CN114015504A - Method for preparing natural antioxidant by utilizing chilli seeds - Google Patents
Method for preparing natural antioxidant by utilizing chilli seeds Download PDFInfo
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- CN114015504A CN114015504A CN202111293645.5A CN202111293645A CN114015504A CN 114015504 A CN114015504 A CN 114015504A CN 202111293645 A CN202111293645 A CN 202111293645A CN 114015504 A CN114015504 A CN 114015504A
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- natural antioxidant
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0082—Regulation; Control
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/16—Evaporating by spraying
- B01D1/18—Evaporating by spraying to obtain dry solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
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- 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
- B01D11/0288—Applications, solvents
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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Botany (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a method for preparing a natural antioxidant by utilizing chilli seeds, which comprises the following steps: separating seed and skin of dry pepper, collecting pepper seeds, and micronizing to obtain dry pepper seed powder; mixing dry pepper seed powder and a degreasing solvent in proportion, stirring at normal temperature, separating a solid phase and a liquid phase, collecting the solid phase pepper seed powder, volatilizing the solvent and drying again; adding methanol solution into the dried chilli seed powder, heating and stirring, and separating solid and liquid phases; collecting the extract, performing rotary evaporation, removing the solvent methanol, drying under vacuum condition, and pulverizing to obtain natural antioxidant product. The method disclosed by the invention is simple and easy to implement, has low cost, and the product has good antioxidation, is purely natural and non-toxic, and can improve the additional value of the pepper product.
Description
Technical Field
The invention relates to a preparation method of a natural antioxidant, in particular to a method for preparing a natural antioxidant by using chilli seeds.
Background
At present, artificial antioxidants such as BHT, BHA, TBHQ and the like are added in the food industry to inhibit the oxidative rancidity of edible oil and fat-rich food, and the artificial antioxidants can generate toxic effects on human bodies when being used in large quantities or for a long time. With the development of social economy and the continuous improvement of the living standard of people, the food safety problem is more and more emphasized by people. Therefore, the development of natural and safe antioxidants has become the development direction of food antioxidants.
In the research of natural and safe antioxidants, researchers have focused their attention on edible plant materials. Since the middle of the 20 th century, hundreds of antioxidants, mainly phenols widely distributed in the plant world, have been extracted from spices, medicinal materials, and crops. Capsicum is an important vegetable and seasoning. The dry red chilli seeds account for about 39% of the total weight of the whole fruit, and the chilli seeds are rich in various antioxidant ingredients.
At present, the antioxidant ingredients are extracted from the chilli seeds by an enzymolysis method, and the method has high cost and strict requirements on process conditions, and is not suitable for large-scale industrial application.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for preparing a natural antioxidant by using chilli seeds, so as to achieve the purposes of simple process, low cost and good antioxidation of products.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for preparing natural antioxidant by using chilli seeds comprises the following steps:
(1) pretreatment: separating seed and skin of dry pepper, collecting pepper seeds, and micronizing to obtain dry pepper seed powder;
(2) degreasing: mixing dry pepper seed powder and a degreasing solvent in proportion, stirring at normal temperature, separating a solid phase and a liquid phase, collecting the solid phase pepper seed powder, volatilizing the solvent and drying again;
(3) extraction: adding methanol solution into the dried chilli seed powder, heating and stirring, and separating solid and liquid phases;
(4) and (3) purification: collecting the extract, performing rotary evaporation, removing the solvent methanol, drying under vacuum condition, and pulverizing to obtain natural antioxidant product.
In the scheme, the degreasing solvent is any one of petroleum ether, n-hexane and ethyl acetate.
In the scheme, in the step (1), the dried pepper seed powder is obtained by passing through a 100-sand 200-mesh screen after the superfine grinding.
In the scheme, in the step (2), the mass ratio of the dry pepper seed powder to the degreasing solvent is 1:5-1: 10.
