Pickering emulsion with clove oil embedded in amphiphilic thermal gel and preparation method of Pickering emulsion

Abstract

The invention discloses a Pickering emulsion with clove oil embedded in amphiphilic thermal gel and a preparation method of the Pickering emulsion, and belongs to the technical field of polymer modification. The preparation method comprises the following steps: performing carboxymethylation on thermal gel, and grafting octadecylamine to obtain the amphiphilic thermal gel. And dissolving the amphiphilic thermal gel in an aqueous solution, adding clove oil, and carrying out homogenization treatment to obtain the clove oil-loaded Pickering emulsion. The clove oil emulsion prepared by the method is in a stable O / W type, and has stronger antibacterial property compared with unembedded clove oil. The clove oil emulsion solves the problem that clove oil is easy to volatilize and oxidize, the oxidation resistance and antibacterial activity of the clove oil emulsion are improved, no emulsifier is contained in the preparation process, the prepared clove oil emulsion is high in stability, a safe and long-acting antibacterial agent is provided for the fields of food and medicines, and the clove oil emulsion has a good application prospect.

Description

technical field

[0001] The invention relates to an amphiphilic thermogel-embedded Pickering emulsion of clove oil and a preparation method thereof, in particular to an octadecylamine-modified carboxymethylated thermogel-embedded Pickering emulsion of clove oil and a preparation method thereof , belongs to the technical field of polymer material modification. Background technique

[0002] Clove oil (CEO) mainly contains phenylpropanoid compounds such as eugenol and its derivatives. Due to its biological properties, including antioxidant, antibacterial, insecticidal, analgesic and anticancer activities, it is widely used in food, hygiene, biomedicine, pharmaceutical, Widely used in packaging and cosmetic industries. However, clove oil is prone to oxidation, is greatly affected by temperature, and is stable and volatile, which limits its application. At present, Tween is mainly used as the emulsifier in the emulsion system. Pickering emulsions that use solid particles instead...

Examples

Embodiment 1

[0053] (1) Carboxymethylation of thermal gel: 3 g of thermal gel (Mw=2.48×10 6 Da) was dissolved in 100 mL of isopropanol solution, stirred at room temperature for 30 min, added 7 mL of 30% sodium hydroxide dropwise, continued to stir for 90 min, slowly added 8 g of chloroacetic acid, stirred at 50 ° C for 8 h, there was solid precipitation, and the solid product was separated and collected ; Wash the product with methanol-acetic acid (7:3) mixture, 80% methanol mixture, methanol and acetone, redissolve the product in 200 mL of deionized water, and dialyze the product in deionized water for 3 days with an 8000-14000Da dialysis bag, After vacuum freeze-drying, carboxymethylated thermogel (CMCD, Mw=3.125486×10 6 ).

[0054] The degree of substitution of carboxymethyl group was determined by acid-base titration, and the degree of substitution of carboxymethyl group was 0.95.

[0055] (2) Amidation of carboxymethylated thermal gel: Weigh 1 g of CMCD and dissolve it in 200 mL of ...

Embodiment 2

[0062] (1) Carboxymethylation of thermal gel: 3 g of thermal gel (Mw=2.48×10 6 Da) was dissolved in 150 mL of isopropanol solution, stirred at room temperature for 40 min, added dropwise 10 mL of 50% sodium hydroxide, continued to stir for 90 min, slowly added 3 g of chloroacetic acid, stirred at 50 ° C for 9 h, there was solid precipitation, and the solid product was separated and collected ; The product was washed with methanol-acetic acid mixture (7:3), 80% methanol mixture, methanol, and acetone, redissolved in 200 mL of deionized water, and dialyzed in deionized water with 8000-14000Da dialysis bag for 3 days , carboxymethylated thermogel (CMCD) was obtained after vacuum freeze-drying.

[0063] The degree of carboxymethyl substitution was determined by acid-base titration, and the degree of carboxymethyl substitution was determined to be 0.6.

[0064] (2) Amidation of carboxymethylated thermal gel: Weigh 1 g of CMCD and dissolve it in 200 ml of deionized water, stir magn...

