioxidant is obviously better than that of the antioxidant with only one antioxidant, and the phenomenon is called as synergistic action among the antioxidants. The current synergy between antioxidants is mainly attributed to three mechanisms of action: regeneration between antioxidants, reduction of peroxide radical formation, and metal ion chelation. Among them, the regeneration is considered to be a main cause of the synergistic action of the antioxidant. Recent studies have shown that regeneration occurs between antioxidants of the same solubility, and that regeneration may occur between antioxidants of different solubilities. The effective verification of the regeneration effect among different soluble antioxidants can be well applied to two-phase and multi-phase food systems; the regeneration effect of antioxidants with different solubilities is verified, and an effective theoretical basis is provided for the application in a subsequent food system.
At present, the most common method for verifying the regeneration effect of antioxidants with different solubilities is to study the oxidation degree of a system in which a compound antioxidant is located and the oxidation inhibition condition of a single antioxidant to the system, and analyze the regeneration effect by analyzing the generation rule of hydroperoxide or the change condition of oxygen consumption in the oxidation process. Although the method can be used for verifying whether the regeneration action exists between the antioxidants, the operation is complex and the influence factors are more.
Disclosure of Invention
In order to solve the problems of complicated operation and high cost of the method for verifying whether the antioxidants are fully regenerated in the prior art, the method for verifying whether the antioxidants with different solubilities have regeneration effects is provided, and the method for verifying whether the antioxidants with different solubilities have regeneration effects is simple, intuitive and efficient in operation, so that the antioxidants with different solubilities can be well applied to different food systems in the later period.
The invention provides a method for verifying the regeneration effect among antioxidants by constructing a solid-liquid two-phase separable regeneration system, which comprises the following steps:
(1) preparation of separable regeneration system liquid phase:
dissolving the fat-soluble antioxidant in methanol to obtain a fat-soluble antioxidant solution, namely a separable system regeneration system liquid phase.
(2) Preparation of beta-cyclodextrin inclusion compound containing water-soluble antioxidant:
(2.1) preparing a beta-cyclodextrin solution and a water-soluble antioxidant aqueous solution: weighing beta-cyclodextrin in deionized water, heating in a water bath, and fully dissolving to obtain a beta-cyclodextrin solution; dissolving a water-soluble antioxidant in deionized water to prepare a water-soluble antioxidant aqueous solution;
(2.2) preparing a beta-cyclodextrin solution containing a water-soluble antioxidant: dropwise adding a water-soluble antioxidant aqueous solution into the beta-cyclodextrin solution at a constant speed, and magnetically stirring in a magnetic water bath stirring pot;
(2.3) preserving and reserving: and (3) cooling the solution prepared in the step (2.2), crystallizing at 4 ℃, filtering and collecting crystals after no crystals are separated out, rinsing, and drying in vacuum to obtain a solid.
(3) Verification of regeneration effect between antioxidants in solid-liquid two-phase separable regeneration system
(3.1) setting of regeneration group:
and (3) putting the beta-cyclodextrin inclusion compound solid containing the water-soluble antioxidant prepared in the step (2) into the liquid phase of the separable regeneration system prepared in the step (1) to obtain a solid-liquid two-phase separable system, namely a regeneration group.
(3.2) setting of control group:
putting the beta-cyclodextrin inclusion compound without the water-soluble antioxidant with the same mass into the liquid phase of the separable regeneration system prepared in the step (1) to serve as a control group.
(3.3) verification of regeneration: and (3) carrying out shaking table oscillation reaction on the regeneration group and the control group in a sealed dark place, controlling the reaction time to be the same, and measuring the antioxidant capacity of the solutions in the regeneration group and the control group by using a DPPH scavenging free radical method. When the antioxidant capacity of the regeneration group solution is higher than that of the control group, the added water-soluble antioxidant can regenerate the antioxidant in the liquid phase; if there is no significant difference between the two, it is an indication that there is no regeneration between the two antioxidants.
In one embodiment of the present invention, the heating temperature of the β -cyclodextrin water bath in step (2.1) is 60 ℃.
