CN113355156B - Antioxidant, preparation method thereof and application thereof in edible oil - Google Patents

Antioxidant, preparation method thereof and application thereof in edible oil Download PDF

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CN113355156B
CN113355156B CN202110733288.3A CN202110733288A CN113355156B CN 113355156 B CN113355156 B CN 113355156B CN 202110733288 A CN202110733288 A CN 202110733288A CN 113355156 B CN113355156 B CN 113355156B
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antioxidant
cumin
garlic
oil
supercritical extraction
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CN113355156A (en
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任元元
吴淼
陈功
游敬刚
张鑫
邹育
孟资宽
华苗苗
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Sichuan Food Fermentation Industry Research and Design Institute
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    • 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
    • C11B5/00—Preserving by using additives, e.g. anti-oxidants
    • C11B5/0085—Substances of natural origin of unknown constitution, f.i. plant extracts
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/06—Preservation of finished products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0203—Solvent extraction of solids with a supercritical fluid
    • 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
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • 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
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C11B9/025—Recovery by solvent extraction
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Botany (AREA)
  • Biochemistry (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Fats And Perfumes (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention relates to the technical field of antioxidation, and discloses an antioxidant, a preparation method thereof and application thereof in edible oil; the antioxidant comprises mixed extracts of star anise, cassia bark, cumin and garlic, and the preparation method of the antioxidant comprises the following steps: mixing the star anise, the cassia bark and the cumin, and crushing and screening to obtain screened materials; slicing and crushing the garlic to obtain crushed material; mixing the screened material and the crushed material, and extracting to obtain the product; the invention also discloses edible oil added with the antioxidant; according to the invention, the mixed extract of star anise, cassia bark, cumin and garlic is used as the antioxidant, so that the synergistic effect of the components is achieved, the antioxidant effect of the antioxidant on edible oil is improved, and the antioxidant is safe and harmless.

Description

Antioxidant, preparation method thereof and application thereof in edible oil
Technical Field
The invention relates to the technical field of oxidation resistance, and for example relates to an antioxidant, a preparation method thereof, application of the antioxidant in edible oil, and the edible oil added with the antioxidant.
Background
The edible oil is particularly easy to be automatically oxidized due to the factors of illumination, oxygen and the like in the external environment in the process of storage and circulation, so that the quality of the edible oil is deteriorated, the original nutritive value and flavor are lost, and even harmful substances are generated. To avoid this, the addition of antioxidants to edible oils is a simple and effective way. Antioxidants are classified into synthetic antioxidants and natural antioxidants according to their sources, and the synthetic antioxidants commonly used in industry include Butyl Hydroxy Anisole (BHA), 2, 6-di-tert-butyl-p-cresol (BHT), propyl Gallate (PG), and tert-butyl hydroquinone (TBHQ), which can solve the problem of oxidation of fats and oils, but also pose a safety hazard to consumers. Therefore, the natural antioxidant is used to replace the synthetic antioxidant, which is a trend of food antioxidant development in the future.
Chinese patent document CN201910552704.2, application date 2019.06.25, with the name: an antioxidant edible oil additive is disclosed, which comprises astaxanthin, pseudo-ginseng extract, linseed oil, pine needle powder, cassia bark, an edible oil curing agent, hawthorn, a trace element additive and a vitamin additive. The antioxidant edible oil additive is prepared by reasonably matching healthy raw materials, and has no side effect on human body; however, the antioxidant edible oil additive does not fully utilize the characteristics of the raw materials, and is simply mixed, so that the antioxidant effect is poor.
In summary, there is a need for an antioxidant and a preparation method thereof, so as to achieve synergistic interaction between the components, thereby improving the antioxidant effect of the antioxidant on edible oil, and having safe and harmless effects.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an antioxidant, a preparation method and application thereof and edible oil added with the antioxidant, so that at least the components of the antioxidant are synergistic, the antioxidant effect of the antioxidant on the edible oil is improved, and the edible oil is safe and harmless.
The purpose of the invention is realized by the following technical scheme:
in one aspect, an antioxidant is provided, comprising a mixed extract of anise, cinnamon, cumin and garlic.
In some embodiments, the raw materials of the antioxidant comprise, by weight, 8-10 parts of anise, 17-20 parts of cassia bark, 6-8 parts of cumin and 4-6 parts of garlic.
