Preparation method for reducing pungent smell of garlic oil

Abstract

The invention discloses a preparation method for reducing pungent smell of garlic oil, which comprises the following steps: 1) dissolving beta-cyclodextrin in ultrapure water according to the mass fraction of 10%, and stirring to obtain clear liquid; 2) adding absolute ethyl alcohol into the garlic oil to be emulsified, and stirring until the garlic oil is completely dispersed; (3) slowly dropwise adding the absolute ethyl alcohol / garlic oil solution into the beta-cyclodextrin solution according to the mass ratio of the garlic oil to the beta-cyclodextrin being (1: 6)-(1: 14), stirring for 10 minutes, and homogenizing for 1 hour at the reaction temperature of 45-75 DEG C and the rotating speed of 1000 revolutions per minute to complete inclusion of the garlic oil and the beta-cyclodextrin; 4) carrying out vacuum filtration on the reacted emulsion to obtain a wet microcapsule powder filter cake; and 5) carrying out vacuum drying on the wet micro-capsule powder filter cake for 2-4 hours to obtain the garlic oil micro-capsule powder. The invention has the advantages of simple preparation method, low cost, excellent effect and the like, and is suitable for the fields of food, feed, health care products and the like.

Description

Technical Field

[0001] The invention relates to the field of food and feed additive preparation, and in particular to a preparation method for reducing the pungent smell of garlic oil. Background Art

[0002] Garlic oil is a natural vegetable oil extracted from garlic, rich in biologically active sulfides (such as allicin, alliin, etc.), which give garlic oil significant pharmacological functions and broad application prospects. Garlic oil plays an important role in many fields such as aquaculture, food, health products and agriculture.

[0003] Garlic oil is commonly used in seasoning, cooking, health foods and functional beverages. Its antioxidant, antibacterial and antiviral effects make it widely used in extending the shelf life of food and improving food hygiene. In addition, garlic oil is widely used in the preparation of health products, especially in products that enhance immunity, blood circulation, reduce lipids and blood pressure. Since garlic oil has the function of regulating blood lipids and blood pressure, it is widely used in the prevention and adjuvant treatment of cardiovascular diseases.

[0004] Garlic oil can also be used as a natural pesticide and plant protection agent, mainly used to resist plant diseases and insects. Its natural antibacterial, insect repellent, antioxidant and mildew-proof effects make it a promising environmentally friendly pesticide.

[0005] In the aquaculture industry, garlic oil has powerful antibacterial, antiviral and antifungal effects, which can help improve the immunity of animals and prevent and treat various bacterial and viral infections. Studies have shown that allicin in garlic oil can inhibit the growth of pathogenic bacteria such as Escherichia coli, Salmonella, and Streptococcus, so it can effectively reduce the use of antibiotics and reduce the production of drug-resistant strains in the aquaculture process. Garlic oil is often used as a natural antibacterial agent and immunopotentiator, added to animal feed to improve the immunity and growth performance of animals. However, the strong smell of garlic oil makes the feed less palatable, and livestock and poultry refuse to eat it, affecting its actual effect. In addition, garlic oil is easily oxidized when exposed to air and high temperature conditions, losing its active ingredients, further limiting its application in the aquaculture industry. Summary of the invention

[0006] In view of the problems and defects existing in the above-mentioned prior art, the object of the present invention is to provide a preparation method for reducing the pungent smell of garlic oil. The method uses β-cyclodextrin to microencapsulate the garlic oil. Microencapsulation can not only effectively reduce the odor release and improve the stability of garlic oil, but also prolong its shelf life in feed or food.

[0007] The technical solution adopted to achieve the above purpose is: a preparation method based on β-cyclodextrin embedded garlic oil, comprising the following steps:

[0008] 1) Dissolve β-cyclodextrin in ultrapure water at a mass fraction of 10% and stir until the liquid becomes clear;

[0009] 2) adding anhydrous ethanol to the garlic oil to be emulsified to improve dispersibility, and stirring until the garlic oil is completely dispersed;

[0010] 3) Slowly add the dispersed anhydrous ethanol / garlic oil solution dropwise into the β-cyclodextrin solution at a mass ratio of 1:6 to 1:14 of garlic oil to β-cyclodextrin, stir for 10 min, and homogenize at a reaction temperature of 45 to 75 ° C and a speed of 1000 rpm for 1 hour to complete the inclusion of garlic oil and β-cyclodextrin;

[0011] 4) Pour the emulsion after the reaction into a suction filtration device, and use a vacuum pump to remove excess water to obtain a moist microcapsule powder filter cake;

[0012] 5) Spread the wet microcapsule powder filter cake on a drying tray and continue drying in a vacuum drying oven for 2 to 4 hours until the product is completely dry to obtain garlic oil microcapsule powder.