In the scheme, in the step (2), the stirring time is 1-3h, the drying temperature is 40-50 ℃, and the drying time is 2-4 h.
In the scheme, in the step (3), the mass ratio of the pepper seed powder to the methanol solution is 1:5-1: 10.
In the scheme, in the step (3), the heating temperature is 40-50 ℃, and the stirring time is 2-4 h.
In the scheme, in the step (4), the rotary evaporation condition is 40-50 ℃ and less than-0.08 MPa.
In the scheme, in the step (4), the drying temperature is 45-55 ℃, and the drying time is 3-5 h.
Through the technical scheme, the method for preparing the natural antioxidant by utilizing the chilli seeds, provided by the invention, has the following beneficial effects:
1. the invention can greatly improve the yield of the natural antioxidant product by controlling the mass ratio of the dry pepper seed powder to the methanol solvent.
2. The invention can improve the oxidation activity of the natural antioxidant by controlling the drying temperature during purification.
3. The preparation method is simple and feasible, has low requirements on process conditions, high yield and low cost, and the product has good antioxidation, is purely natural and non-toxic, and can improve the additional value of the pepper product.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below.
Example 1:
separating seed and skin of dry pepper, collecting pepper seeds, micronizing, and sieving with 100 mesh sieve to obtain dry pepper seed powder. Mixing 500kg of dry pepper seed powder with petroleum ether according to the mass ratio of 1:6, stirring at normal temperature for 1h, separating a solid phase from a liquid phase, collecting pepper seed powder solids, volatilizing the solvent, drying again at 45 ℃ for 2h, adding 3000kg of methanol solution, heating to 40 ℃, stirring for 2h, and separating the solid phase from the liquid phase; collecting extractive solution, rotary steaming at 40 deg.C under-0.08 MPa, removing solvent methanol, oven drying at 45 deg.C under vacuum condition for 4 hr, and pulverizing to obtain 13.6kg of natural antioxidant product.
Example 2:
separating seed and skin of dry Capsici fructus, collecting Capsici fructus seed, micronizing, and sieving with 100 mesh sieve to obtain Capsici fructus seed powder. Mixing 1000kg of dry pepper seed powder and n-hexane according to the mass ratio of 1:8, stirring at normal temperature for 1h, separating a solid phase and a liquid phase, collecting pepper seed powder solids, volatilizing the solvent, drying at 48 ℃ for 4h again, adding 8000kg of methanol solution, heating to 45 ℃, stirring for 3h, and separating the solid phase and the liquid phase; collecting extractive solution, rotary steaming at 45 deg.C under-0.08 MPa, removing solvent methanol, oven drying at 48 deg.C under vacuum for 5 hr, and pulverizing to obtain 28.3kg natural antioxidant product.
Comparative example 1:
separating seed and skin of dry pepper, collecting pepper seeds, micronizing, and sieving with 100 mesh sieve to obtain dry pepper seed powder. Mixing 500kg of dry pepper seed powder with petroleum ether according to the mass ratio of 1:6, stirring at normal temperature for 1h, separating a solid phase from a liquid phase, collecting pepper seed powder solids, volatilizing the solvent, drying at 45 ℃ for 2h again, adding 500kg of methanol solution, heating to 40 ℃, stirring for 2h, and separating the solid phase from the liquid phase; collecting extractive solution, rotary steaming at 40 deg.C under-0.08 MPa, removing solvent methanol, oven drying at 45 deg.C under vacuum condition for 4 hr, and pulverizing to obtain 4.2kg of natural antioxidant product.
Comparing comparative example 1 with example 1, it was found that changing the ratio of the extraction solvent methanol to paprika below the optimum ratio range resulted in a substantial decrease in the yield of the final extracted natural antioxidant product.