In some embodiments, the weight percentage of volatile oils in the star anise is not less than 8%; and/or the weight percentage of the volatile oil in the cassia bark is not less than 1 percent; and/or the weight percentage of the volatile oil in the cumin is not less than 3 percent; and/or the weight percentage of the volatile oil in the garlic is not less than 0.2%; and/or the weight percentage of the moisture in the aniseed is not more than 5 percent; and/or the weight percentage of the water in the cassia bark is not more than 5 percent; and/or the weight percentage of moisture in the cumin is not more than 5%.
In some of the above embodiments, the anise extract in the antioxidant contains active substances such as anisic aldehyde and anise camphor, which can inhibit chain reaction by scavenging free radicals generated by oxidation reaction of edible oil, thereby achieving antioxidant effect; wherein the active substance is reactive with superoxide radical (. O) 2 - ) The scavenging ability of (A) is obvious, and the scavenging ability of (B) is slightly weaker than that of other free radicals.
The extract of cortex Cinnamomi Japonici in the antioxidant contains active substances such as cinnamaldehyde and coumarin, which can scavenge hydroxyl free radical (. OH) and nitrogen dioxide free radical (NO) 2 H), and the like, and has the capability of chelating metal ions and reducing; wherein, the active substance has prominent scavenging ability to 1, 1-diphenyl-2-trinitrophenylhydrazine free radical (DPPH), and has weaker scavenging ability to other free radicals.
The cumin extract in the antioxidant contains volatile substances such as cuminic aldehyde and cuminic alcohol, and the volatile substances have the capability of reducing iron ions and can scavenge free radicals by inhibiting the capability of transferring electrons by the free radicals; the volatile substance has better scavenging ability for hydroxyl free radicals (. OH), and tests prove that under the same concentration, the clearance rate of the cumin extract for the hydroxyl free radicals (. OH) is higher than that of 2, 6-di-tert-butyl-p-cresol (BHT) and vitamin C (Vc), but the clearance ability for other free radicals is slightly weaker.
The garlic extract in the antioxidant belongs to polyphenols, has good antioxidant capacity, has good scavenging effect on 2, 2-diaza-bis (3-ethyl-benzothiazole-6-sulfonic acid) diammonium salt (ABTS), hydroxyl free radical (. OH) and 1, 1-diphenyl-2-trinitrophenylhydrazine free radical (DPPH), and has slightly weak scavenging capacity on other free radicals.
In some embodiments, the ratio of the raw materials of the antioxidant is controlled to prepare four extracts in corresponding ratios, so as to form the antioxidant with excellent stability and oxidation resistance; the four extracts can generate a synergistic effect after being compounded because different extracts have different abilities of eliminating different free radicals, so that the antioxidant has remarkable eliminating ability to various free radicals, and has excellent reducing ability.
In another aspect, there is provided a method of making an antioxidant as described in any of the above embodiments, comprising: mixing the star anise, the cinnamon and the cumin, and crushing and screening to obtain screened materials; slicing and crushing the garlic to obtain crushed material; and mixing the screening material and the crushed material, and extracting to obtain the fertilizer.
In some embodiments, the screen is 60 to 80 mesh; and/or the extraction is supercritical extraction.
In some embodiments, the supercritical extraction medium is carbon dioxide.
In some embodiments, the temperature of the supercritical extraction is 40 to 45 ℃; and/or the pressure of the supercritical extraction is 33-35 MPa; and/or the time of the supercritical extraction is 50-60 min; and/or the flow rate of the carbon dioxide is 24-32L/h.
In some of the above embodiments, the content of the volatile oil in the anise, cinnamon and cumin is controlled to ensure the yield of the antioxidant. In addition, the water content in the aniseed, the cinnamon and the cumin is controlled, so that the supercritical carbon dioxide extraction is facilitated; for example, if the moisture content is high, the difficulty of the supercritical extraction increases.
In a further aspect, there is provided a use of the antioxidant of any of the above embodiments in an edible oil.
In another aspect, there is provided an edible oil added with the antioxidant described in any of the above embodiments.
In some embodiments, the antioxidant is present in an amount of 3% to 5% by weight of the edible oil; and/or the edible oil comprises at least one of rapeseed oil, peanut oil, corn oil, lard, tallow and chicken oil.