[0013] Furthermore, in step 1, the stirring speed is 800 rpm and the temperature is 50°C.

[0014] Furthermore, in step 2, the mass ratio of anhydrous ethanol to garlic oil is 10:1.

[0015] Furthermore, in step 5, the drying temperature of the vacuum drying oven is 50-60°C.

[0016] The invention has the advantages that, through the embedding effect of beta-cyclodextrin, the volatile sulfide of garlic oil can be effectively enclosed in the capsule wall, which greatly reduces the pungent smell of garlic oil and solves the problem of the acceptance of traditional garlic oil due to the heavy smell. In addition, the microencapsulated garlic oil is more stable during storage and transportation. DETAILED DESCRIPTION

[0017] The following is a further description of the technical solution of the present invention in combination with the embodiments of the present invention. Obviously, based on the embodiments of the present invention, the embodiments modified in different ways by other persons in the art without creative work should be regarded as the protection scope of the present invention.

[0018] Example 1

[0019] A preparation method based on β-cyclodextrin embedded garlic oil comprises the following steps:

[0020] 1) Preparation of β-cyclodextrin solution: dissolve β-cyclodextrin in ultrapure water at a mass fraction of 10%, and stir continuously at a stirring speed of 800 rpm and a temperature of 50° C. until a clear liquid is obtained;

[0021] 2) Garlic oil emulsification: add anhydrous ethanol to garlic oil in a mass ratio of 10:1 to the garlic oil to be emulsified to improve the dispersibility, and stir until the garlic oil is completely dispersed;

[0022] 3) Inclusion reaction: Slowly add the dispersed anhydrous ethanol / garlic oil solution to the stirring β-cyclodextrin solution at a mass ratio of 1:6 between garlic oil and β-cyclodextrin, and stir for 10 minutes. The reaction temperature is 45°C, and the speed is 1000 rpm for 1 hour to complete the inclusion of garlic oil and β-cyclodextrin.

[0023] 4) Vacuum filtration: Pour the emulsion after the reaction into the filtration device, and use a vacuum pump to filter and remove excess water to obtain a moist microcapsule powder filter cake.

[0024] 5) Formation of garlic oil microcapsule powder: Spread the wet microcapsule powder filter cake on a drying tray and continue drying in a vacuum drying oven for 2 hours until the product is completely dry to obtain garlic oil microcapsule powder.

[0025] Example 2

[0026] A preparation method based on β-cyclodextrin embedded garlic oil comprises the following steps:

[0027] 1) Preparation of β-cyclodextrin solution: Dissolve β-cyclodextrin in ultrapure water at a mass fraction of 10%, and continue stirring at a stirring speed of 800 rpm and a temperature of 50° C. until a clear liquid is obtained;

[0028] 2) Garlic oil emulsification: add anhydrous ethanol to garlic oil in a mass ratio of 10:1 to the garlic oil to be emulsified to improve the dispersibility, and stir until the garlic oil is completely dispersed;

[0029] 3) Inclusion reaction: Slowly add the dispersed anhydrous ethanol / garlic oil solution to the stirring β-cyclodextrin solution at a mass ratio of 6 to 14 of garlic oil to β-cyclodextrin, and stir for 10 minutes. The reaction temperature is 55°C, and the speed is 1000 rpm for 1 hour to complete the inclusion of garlic oil and β-cyclodextrin.

[0030] 4) Vacuum filtration: Pour the emulsion after the reaction into the filtration device, and use a vacuum pump to filter and remove excess water to obtain a moist microcapsule powder filter cake.

[0031] 5) Formation of garlic oil microcapsule powder: Spread the wet microcapsule powder filter cake on a drying tray and continue drying in a vacuum drying oven for 3 hours until the product is completely dry to obtain garlic oil microcapsule powder.

[0032] Example 3

[0033] A preparation method based on β-cyclodextrin embedded garlic oil comprises the following steps:

[0034] 1) Preparation of β-cyclodextrin solution: Dissolve β-cyclodextrin in ultrapure water at a mass fraction of 10%, and continue stirring at a stirring speed of 800 rpm and a temperature of 50° C. until a clear liquid is obtained;

[0035] 2) Garlic oil emulsification: add anhydrous ethanol to garlic oil in a mass ratio of 10:1 to the garlic oil to be emulsified to improve the dispersibility, and stir until the garlic oil is completely dispersed;

[0036] 3) Inclusion reaction: Slowly add the dispersed anhydrous ethanol / garlic oil solution to the stirring β-cyclodextrin solution at a mass ratio of 3:7 of garlic oil to β-cyclodextrin, and stir for 10 minutes. The reaction temperature is 75°C, and the speed is 1000 rpm for 1 hour to complete the inclusion of garlic oil and β-cyclodextrin.