Comparative example 2
Separating seed and skin of dry pepper, collecting pepper seeds, micronizing, and sieving with 100 mesh sieve to obtain dry pepper seed powder. Mixing 500kg of dry pepper seed powder with petroleum ether according to the mass ratio of 1:6, stirring at normal temperature for 1h, separating a solid phase from a liquid phase, collecting pepper seed powder solids, volatilizing the solvent, drying again at 45 ℃ for 2h, adding 3000kg of methanol solution, heating to 40 ℃, stirring for 2h, and separating the solid phase from the liquid phase; collecting extractive solution, rotary steaming at 40 deg.C under-0.08 MPa, removing solvent methanol, oven drying at 60 deg.C under vacuum condition for 4 hr, and pulverizing to obtain 13.2kg natural antioxidant.
Antioxidant Activity measurement experiment
The ethanol solution of the natural antioxidant prepared in the example 1 and the comparative example 2 is prepared, and the mass concentration of the natural antioxidant is 0.04%. 4ml of each of the two solutions was taken, 4.1ml of an ethanol solution of linoleic acid with a concentration of 2.51% was added, 8ml of 0.05mol/L phosphate buffer (pH7.0) was added, and the mixture was cultured in a water bath at 40 ℃ in a dark place for 1 to 7 days. The blank was not supplemented with any antioxidant, and the control was a 0.04% ethanol solution in Butylated Hydroxyanisole (BHA).
The antioxidant activity was measured daily: adding 9.7ml 75% ethanol and 0.1ml 30% ammonium thiocyanate into 0.1ml culture solution, adding 0.1ml 0.02mol/L FeCl2Standing the solution with 3.5% HCl solution for 3min, and measuring the light absorption value at 500nm wavelength. The measurement was continued for 7 days in the same manner, and the results are shown in Table 1.
TABLE 1 Absorbance values of different antioxidants
As can be seen from the experimental results in Table 1, the antioxidant activity of the natural antioxidant extracted from the pepper seeds in example 1 is equivalent to that of the commonly used antioxidant BHA, and is obviously superior to that of the blank group without any antioxidant, which indicates that the natural antioxidant can be used in food instead of toxic chemical antioxidant. Example 1 compared with comparative example 2, comparative example 2 has a weaker antioxidant activity than example 1 because the drying temperature of comparative example 2 during final purification of the product is too high, resulting in partial oxidation of the antioxidant, reducing the antioxidant activity.
Experiment of antioxidant Effect
The natural antioxidant product in example 2 is accurately weighed, added into 100g of lard according to the mass ratio of 0.2% to 0.5%, heated and stirred uniformly, meanwhile, a control group (100g of lard without any antioxidant) is set, the sample group and the control group are stored at 70 ℃, and the peroxide values of the sample group and the control group are measured periodically (12h/24h/48h/72h), and the results are shown in table 2.
TABLE 2 peroxide values (mmol/kg) in lard at different antioxidants and different times
| 12h | 24h | 48h | 72h | |
| Control group | 12.2 | 18.6 | 48.5 | 108.7 |
| Sample set (0.2%) | 10.8 | 15.4 | 17.6 | 27.5 |
| Sample set (0.5%) | 5.3 | 10.9 | 12.3 | 14.0 |
As can be seen from the experimental results in Table 2, the natural antioxidant extracted from the chilli seeds can effectively inhibit oxidation rancidity of lard, the inhibition effect is different in different addition amounts, and the inhibition effect is better when the addition amount is higher.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A method for preparing a natural antioxidant by utilizing chilli seeds is characterized by comprising the following steps:
(1) pretreatment: separating seed and skin of dry pepper, collecting pepper seeds, and micronizing to obtain dry pepper seed powder;
(2) degreasing: mixing dry pepper seed powder and a degreasing solvent in proportion, stirring at normal temperature, separating a solid phase and a liquid phase, collecting the solid phase pepper seed powder, volatilizing the solvent and drying again;
(3) extraction: adding methanol solution into the dried chilli seed powder, heating and stirring, and separating solid and liquid phases;
(4) and (3) purification: collecting the extract, performing rotary evaporation, removing the solvent methanol, drying under vacuum condition, and pulverizing to obtain natural antioxidant product.