In some of the above embodiments, by limiting the addition amount of the antioxidant, the antioxidant effect of the antioxidant on the edible oil can be improved under the condition that the flavor of the edible oil is ensured. For example, if the amount of the antioxidant added is too low, the antioxidant effect is not good; for example, if the amount of the antioxidant added is too high, the flavor of the edible oil is impaired.
The invention has the beneficial effects that:
1. according to the invention, the mixed extract (volatile oil) of the aniseed, the cinnamon, the cumin and the garlic is used as the antioxidant of the edible oil, and the natural antioxidant replaces the artificially synthesized antioxidant, so that the potential safety hazard of consumers caused by adding the artificially synthesized antioxidant to the edible oil is solved, and the safety of food is improved.
2. The antioxidant of the invention can greatly improve the antioxidation effect on the edible oil, thereby effectively prolonging the shelf life of the edible oil.
3. The extracts in the antioxidant can generate positive synergistic effect, the defect of single function of a single extract is overcome, and various antioxidant active substances with different action mechanisms are synergistically enhanced, so that excellent antioxidant effect is realized, and the shelf life of the edible oil is prolonged.
4. The invention adopts the supercritical extraction technology, ensures higher extraction yield by utilizing lower viscosity and higher diffusion coefficient of fluid in the supercritical extraction, thereby efficiently extracting volatile oil in star anise, cassia bark, cumin and garlic, avoiding residual solvent pollution caused by the traditional organic solvent extraction, and being safe and environment-friendly.
Detailed Description
The technical solutions in some embodiments of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived from the embodiments provided by the invention and obtained by a person skilled in the art, are within the scope of the present disclosure.
In describing some embodiments, the expression "a and/or B" may be used. It is readily understood that "a and/or B" includes the following three combinations: a alone, B alone, and a combination of A and B.
Example 1
1. An antioxidant comprises mixed extracts of fructus Anisi Stellati, cortex Cinnamomi Japonici, cuminum celery and Bulbus Allii.
Wherein the raw materials of the antioxidant comprise 8 parts of aniseed, 17 parts of cassia bark, 6 parts of cumin and 4 parts of garlic in parts by weight; the weight percentage of volatile grease in the star anise is 8 percent, and the weight percentage of water is 5 percent; the weight percentage of volatile oil and fat in the cassia bark is 1 percent, and the weight percentage of water is 5 percent; the weight percentage of the volatile oil in the cumin is 3 percent, and the weight percentage of the water is 5 percent; the weight percentage of the volatile oil in the garlic is 0.2 percent.
2. A method for preparing the antioxidant comprises the following steps:
s1, mixing star anise, cassia bark and cumin, crushing, and sieving by using a 60-mesh sieve to obtain sieved materials;
s2, cutting garlic into slices and then chopping the slices to obtain crushed materials;
s3, mixing the sieved material and the crushed material, putting the mixture into an extraction kettle, and performing supercritical extraction to obtain the product; wherein, the supercritical extraction conditions are as follows: the medium is carbon dioxide, the flow rate of the carbon dioxide is 24L/h, the temperature is 40 ℃, the pressure is 33Mpa, and the time is 50min.
3. Rapeseed oil added with the antioxidant; wherein the weight of the antioxidant accounts for 5% of the weight of the rapeseed oil.
Example 2
1. An antioxidant comprises mixed extracts of fructus Anisi Stellati, cortex Cinnamomi Japonici, cuminum celery and Bulbus Allii.
Wherein, the raw materials of the antioxidant comprise 9 parts of aniseed, 19 parts of cassia bark, 7 parts of cumin and 5 parts of garlic by weight; the weight percentage of volatile grease in the star anise is 8 percent, and the weight percentage of water is 5 percent; the weight percentage of volatile oil and fat in the cassia bark is 1 percent, and the weight percentage of water is 5 percent; the weight percentage of the volatile oil and fat in the cumin is 3 percent, and the weight percentage of the water is 5 percent; the weight percentage of the volatile oil in the garlic is 0.2 percent.
2. A method for preparing the antioxidant comprises the following steps:
s1, mixing star anise, cassia bark and cumin, crushing, and sieving with a 70-mesh sieve to obtain sieved materials;
s2, cutting garlic into slices and then chopping the slices to obtain crushed materials;
s3, mixing the sieved material and the crushed material, putting the mixture into an extraction kettle, and performing supercritical extraction to obtain the product; wherein, the supercritical extraction conditions are as follows: the medium is carbon dioxide, the flow rate of the carbon dioxide is 28L/h, the temperature is 43 ℃, the pressure is 34Mpa, and the time is 55min.