In one embodiment of the invention, the temperature of the magnetic water bath stirring pot in the step (2.2) is 60 ℃, and the stirring time is 6 hours.
In one embodiment of the present invention, in the step (3.3), the DPPH radical scavenging method specifically comprises the following steps: prepare 0.1mmol/L DPPH-methanol solution. When the antioxidant is required to be used, the antioxidant and DPPH are reacted for 30min in a dark place at room temperature, and after the reaction is stable, the absorbance is recorded by ultraviolet detection at 517 nm.
In one embodiment of the present invention, the fat-soluble antioxidant is TBHQ tertbutylhydroquinone.
In one embodiment of the present invention, in the step (2.1), 30g of beta-cyclodextrin is weighed and dissolved in 420g of deionized water by heating in a water bath at 60 ℃ to obtain a beta-cyclodextrin solution.
In one embodiment of the invention, in step (2.2), the magnetic stirring is carried out in a magnetic water bath stirring kettle at 60 ℃ for 6 hours.
In one embodiment of the present invention, the concentration of the fat-soluble antioxidant solution is 1 mmol/L.
In one embodiment of the present invention, the method of binding the water-soluble antioxidant to the β -cyclodextrin to form a solid is a crystallization method.
In an embodiment of the present invention, in the method for verifying the regeneration effect between antioxidants in the solid-liquid two-phase separable regeneration system, the water-soluble antioxidant bound to the β -cyclodextrin is not dissolved in an organic solvent, but is contacted with an organic phase, and the change of the content of the fat-soluble antioxidant in the organic phase can be characterized by measuring the antioxidant capacity in the organic phase, so that the operation of researching the regeneration effect between different soluble antioxidants is simpler and more convenient, and the verification result is more intuitive.
Advantageous effects
1. The invention avoids that the antioxidant capacity of one antioxidant can not be directly measured after the mutual reaction of the antioxidants by constructing a solid-liquid two-phase separable regeneration system, and the method is simpler, more convenient and more intuitive and is less influenced by other factors.
2. The method adopts a DPPH scavenging free radical method to measure the change of the antioxidant capacity in the liquid phase solution, can indirectly represent the change of the content of the fat-soluble antioxidant, does not need large instruments and equipment, and has lower cost.
3. The variables in the separable system can be modified and adjusted according to the requirements of practical application, so that whether regeneration exists between the antioxidants is proved under specific conditions.
4. The antioxidant combination with the regeneration function, which is verified by a solid-liquid two-phase separable regeneration system, can be considered to be applied to a food system to prolong the shelf life of products.
Drawings
FIG. 1: the construction of a solid-liquid two-phase separable regeneration system is shown schematically.
FIG. 2: peroxide values of different sample sets of cream puffs varied over time at different temperatures.
Detailed Description
In order to better understand the present invention, the following examples are further described, but the scope of the present invention is not limited to the examples.
Example 1: verification of regeneration effect of ascorbic acid on TBHQ
(1) Preparation of beta-cyclodextrin inclusion compound containing ascorbic acid
Weighing 30g of beta-cyclodextrin in 420g of deionized water, and heating in a water bath at 60 ℃ to fully dissolve the beta-cyclodextrin to obtain a beta-cyclodextrin solution.
An ascorbic acid solution was prepared by dissolving 15g of ascorbic acid in 150mL of deionized water.
And (3) dropwise adding an ascorbic acid solution into the beta-cyclodextrin solution at a constant speed, and magnetically stirring for 6 hours at 60 ℃ in a magnetic water bath stirring pot. And cooling the solution, placing the cooled solution in a refrigerator at 4 ℃ for crystallization, filtering and collecting crystals after no crystals are separated out, rinsing and drying in vacuum to obtain a solid.