Embodiment 3

[0069] With reference to Example 1, only the addition of clove oil in step (4) is replaced by 3mL (corresponding to the consumption ratio of CMCD-ODA1 and clove oil 1gCMCD-ODA1:40mL clove oil becomes 1gCMCD-ODA1:60mL clove oil) ); otherwise unchanged, the corresponding emulsion was obtained.

[0070] It was found that the carrier concentration of the obtained clove oil emulsion system was too low, the oil-water stratification phenomenon occurred in the emulsion system, and the system stability was low. In Example 1, the emulsion system with 2 mL of clove oil added has good uniformity and stability.

technical field

[0001] The invention relates to an amphiphilic thermogel-embedded Pickering emulsion of clove oil and a preparation method thereof, in particular to an octadecylamine-modified carboxymethylated thermogel-embedded Pickering emulsion of clove oil and a preparation method thereof , belongs to the technical field of polymer material modification. Background technique

[0002] Clove oil (CEO) mainly contains phenylpropanoid compounds such as eugenol and its derivatives. Due to its biological properties, including antioxidant, antibacterial, insecticidal, analgesic and anticancer activities, it is widely used in food, hygiene, biomedicine, pharmaceutical, Widely used in packaging and cosmetic industries. However, clove oil is prone to oxidation, is greatly affected by temperature, and is stable and volatile, which limits its application. At present, Tween is mainly used as the emulsifier in the emulsion system. Pickering emulsions that use solid particles instead...

Examples

Embodiment 1

[0053] (1) Carboxymethylation of thermal gel: 3 g of thermal gel (Mw=2.48×10 6 Da) was dissolved in 100 mL of isopropanol solution, stirred at room temperature for 30 min, added 7 mL of 30% sodium hydroxide dropwise, continued to stir for 90 min, slowly added 8 g of chloroacetic acid, stirred at 50 ° C for 8 h, there was solid precipitation, and the solid product was separated and collected ; Wash the product with methanol-acetic acid (7:3) mixture, 80% methanol mixture, methanol and acetone, redissolve the product in 200 mL of deionized water, and dialyze the product in deionized water for 3 days with an 8000-14000Da dialysis bag, After vacuum freeze-drying, carboxymethylated thermogel (CMCD, Mw=3.125486×10 6 ).

[0054] The degree of substitution of carboxymethyl group was determined by acid-base titration, and the degree of substitution of carboxymethyl group was 0.95.

[0055] (2) Amidation of carboxymethylated thermal gel: Weigh 1 g of CMCD and dissolve it in 200 mL of ...

Embodiment 2

[0062] (1) Carboxymethylation of thermal gel: 3 g of thermal gel (Mw=2.48×10 6 Da) was dissolved in 150 mL of isopropanol solution, stirred at room temperature for 40 min, added dropwise 10 mL of 50% sodium hydroxide, continued to stir for 90 min, slowly added 3 g of chloroacetic acid, stirred at 50 ° C for 9 h, there was solid precipitation, and the solid product was separated and collected ; The product was washed with methanol-acetic acid mixture (7:3), 80% methanol mixture, methanol, and acetone, redissolved in 200 mL of deionized water, and dialyzed in deionized water with 8000-14000Da dialysis bag for 3 days , carboxymethylated thermogel (CMCD) was obtained after vacuum freeze-drying.

[0063] The degree of carboxymethyl substitution was determined by acid-base titration, and the degree of carboxymethyl substitution was determined to be 0.6.

[0064] (2) Amidation of carboxymethylated thermal gel: Weigh 1 g of CMCD and dissolve it in 200 ml of deionized water, stir magn...

Embodiment 3

[0069] With reference to Example 1, only the addition of clove oil in step (4) is replaced by 3mL (corresponding to the consumption ratio of CMCD-ODA1 and clove oil 1gCMCD-ODA1:40mL clove oil becomes 1gCMCD-ODA1:60mL clove oil) ); otherwise unchanged, the corresponding emulsion was obtained.

[0070] It was found that the carrier concentration of the obtained clove oil emulsion system was too low, the oil-water stratification phenomenon occurred in the emulsion system, and the system stability was low. In Example 1, the emulsion system with 2 mL of clove oil added has good uniformity and stability.

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