3. Rapeseed oil added with the antioxidant; wherein the weight of the antioxidant accounts for 4% of the weight of the rapeseed oil.
Example 3
1. An antioxidant comprises mixed extracts of fructus Anisi Stellati, cortex Cinnamomi Japonici, cuminum celery and Bulbus Allii.
Wherein, the raw materials of the antioxidant comprise 10 parts of aniseed, 20 parts of cassia bark, 8 parts of cumin and 6 parts of garlic by weight; the weight percentage of volatile grease in the star anise is 8 percent, and the weight percentage of water is 5 percent; the weight percentage of volatile oil and fat in the cassia bark is 1 percent, and the weight percentage of water is 5 percent; the weight percentage of the volatile oil and fat in the cumin is 3 percent, and the weight percentage of the water is 5 percent; the weight percentage of the volatile oil in the garlic is 0.2 percent.
2. A method for preparing the antioxidant comprises the following steps:
s1, mixing star anise, cassia bark and cumin, crushing, and sieving with an 80-mesh sieve to obtain sieved materials;
s2, cutting garlic into slices and then chopping the slices to obtain crushed materials;
s3, mixing the sieved material and the crushed material, putting the mixture into an extraction kettle, and performing supercritical extraction to obtain the product; wherein, the supercritical extraction conditions are as follows: the medium is carbon dioxide, the flow rate of the carbon dioxide is 32L/h, the temperature is 45 ℃, the pressure is 35Mpa, and the time is 60min.
3. Rapeseed oil added with the antioxidant; wherein, the weight of the antioxidant accounts for 3 percent of the weight of the rapeseed oil.
Blank control example
The rapeseed oil in the embodiment 3 of the invention is compared with a blank control example, wherein the blank control example is different from the embodiment 3 in that: no antioxidant was added to the rapeseed oil (in this blank control example, no antioxidant was added to the rapeseed oil, compared to example 3, in order to demonstrate that the antioxidant of the present invention has a good effect).
Comparative example 1
The rapeseed oil of example 3 according to the invention is compared with comparative example 1, wherein comparative example 1 differs from example 3 in that: the antioxidant was replaced with an extract of anise, the weight of the raw materials being the same as the total weight of the raw materials in example 3. The preparation method of the aniseed extract comprises the following steps: pulverizing star anise, sieving with a 80-mesh sieve to obtain sieved materials, mixing the sieved materials, putting into an extraction kettle, and performing supercritical extraction on the materials, wherein the medium is carbon dioxide, the flow rate of the carbon dioxide is 32L/h, the temperature is 45 ℃, the pressure is 35Mpa, and the time is 60min to obtain the star anise antioxidant (compared with the comparative example 3, the antioxidant is replaced by the star anise extract, which is used for proving that the antioxidant has a better effect).
Comparative example 2
The rapeseed oil of the invention in example 3 is compared with the rapeseed oil of the comparative example 2, wherein the comparative example 2 differs from the example 3 in that: the antioxidant was replaced with an extract of cinnamon, the weight of the raw materials being the same as the total weight of the raw materials in example 3. The preparation method of the cinnamon extract comprises the following steps: crushing cinnamon, sieving with a 80-mesh sieve to obtain a sieved material, mixing the sieved materials, putting into an extraction kettle, and performing supercritical extraction with a medium of carbon dioxide, a flow rate of the carbon dioxide of 32L/h, a temperature of 45 ℃, a pressure of 35Mpa and a time of 60min to obtain the antioxidant (compared with example 3, the antioxidant is replaced by the extract of the cinnamon to prove that the antioxidant has a better effect).
Comparative example 3
The rapeseed oil of example 3 according to the invention is compared with comparative example 3, wherein comparative example 3 differs from example 3 in that: the antioxidant was replaced with cumin extract, the weight of the raw materials being the same as the total weight of the raw materials in example 3. The preparation method of the cumin extract comprises the following steps: crushing cumin, sieving by a sieve of 80 meshes to obtain sieved materials, mixing the sieved materials, putting the sieved materials into an extraction kettle, and performing supercritical extraction on the materials, wherein the medium of the supercritical extraction is carbon dioxide, the flow rate of the carbon dioxide is 32L/h, the temperature is 45 ℃, the pressure is 35Mpa, and the time is 60min to obtain the cumin antioxidant (compared with the comparative example 3, the antioxidant is replaced by the cumin extract, which is used for proving that the antioxidant has better effect).