(2) Construction of solid-liquid two-phase separable regeneration system
A1 mmol/L solution of TBHQ in methanol was prepared and 10mL aliquots were taken in 10mL centrifuge tubes. 1g of ascorbic acid and beta-cyclodextrin inclusion compound was weighed into a centrifuge tube, which was a regeneration group. The other portion was supplemented with 1g of beta-cyclodextrin as a control. Two samples were placed on a shaker at 300rpm for 2, 4, 6, 8 days and the reaction was carried out at 25 ℃.
(3) Reproducibility verification
And (3) taking 0.5mL of TBHQ methanol solutions of the regeneration group and the control group at different time points, adding 3mL of DPPH, reacting for 30min in a dark place at room temperature, and after the reaction is stable, detecting and recording the absorbance at 517nm by using ultraviolet. And comparing the oxidation resistance of the regeneration group with that of the control group to judge whether the ascorbic acid has the regeneration effect on the TBHQ. The experimental schematic diagram is shown in figure 1.
Example 2: application experiment of combining ascorbic acid and TBHQ in cream puff proved by solid-liquid two-phase separable system
(1) Manufacturing the puff shell:
adding butter, sugar, water and salt into a pan, heating with middle fire, and stirring to uniformly distribute the oil. Turning to slow fire after boiling, pouring all the flour, quickly stirring to completely mix the flour and the water together until the flour and the water are completely mixed, and turning off the fire. Cooling the batter to 60-65 deg.C, dividing into three groups of control experiments, adding ascorbic acid into two groups, adding 0.2% ascorbic acid into one group, and mixing well. And adding a small amount of eggs, stirring until the batter completely absorbs the eggs, and lifting the batter to form an inverted triangle, wherein the distance from the sharp corner to the bottom is 4cm and the batter cannot slide. Padding tin paper on a baking tray, extruding the batter on the baking tray at equal intervals, preheating in an oven at 210 ℃, and baking for 15 min; when the batter is expanded, the temperature of the oven is reduced to 180 ℃, the baking is continued for 30min, and the batter can be taken out of the oven after the surface is yellow brown.
(2) Preparing puff filling cream:
weighing 3 parts of light cream in equal amount, adding no TBHQ in one part, adding 0.02% of TBHQ in the two parts, and mixing uniformly. Whipping the whipped cream with a whipper to cream for subsequent experiments, the amounts of TBHQ and ascorbic acid added to the puff are shown in Table 1.
TABLE 1 amounts of TBHQ and ascorbic acid added to the puff
(3) Accelerated cream puff storage test
Three groups of puff were placed in one portion each at 4, 15, 25, 30 ℃ storage conditions for accelerated storage experiments.
(4) Extraction of oil from cream
Placing the puff in a conical flask, heating to melt at 70 ℃ in a constant-temperature drying oven, cooling to room temperature, adding petroleum ether according to 3 times of the volume of cream, shaking uniformly, and standing for 12h for extraction. The filter paper was soaked with anhydrous sodium sulfate, the sample was collected by filtration through a funnel, and the petroleum ether was removed by rotary evaporation of the filtrate at 40 ℃. The collected sample was purged with nitrogen and centrifuged at 8000rpm for 10min to remove residual solvent and impurities. Collecting the obtained oil and fat for later use.
(5) Measurement of peroxide value of butter fat
The fat and oil peroxide value of cream is measured by referring to the titration method in GB 5009.227-2016 (determination of peroxide value in food). As a result: the ascorbic acid-TBHQ is combined and applied to the cream puff to effectively slow the rise of the grease oxidation resistance value of cream. The results are shown in FIG. 2.
FIG. 2 shows the peroxide value of cream in the puff of three sample groups.
