Method for verifying regeneration effect between antioxidants through establishing a separable regeneration system

Patent metadata

Field	Value
Publication number	US-11119087-B2
Application number	US-201916460635-A
Country	US
Kind code	B2
Filing date	Jul 2, 2019
Priority date	May 16, 2019
Publication date	Sep 14, 2021
Grant date	Sep 14, 2021

Abstract

The invention provides a method for establishing a separable regeneration system for verifying regeneration effect between two antioxidants, which belongs to the field of regeneration effect of antioxidants. According to different solubilities of two antioxidants, lipid-soluble antioxidant is first combined into PE film, and water-soluble antioxidant is dissolved into deionized water and a separable regeneration system where antioxidants can contact with other but not dissolve in each other is formed. This method compares the differences of change of antioxidant capacity in aqueous phase with and without lipid-soluble antioxidant so that to judge whether the added lipid-soluble antioxidant has regeneration effect on aqueous-soluble antioxidant. The present invention effectively verifies the regeneration effect between different antioxidants, and has advantages of simple operation, less interference factors, intuitive and high efficiency.

First claim

The invention claimed is:

1. A method for verifying regeneration effect between antioxidants through establishing a separable regeneration system comprising the steps:
(1) preparing an aqueous phase of separable regeneration system: completely dissolving water-soluble antioxidant into deionized water, and then obtaining aqueous solution of water-soluble antioxidant, that is aqueous phase of separable regeneration system;
(2) preparing a separable thermoplastic resin film with lipid-soluble antioxidant
(2.1) preparing thermoplastic resin film: thermoplastic resin masterbatch without antioxidant is first hot-melt extruded into a thermoplastic resin film with thickness of 1.5-3.0 mm using an open type rubber mixer; the 1.5-3.0 mm thermoplastic resin film is placed on a resistant polyimide film, and is pressed by a flat vulcanizer into one thermoplastic resin film with thickness of 0.10-0.20 mm;
(2.2) preparing thermoplastic resin film with lipid-soluble antioxidant: cutting a prepared 0.10-0.20 mm thermoplastic resin film in step (2.1) into two pieces; placing lipid-soluble antioxidant between the two pieces of thermoplastic resin films, and combining the lipid-soluble antioxidant with the two pieces of thermoplastic resin films, thus obtaining a whole piece of thermoplastic resin film; cutting the whole piece of thermoplastic resin film into two pieces and hot-pressing them into a whole piece of film; repeating the cutting and hot-pressing procedure for 3-5 times;
(2.3) storage and reserve: washing the prepared thermoplastic resin film with lipid-soluble antioxidant prepared in step (2.2) with water; drying the thermoplastic resin film with lipid-soluble antioxidant in an oven at 25° C. for 24 h; sealing and storing the films in a refrigerator at 4° C. before use;
(3) verification of regeneration effect between antioxidants in the separable regeneration system
(3.1) setup of regeneration group: transferring the thermoplastic resin film with lipid-soluble antioxidant prepared in step (2.3) into the aqueous phase of separable regeneration system prepared in step (1) as regeneration group, a surface area of the thermoplastic resin film with lipid-soluble antioxidant is recorded as S, a weight of the thermoplastic resin film with lipid-soluble antioxidant is recorded as m;
(3.2) setup of control group: transferring the thermoplastic resin film without lipid-soluble antioxidant from step (2.1) with surface area S and weight m into the aqueous phase of separable regeneration system prepared in step (1) as control group;
(3.3) verification of regeneration effect: sealing reactors of regeneration group and control group; measuring antioxidant capacity of aqueous phase in both groups after same reaction duration through scavenging hydroxyl radical method; when antioxidant capacity of regeneration group is significantly higher than that of control group, it is proved that the added lipid-soluble antioxidant is capable of regenerating the antioxidant in aqueous phase; otherwise, it is proved that the antioxidant in aqueous phase is capable of regenerating the lipid-soluble antioxidant in the thermoplastic resin film; wherein the regeneration effect does not exist between the antioxidant in the aqueous phase and the lipid-soluble antioxidant when no difference in antioxidant capacity is observed between the regeneration group and the control group.

2. The method according to claim 1 , wherein in the preparing thermoplastic resin film in the step (2.1), parameters of open type rubber mixer is set as follows: operation temperature of a front drum is 150-175° C. and that of a rear drum is 150-175° C.; drum space is 1.5-3.0 mm; parameters of flat vulcanizer is set as follows: operation temperature of upper and lower plats is 145-160° C.; and operation pressure is 1000-1400 Pa.

3. The method according to claim 1 , wherein reaction temperature after sealing the reactors in step (3.3) is ranging from 10-30° C.

4. The method according to claim 3 , wherein the scavenging hydroxyl radical method in the step (3.3) further comprises the sub-steps as follows: adding 1 mL of antioxidant aqueous-solution into 0.5 mL of salicylic acid solution at 12 mmol/L, 0.5 mL of FeSO 4 aqueous solution at 0.9 mol/L, 0.5 mL of H 2 O 2 aqueous solution at 9 mmol/L and reacting at 37° C. for 1 h in water bath and there exist sediments in a lower layer; taking 1 mL of upper solution and diluting it to 4 mL; measuring an absorbance value of the diluted upper solution at 510 nm.

5. The method according to claim 3 , wherein the thermoplastic resin film is made by either polyethylene or polyvinyl chloride.

6. The method according to claim 1 , wherein the scavenging hydroxyl radical method in the step (3.3) further comprises the sub-steps as follows: adding 1 mL of antioxidant aqueous-solution into 0.5 mL of salicylic acid solution at 12 mmol/L, 0.5 mL of FeSO 4 aqueous solution at 0.9 mol/L, 0.5 mL of H 2 O 2 aqueous solution at 9 mmol/L and reacting at 37° C. for 1 h in water bath and there exist sediments in a lower layer; taking 1 mL of upper solution and diluting it to 4 mL; measuring an absorbance value of the diluted upper solution at 510 nm.

7. The method according to claim 6 , wherein the thermoplastic resin film is made by either polyethylene or polyvinyl chloride.

8. The method according to claim 1 wherein the thermoplastic resin film is made by either polyethylene or polyvinyl chloride.

9. The method according to claim 8 , wherein the method of combining the lipid-soluble antioxidant with the two pieces of the thermoplastic resin films in step (2.2) includes hot pressing, mixing, and extruding processes.

10. The method according to claim 1 , wherein the method of combining the lipid-soluble antioxidant with the two pieces of the thermoplastic resin films in step (2.2) includes hot pressing, mixing, and extruding processes.

Assignees

• Univ Jiangnan

Inventors

• Yu Hang
• He yaxin
• Xie Yunfei
• Guo Yahui
• Cheng Yuliang
• Yao Weirong

Classifications

• G01N31/16

  using titration · CPC title

• A23V2002/00

  Food compositions, function of food ingredients or processes for food or foodstuffs · CPC title

• A23G1/545

  Hollow products, e.g. with inedible or edible filling, fixed or movable within the cavity · CPC title

• A23G1/426

  containing vitamins or antibiotics · CPC title

• G01N33/02 Primary

  Food · CPC title