Comparative example 4
The rapeseed oil of example 3 according to the invention is compared with comparative example 4, wherein comparative example 4 differs from example 3 in that: the antioxidant was replaced with an extract of garlic, the weight of the raw materials of which was the same as the total weight of the raw materials in example 3. The preparation method of the garlic extract comprises the following steps: cutting garlic into slices, chopping to obtain crushed materials, mixing the crushed materials, putting the crushed materials into an extraction kettle, and performing supercritical extraction on the crushed materials in the presence of carbon dioxide in a medium of 32L/h at 45 ℃ and 35Mpa for 60min to obtain the garlic antioxidant, wherein the antioxidant is replaced by garlic extract in comparison with example 3, so as to prove that the antioxidant has a better effect.
Comparative example 5
The rapeseed oil of example 3 according to the invention is compared with a control example 5, wherein the control example 5 differs from the example 3 in that: the antioxidant was replaced with an extract of anise, the weight of the raw material being the same as the weight of anise in example 3. The preparation method of the aniseed extract comprises the following steps: pulverizing star anise, sieving with a 80-mesh sieve to obtain sieved materials, mixing the sieved materials, putting the materials into an extraction kettle, and performing supercritical extraction on the materials, wherein the medium is carbon dioxide, the flow rate of the carbon dioxide is 32L/h, the temperature is 45 ℃, the pressure is 35Mpa, and the time is 60min to obtain the star anise antioxidant.
Comparative example 6
The rapeseed oil of example 3 according to the invention is compared with a comparative example 6, wherein the comparative example 6 differs from the example 3 in that: the antioxidant was replaced with cinnamon extract, and the weight of the raw materials was the same as that of cinnamon in example 3. The preparation method of the cinnamon bark extract comprises the following steps: crushing cinnamon, sieving with a 80-mesh sieve to obtain sieved materials, mixing the sieved materials, placing the sieved materials into an extraction kettle, and performing supercritical extraction on the materials, wherein the medium is carbon dioxide, the flow rate of the carbon dioxide is 32L/h, the temperature is 45 ℃, the pressure is 35Mpa, and the time is 60min to obtain the antioxidant (compared with the comparative example 3, the antioxidant is replaced by the extract of the cinnamon, which is used for proving that the antioxidant has a better effect).
Comparative example 7
The rapeseed oil of example 3 according to the invention is compared with comparative example 7, wherein comparative example 7 differs from example 3 in that: the antioxidant was replaced with cumin extract, the weight of the raw materials being the same as the weight of cumin in example 3. The preparation method of the cumin extract comprises the following steps: crushing cumin, sieving by a sieve of 80 meshes to obtain sieved materials, mixing the sieved materials, putting the sieved materials into an extraction kettle, and performing supercritical extraction on the materials, wherein the medium of the supercritical extraction is carbon dioxide, the flow rate of the carbon dioxide is 32L/h, the temperature is 45 ℃, the pressure is 35Mpa, and the time is 60min to obtain the cumin antioxidant (compared with the comparative example 3, the antioxidant is replaced by the cumin extract, which is used for proving that the antioxidant has better effect).
Comparative example 8
The rapeseed oil of example 3 according to the invention is compared with a control example 8, wherein the control example 8 differs from the example 3 in that: the antioxidant was replaced with an extract of garlic, the weight of the raw material of which was the same as that of garlic in example 3. The preparation method of the garlic extract comprises the following steps: cutting garlic into slices, chopping to obtain crushed material, mixing the crushed material, putting the crushed material into an extraction kettle, and performing supercritical extraction in the presence of carbon dioxide in a medium at a flow rate of 32L/h, a temperature of 45 ℃ and a pressure of 35MPa for 60min to obtain the garlic antioxidant (in the comparative example, compared with example 3, the antioxidant is replaced by garlic extract, which is used for proving that the antioxidant has a better effect).