[0037] 4) Vacuum filtration: Pour the emulsion after the reaction into the filtration device, and use a vacuum pump to filter and remove excess water to obtain a moist microcapsule powder filter cake.

[0038] 5) Formation of garlic oil microcapsule powder: Spread the wet microcapsule powder filter cake on a drying tray and continue drying in a vacuum drying oven for 4 hours until the product is completely dry to obtain garlic oil microcapsule powder.

[0039] Test Example 1

[0040] Effects of different ratios of garlic oil and β-cyclodextrin on encapsulation efficiency and odor

[0041] Preparation of β-cyclodextrin solution: Dissolve 6 g, 8 g, 10 g, 12 g, and 14 g of β-cyclodextrin in 100 ml of ultrapure water at 50°C, and stir with a magnetic stirrer at 800 rpm until completely dissolved. Use a pH meter to check the pH value of the solution and adjust it to neutral (pH 6-7). Filter the solution using a 0.45 μL filter membrane to ensure that the solution is clear.

[0042] Garlic oil emulsification: Weigh 1 gram of garlic oil, slowly add 10 ml of anhydrous ethanol to the garlic oil, and gently stir with a glass rod for about 5 to 10 minutes until the garlic oil is completely dispersed in the anhydrous ethanol to form a uniform solution, ensuring that the garlic oil is evenly dispersed in the ethanol.

[0043] Inclusion reaction: Slowly add the dispersed anhydrous ethanol / garlic oil solution to the stirring β-cyclodextrin solution according to the mass ratio of garlic oil to β-cyclodextrin of 1:6, 1:8, 1:10, 1:12, and 1:14, and stir for 10 minutes. The reaction temperature is 55°C and the speed is 1000 rpm for 1 hour to complete the inclusion of garlic oil and β-cyclodextrin.

[0044] Vacuum filtration: Pour the emulsion after the reaction into the filtration device, and use the vacuum pump to filter and remove excess water to obtain a moist microcapsule powder filter cake.

[0045] Formation of garlic oil microcapsule powder: Spread the wet microcapsule powder filter cake on a drying tray and continue drying in a vacuum drying oven for 2 to 4 hours until the product is completely dry to obtain garlic oil microcapsule powder.

[0046] Determination of garlic oil embedding rate: Take anhydrous ethanol as blank, measure absorbance at the maximum absorption wavelength of garlic oil at 280 nanometers, and draw a standard curve of garlic oil. Weigh 2 portions of 1 gram of garlic oil microcapsule powder, add 10 ml of anhydrous ethanol respectively, ultrasonicate at 900W for 1 minute and 30 minutes respectively at room temperature, centrifuge at 8000 rpm for 10 minutes, take the supernatant, measure absorbance at 280 nanometers, and obtain the mass m1 and m2 of garlic oil in the supernatant. The calculation formula of garlic oil embedding rate is A=(m2-m1) / m0*100%. Where: A=garlic oil embedding rate, %; m0=amount of garlic oil input, g; m1=amount of garlic oil on the surface of microcapsule powder, g; m2=amount of garlic oil in microcapsule powder, g.

[0047] Table 1 Effect of different ratios of garlic oil and β-cyclodextrin on encapsulation efficiency and odor

[0048]

[0049] Result analysis:

[0050] Table 1 shows that the ratio of 1:10 showed the best embedding effect, with an embedding rate of 66.9%, and the pungent smell of garlic oil was slight. When the ratio of β-cyclodextrin was further increased, the embedding rate decreased, suggesting that there may be an excess of β-cyclodextrin that failed to effectively encapsulate the garlic oil. Therefore, 1:10 is the best ratio in this experiment.

[0051] Experimental Example 2 Effect of different inclusion reaction temperatures on encapsulation efficiency and odor

[0052] Preparation of β-cyclodextrin solution: Dissolve 10 g of β-cyclodextrin in 100 ml of ultrapure water at 50°C and stir with a magnetic stirrer at 800 rpm until completely dissolved. Use a pH meter to check the pH of the solution and adjust it to neutral (pH 6-7). Filter the solution using a 0.45 μL filter membrane to ensure that the solution is clear.