In conclusion, the solid-liquid two-phase separable regeneration system constructed by the invention can effectively verify the regeneration effect among different soluble antioxidants, and has the advantages of simple operation and low cost; experiments prove that the antioxidant combination with regeneration function has better antioxidant effect in a food system.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for verifying the regeneration effect among antioxidants by constructing a solid-liquid two-phase separable regeneration system is characterized by comprising the following steps:
(1) preparation of separable regeneration system liquid phase:
dissolving a fat-soluble antioxidant in methanol to obtain a fat-soluble antioxidant solution, namely a separable system regeneration system liquid phase;
(2) preparation of beta-cyclodextrin inclusion compound containing water-soluble antioxidant:
(2.1) preparing a beta-cyclodextrin solution and a water-soluble antioxidant aqueous solution: weighing beta-cyclodextrin in deionized water, heating in a water bath, and fully dissolving to obtain a beta-cyclodextrin solution; dissolving a water-soluble antioxidant in deionized water to prepare a water-soluble antioxidant aqueous solution;
(2.2) preparing a beta-cyclodextrin solution containing a water-soluble antioxidant: dropwise adding a water-soluble antioxidant aqueous solution into the beta-cyclodextrin solution at a constant speed, and magnetically stirring in a magnetic water bath stirring pot;
(2.3) preserving and reserving: cooling the solution prepared in the step (2.2), placing the cooled solution in a refrigerator at 4 ℃ for crystallization, filtering and collecting crystals after no crystals are separated out, rinsing, and drying in vacuum to obtain a solid;
(3) verification of regeneration effect between antioxidants in a solid-liquid two-phase separable regeneration system:
(3.1) setting of regeneration group:
putting the beta-cyclodextrin inclusion compound solid containing the water-soluble antioxidant prepared in the step (2) into the liquid phase of the separable regeneration system prepared in the step (1) to obtain a solid-liquid two-phase separable system which is a regeneration group;
(3.2) setting of control group:
putting the beta-cyclodextrin inclusion compound without the water-soluble antioxidant with the same mass into the liquid phase of the separable regeneration system prepared in the step (1) to serve as a control group;
(3.3) verification of regeneration: carrying out shaking table oscillation reaction on the regeneration group and the control group in a sealed dark place, controlling the reaction time to be the same, and measuring the antioxidant capacity of the solution in the regeneration group and the control group by using a DPPH scavenging free radical method; when the antioxidant capacity of the regeneration group solution is higher than that of the control group, the added water-soluble antioxidant can regenerate the antioxidant in the liquid phase; if there is no significant difference between the two, it is an indication that there is no regeneration between the two antioxidants.
2. The method according to claim 1, wherein the heating temperature of the β -dextrin water bath in the step (2.1) is 60 ℃.
3. The method according to claim 1 or 2, wherein the temperature of the magnetic water bath stirring pot in the step (2.2) is 60 ℃, and the stirring time is 6 hours.
4. The method according to any one of claims 1 to 3, wherein in step (3.3), the DPPH scavenging free radical method comprises the following specific steps: prepare 0.1mmol/L DPPH-methanol solution.
5. The method as claimed in any one of claims 1 to 3, wherein the antioxidant is reacted with DPPH at room temperature in a dark place for 30min, and after the reaction is stabilized, the absorbance is recorded by UV detection at 517 nm.
6. The method according to any one of claims 1 to 5, wherein the fat-soluble antioxidant is TBHQ tertbutylhydroquinone.
7. The method according to any one of claims 1 to 6, wherein the step (2.1) is to weigh 30g of beta-cyclodextrin into 420g of deionized water, and heat the mixture in a water bath at 60 ℃ to fully dissolve the beta-cyclodextrin to obtain the beta-cyclodextrin solution.
8. The method according to any one of claims 1 to 7, wherein in step (2.2), the magnetic stirring is carried out in a magnetic water bath stirring kettle at 60 ℃ for 6 hours.
9. The method according to any one of claims 1 to 8, wherein the concentration of the fat-soluble antioxidant solution is 1 mmol/L.
10. The method according to any one of claims 1 to 9, wherein the method for binding the water-soluble antioxidant to the β -cyclodextrin to form a solid is a crystallization method.
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| Regeneration of tert-butylhydroquinone by tea polyphenols;Yafang Guo 等;《Food Research International》;20170220;第1-8页 * |
| Regenerative efficacy of tert-butyl hydroquinone (TBHQ) on dehydrogenated ascorbic acid and its corresponding application to liqueur chocolate;Hang Yu 等;《Food Bioscience》;20210512;第1-8页 * |
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