Comparative example 9
The rapeseed oil of example 3 according to the invention is compared with a comparative example 9, wherein the comparative example 9 differs from the example 3 in that: replacing supercritical extraction during antioxidant preparation with conventional organic solvent extraction at 45 deg.C for 60min; other conditions such as the addition amount of the antioxidant and the preparation process steps are the same as those in example 3 of the present invention (in this comparative example, compared with example 3, the supercritical extraction in the preparation of the antioxidant is replaced by the conventional organic solvent extraction, which is used to prove that the antioxidant of the present invention has a better effect).
Comparative example 10
The rapeseed oil of the invention in example 3 is compared with the rapeseed oil of the comparative example 10, wherein the comparative example 10 differs from the example 3 in that: the antioxidant comprises the following raw materials, by weight, 6 parts of star anise, 20 parts of cassia bark, 8 parts of cumin and 10 parts of garlic; other conditions such as the addition amount of the antioxidant and the preparation process steps are the same as those in example 3 of the present invention (in the comparative example, compared with example 3, the proportion of star anise in the raw material of the antioxidant is too low, and the proportion of garlic is too high, which is used for proving that the antioxidant effect of the present invention is better).
Comparative example 11
The rapeseed oil of example 3 according to the invention is compared with a control example 11, wherein the control example 11 differs from the example 3 in that: the raw materials of the antioxidant comprise, by weight, 14 parts of aniseed, 20 parts of cassia bark, 8 parts of cumin and 2 parts of garlic; other conditions such as the addition amount of the antioxidant and the preparation process steps are the same as those in example 3 of the present invention (in the comparative example, compared with example 3, the proportion of star anise in the raw material of the antioxidant is too high, and the proportion of garlic is too low, which is used for proving that the antioxidant effect of the present invention is better).
Comparative example 12
The rapeseed oil of example 3 according to the invention is compared with a control example 12, wherein the control example 12 differs from the example 3 in that: the antioxidant comprises the following raw materials, by weight, 10 parts of star anise, 24 parts of cassia bark, 4 parts of cumin and 6 parts of garlic; other conditions such as the amount of the antioxidant added and the process steps for the preparation were the same as in example 3 of the present invention (in this comparative example, the ratio of cumin in the raw material of the antioxidant was too low and the ratio of cinnamon was too high compared to example 3, which was intended to prove that the antioxidant effect of the present invention was better).
Comparative example 13
The rapeseed oil of example 3 according to the invention is compared with a comparative example 13, wherein the comparative example 13 differs from the example 3 in that: the antioxidant comprises the following raw materials, by weight, 10 parts of star anise, 16 parts of cassia bark, 12 parts of cumin and 6 parts of garlic; other conditions such as the addition amount of the antioxidant and the process steps of the preparation are the same as those in example 3 of the present invention (in this comparative example, the ratio of cumin in the raw material of the antioxidant is too high and the ratio of cinnamon is too low compared to example 3, which proves that the antioxidant effect of the present invention is better).
Test effects
In order to verify the antioxidant effect of the antioxidant of the present invention on edible oil, the rapeseed oils of examples 1 to 3, blank control example and control examples 1 to 13 were prepared into test samples, and the peroxide value (mmol/kg) of each test sample was measured at month 6, month 12, month 18 and month 24 according to the regulation of GB 1536-2004, to compare the level of antioxidant activity in each test sample. According to the regulation of GB 1536-2004, the peroxide value of the first-grade and second-grade edible oils should be less than or equal to 5mmol/kg, and the peroxide value of the third-grade and fourth-grade edible oils should be less than or equal to 6mmol/kg.
The results are shown in the following table:
Figure BDA0003140499040000081
from the above table it can be seen that:
1) The peroxide numbers of examples 1 to 3, especially example 3, were consistently lower than those of comparative examples 1 to 13, while the peroxide numbers of comparative examples 1 to 13 were consistently lower than those of the blank comparative example. Wherein, the peroxide value of the embodiment 1-3 is still less than or equal to 6mmol/kg at the 24 th month, which accords with the national regulation of peroxide values of third and fourth grade edible oil, especially the peroxide value of the embodiment 3 is still less than or equal to 5mmol/kg at the 24 th month, which accords with the national regulation of peroxide values of first and second grade edible oil; the peroxide numbers of comparative examples 1 to 13 did not reach the required value at month 24. This demonstrates that the antioxidant of the present invention can significantly extend the shelf life of edible oils.