[0053] Garlic oil emulsification: Weigh 1 gram of garlic oil, slowly add 10 ml of anhydrous ethanol to the garlic oil, and gently stir with a glass rod for about 5 to 10 minutes until the garlic oil is completely dispersed in the anhydrous ethanol to form a uniform solution, ensuring that the garlic oil is evenly dispersed in the ethanol.

[0054] Inclusion reaction: Slowly add the dispersed anhydrous ethanol / garlic oil solution to the stirring β-cyclodextrin solution at a mass ratio of 1:10 between garlic oil and β-cyclodextrin, and stir for 10 minutes. The reaction temperatures are 35°C, 45°C, 55°C, 65°C, and 75°C, and the speed is 1000 rpm for 1 hour to complete the inclusion of garlic oil and β-cyclodextrin.

[0055] Vacuum filtration: Pour the emulsion after the reaction into the filtration device, and use the vacuum pump to filter and remove excess water to obtain a moist microcapsule powder filter cake.

[0056] Formation of garlic oil microcapsule powder: Spread the wet microcapsule powder filter cake on a drying tray and continue drying in a vacuum drying oven for 2 to 4 hours until the product is completely dry to obtain garlic oil microcapsule powder.

[0057] Determination of garlic oil embedding rate: Take anhydrous ethanol as blank, measure absorbance at the maximum absorption wavelength of garlic oil at 280 nanometers, and draw a standard curve of garlic oil. Weigh 2 portions of 1 gram of garlic oil microcapsule powder, add 10 ml of anhydrous ethanol respectively, ultrasonicate at 900W for 1 minute and 30 minutes respectively at room temperature, centrifuge at 8000 rpm for 10 minutes, take the supernatant, measure absorbance at 280 nanometers, and obtain the mass m1 and m2 of garlic oil in the supernatant. The calculation formula of garlic oil embedding rate is A=(m2-m1) / m0*100%. Where: A=garlic oil embedding rate, %; m0=amount of garlic oil input, g; m1=amount of garlic oil on the surface of microcapsule powder, g; m2=amount of garlic oil in microcapsule powder, g.

[0058] Table 2 Effect of different inclusion reaction temperatures on garlic oil encapsulation rate and odor

[0059]

[0060] Result analysis:

[0061] Too low a temperature will result in insufficient activity of β-cyclodextrin molecules, leading to a low encapsulation rate. Too high a temperature may cause the loss of volatile substances in garlic oil. Therefore, 45°C is the optimal reaction temperature. At this temperature, the garlic oil has a high encapsulation rate and an ideal odor control effect.

[0062] The results show that the content of garlic oil in the prepared garlic oil microcapsule powder is 73.8%.

[0063] In summary, through the study of the garlic oil microcapsule powder inclusion process of the present invention, it is found that when the reaction temperature is 45°C and the ratio of garlic oil to β-cyclodextrin is 1:10, the embedding rate can be significantly improved to achieve the best effect, and the masking effect of the pungent smell of garlic oil is the best. The process is simple to operate, low in cost, and can effectively reduce the pungent smell of garlic oil.

Claims

1. A preparation method for reducing the pungent smell of garlic oil, characterized in that: The following steps are involved: 1) Dissolve β-cyclodextrin in ultrapure water at a mass fraction of 10% and stir until the liquid becomes clear; 2) adding anhydrous ethanol to the garlic oil to be emulsified to improve dispersibility, and stirring until the garlic oil is completely dispersed; 3) Slowly add the dispersed anhydrous ethanol / garlic oil solution dropwise into the β-cyclodextrin solution at a mass ratio of 1:6 to 1:14 of garlic oil to β-cyclodextrin, stir for 10 min, and homogenize at a reaction temperature of 45 to 75 ° C and a speed of 1000 rpm for 1 hour to complete the inclusion of garlic oil and β-cyclodextrin; 4) Pour the emulsion after the reaction into a suction filtration device, and use a vacuum pump to remove excess water to obtain a moist microcapsule powder filter cake; 5) Spread the wet microcapsule powder filter cake on a drying tray and continue drying in a vacuum drying oven for 2 to 4 hours until the product is completely dry to obtain garlic oil microcapsule powder.

2. The method for reducing the pungent smell of garlic oil according to claim 1, characterized in that: The stirring speed described in step 1 is 800 rpm and the temperature is 50°C.

3. The preparation method for reducing the pungent smell of garlic oil according to claim 1, characterized in that: The mass ratio of anhydrous ethanol to garlic oil added in step 2 is 10:

1.

4. The method for reducing the pungent smell of garlic oil according to claim 1, characterized in that In step 5, the drying temperature of the vacuum drying oven is 50-70°C.

Images