2. The method for preparing a natural antioxidant by using chilli seeds as claimed in claim 1, wherein the degreasing solvent is any one of petroleum ether, n-hexane and ethyl acetate.
3. The method for preparing a natural antioxidant from pepper seeds as claimed in claim 1, wherein in the step (1), the dried pepper seed powder is obtained by passing through a 100-200 mesh screen after the micronization.
4. The method for preparing a natural antioxidant by using chilli seeds as claimed in claim 1, wherein in the step (2), the mass ratio of the dry chilli seed powder to the degreasing solvent is 1:5-1: 10.
5. The method for preparing a natural antioxidant by using chilli seeds as claimed in claim 1, wherein in the step (2), the stirring time is 1-3h, the drying temperature is 40-50 ℃, and the drying time is 2-4 h.
6. The method for preparing a natural antioxidant by using chilli seeds as claimed in claim 1, wherein in the step (3), the mass ratio of the chilli seed powder to the methanol solution is 1:5-1: 10.
7. The method for preparing a natural antioxidant by using pepper seeds as claimed in claim 1, wherein the heating temperature in step (3) is 40-50 ℃ and the stirring time is 2-4 h.
8. The method for preparing a natural antioxidant by using chilli seeds as claimed in claim 1, wherein in the step (4), the rotary steaming condition is 40-50 ℃ and less than-0.08 MPa.
9. The method for preparing a natural antioxidant by using chilli seeds as claimed in claim 1, wherein in the step (4), the drying temperature is 45-55 ℃ and the drying time is 3-5 h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111293645.5A CN114015504A (en) | 2021-11-03 | 2021-11-03 | Method for preparing natural antioxidant by utilizing chilli seeds |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111293645.5A CN114015504A (en) | 2021-11-03 | 2021-11-03 | Method for preparing natural antioxidant by utilizing chilli seeds |
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| CN202111293645.5A Pending CN114015504A (en) | 2021-11-03 | 2021-11-03 | Method for preparing natural antioxidant by utilizing chilli seeds |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114657018A (en) * | 2022-04-14 | 2022-06-24 | 遵义职业技术学院 | Deep processing method of chilli seeds |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087815A (en) * | 2013-03-01 | 2013-05-08 | 新疆西尔丹食品有限公司 | Chilli seed oil and preparation method thereof |
| CN109453253A (en) * | 2018-12-28 | 2019-03-12 | 四川大学 | A method of extracting flavonoid antioxidants from Zanthoxylum essential oil processing byproduct |
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2021
- 2021-11-03 CN CN202111293645.5A patent/CN114015504A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087815A (en) * | 2013-03-01 | 2013-05-08 | 新疆西尔丹食品有限公司 | Chilli seed oil and preparation method thereof |
| CN109453253A (en) * | 2018-12-28 | 2019-03-12 | 四川大学 | A method of extracting flavonoid antioxidants from Zanthoxylum essential oil processing byproduct |
Non-Patent Citations (4)
| Title |
|---|
| 丁筑红, 张汝练, 蒋航: "辣椒籽提取物对菜籽油的抗氧化作用", 食品科技, no. 09, pages 56 - 58 * |
| 丁筑红，等: "辣椒籽提取物对猪油抗氧化作用研究", 食品与发酵工业, vol. 30, no. 9, pages 41 - 43 * |
| 刘彩丽;卢基林;张玉军;张健希;王瑞霞;: "辣椒籽中抗氧化成分的提取及抗氧化性能的研究", 河南工业大学学报(自然科学版), vol. 28, no. 02, pages 15 - 18 * |
| 沈文娇，等: "辣椒籽对猪油抗氧化作用研究", 食品与机械, vol. 32, no. 12, pages 170 - 174 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114657018A (en) * | 2022-04-14 | 2022-06-24 | 遵义职业技术学院 | Deep processing method of chilli seeds |
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