2) The peroxide numbers of examples 1 to 3, particularly example 3, were always lower than those of comparative examples 1 to 4, and the peroxide numbers of comparative examples 1 to 4 were always lower than those of the blank control. That is, regarding the antioxidant effect, the antioxidant effect of the garlic extract, the cinnamon extract, the anise extract and the cumin extract added alone is superior to that of the garlic extract, the cinnamon extract, the anise extract and the cumin extract which are not added, but the antioxidant effect of the garlic extract, the cinnamon extract, the anise extract and the cumin extract which are added simultaneously is inferior to that of the garlic extract, the cinnamon extract, the anise extract and the cumin extract. This demonstrates that the simultaneous addition of garlic extract, cinnamon extract, anise extract and cumin extract to the antioxidant of the present invention has a positive synergistic effect on the improvement of antioxidant effect; it is easy to understand that, in the antioxidant, the garlic extract, the cinnamon extract, the anise extract and the cumin extract have positive synergistic effect on improvement of the antioxidant effect, so that when the requirement on the antioxidant effect of the edible oil is the same, the required amount of the antioxidant is lower, and the cost is saved.
3) The examples 1 to 3, particularly example 3, had peroxide numbers lower than those of comparative example 9. This demonstrates that the antioxidant effect of the obtained antioxidant is improved by employing the supercritical extraction technique in the method for preparing an antioxidant according to the present invention.
4) The peroxide numbers of examples 1 to 3, particularly example 3, were lower than those of comparative examples 10 to 13. The antioxidant effect of the antioxidant is improved by controlling the proportion of the raw materials of the antioxidant to prepare the antioxidant containing the four extracts in corresponding proportions.
In conclusion, the antioxidant disclosed by the invention achieves the synergistic effect among the components, so that the antioxidant effect of the antioxidant on edible oil is improved, and the antioxidant is safe and harmless, and has extremely high application value and wide market prospect.
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (6)

1. An antioxidant is characterized in that the antioxidant is a mixed extract of star anise, cassia bark, cumin and garlic; wherein the raw materials of the antioxidant comprise, by weight, 8 to 10 parts of anise, 17 to 20 parts of cassia bark, 6 to 8 parts of cumin and 4 to 6 parts of garlic; the weight percentage of volatile oil in the star anise is not less than 8%, the weight percentage of volatile oil in the cassia bark is not less than 1%, the weight percentage of volatile oil in the cumin is not less than 3%, the weight percentage of volatile oil in the garlic is not less than 0.2%, the weight percentage of moisture in the star anise is not more than 5%, the weight percentage of moisture in the cassia bark is not more than 5%, and the weight percentage of moisture in the cumin is not more than 5%;
a method of making the antioxidant comprising:
mixing the star anise, the cinnamon and the cumin, and crushing and screening to obtain screened materials;
slicing and crushing the garlic to obtain crushed material;
mixing the screening material and the crushed material, and extracting to obtain the product;
wherein the screening is carried out by sieving with a sieve of 60 to 80 meshes;
the extraction is supercritical extraction; wherein the medium for supercritical extraction is carbon dioxide, and the flow rate of the carbon dioxide is 24 to 32L/h; the temperature of the supercritical extraction is 40 to 45 ℃, the pressure of the supercritical extraction is 33 to 35MPa, and the time of the supercritical extraction is 50 to 60min.
2. A process for preparing the antioxidant of claim 1, comprising:
mixing the star anise, the cinnamon and the cumin, and crushing and screening to obtain screened materials;
slicing and crushing the garlic to obtain crushed material;
mixing the screening material and the crushed material, and extracting to obtain the product;
wherein the screening is performed by sieving through a sieve with 60 to 80 meshes;
the extraction is supercritical extraction; wherein the medium for supercritical extraction is carbon dioxide, and the flow rate of the carbon dioxide is 24 to 32L/h; the temperature of the supercritical extraction is 40 to 45 ℃, the pressure of the supercritical extraction is 33 to 35MPa, and the time of the supercritical extraction is 50 to 60min.
3. Use of the antioxidant of claim 1 in an edible oil.
4. An edible oil characterized by the addition of the antioxidant of claim 1.
5. The edible oil of claim 4, wherein the antioxidant is present in an amount of 3% to 5% by weight of the edible oil.
6. The edible oil of claim 4 or 5, wherein the edible oil comprises at least one of canola oil, peanut oil, corn oil, lard, tallow and chicken oil.
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