CN111359553B - Preparation method of biodegradable edible pigment microcapsule - Google Patents
Preparation method of biodegradable edible pigment microcapsule Download PDFInfo
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- CN111359553B CN111359553B CN202010168767.0A CN202010168767A CN111359553B CN 111359553 B CN111359553 B CN 111359553B CN 202010168767 A CN202010168767 A CN 202010168767A CN 111359553 B CN111359553 B CN 111359553B
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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Abstract
A preparation method of a biodegradable food pigment microcapsule comprises the following steps: putting polylactic acid and dichloromethane into a reaction container, stirring, putting into a water bath, heating, and adding polyvinylpyrrolidone and triton X-100 to obtain an oil phase system; mixing methacryloyloxyethyl trimethyl ammonium chloride, deionized water, potassium persulfate and sodium bisulfite, introducing argon, adding carmine, mixing uniformly, putting into a reactor, and stirring uniformly to obtain a W/O internal water phase system; mixing and stirring uniformly polyvinyl alcohol, Tween-80 and deionized water to obtain an external water phase system; adding the W/O internal aqueous phase system into the external aqueous phase system, continuously stirring at the rotating speed of 450r/min until the system is stable, then cooling to room temperature, filtering to obtain spheres, leaching the spheres with hot water, and drying in vacuum to obtain the colored polymer microspheres, namely the biodegradable food pigment microcapsules. The microcapsules prepared by the invention aim to reduce the toxicity of azo pigments.
Description
Technical Field
The invention relates to a preparation method of a biodegradable food pigment microcapsule.
Background
Azo edible pigments have simple structure, bright color, low price and excellent performance, and are widely applied to the fields of food, medicine, cosmetics and the like. However, researches show that some azo pigments can be decomposed in human bodies to form a plurality of aromatic amines, and the aromatic amines can directly act with human cells through in-vivo metabolic activities, possibly cause cell canceration and harm the health of human bodies. Therefore, in order to reduce the physiological toxicity of azo edible pigments, the stable pigment microcapsule particles can be prepared by using the polymer material as the wall material, and the toxicity of the azo pigments is reduced by fully utilizing the physiological safety and stability of the polymer of the microcapsule wall material and the characteristic of non-absorption by the digestive system of an animal.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a biodegradable food pigment microcapsule, and the microcapsule prepared by the method aims at reducing the toxicity of azo pigment and improving the safety of the food pigment.
In order to solve the technical problem, the invention provides a preparation method of a biodegradable food pigment microcapsule, which comprises the following steps:
(1) weighing 0.8-1.5g of polylactic acid and 50mL of dichloromethane, mixing, putting into a reaction vessel, starting stirring, putting the reaction vessel into a water bath, heating to 50 ℃, and then adding 2g of polyvinylpyrrolidone and 0.75g of triton X-100 to obtain an oil phase system;
(2) weighing 4-10mL of methacryloyloxyethyl trimethyl ammonium chloride, 7-12.5mL of deionized water, 0.03-0.075g of potassium persulfate and 0.06-0.15g of sodium bisulfite, mixing, introducing argon for 30min, heating to 30 ℃, keeping the temperature for 5h, adding 0.25-0.1g of carmine, uniformly mixing, and putting into the reactor in the step (1); finally, stirring uniformly at the rotating speed of 400r/min to enable the water phase to form uniform liquid drops to be dispersed in the oil phase system, and obtaining a W/O internal water phase system;
(3) weighing 2.5-7.5g of polyvinyl alcohol, 1.25-1.32 g of Tween-800.5 and 300mL of deionized water, and uniformly stirring at a rotating speed of 400r/min to obtain an external water phase system; adding the W/O internal aqueous phase system obtained in the step (2) into an external aqueous phase system to obtain a W/O/W reversed-phase suspension polymerization system;
(4) continuously stirring the W/O/W reversed phase suspension polymer system at the rotating speed of 450r/min until the system is stable, keeping the temperature of the system at 25-40 ℃, keeping the temperature for 1h, heating to 50 ℃, keeping the temperature for 5h, cooling to room temperature, filtering to obtain spheres, leaching the spheres with water at 85 ℃, and drying in vacuum to obtain the colored polymer microspheres, namely the biodegradable food pigment microcapsules.
Polylactic acid attracts a great deal of researchers' attention as a controllable biodegradable polymer material because it has the following advantages: 1) the food dye has good biocompatibility and has no mutual influence with food dye molecules; 2) the biodegradable film has complete biodegradability in various environments, and the degradation rate is adjustable; 3) the polylactic acid is composed of lactic acid, has no toxicity and immunogenicity, and water and carbon dioxide formed after biodegradation can not generate toxicity to human bodies; 4) the polylactic acid is a renewable resource, has wide material source, and is cheap and good. The polylactic acid is used as a carrier of the edible pigment, so that not only is the direct contact between edible pigment molecules and human organs avoided, but also the stability of the edible pigment in the body is improved, and the pollution of the pigment to the environment is reduced.
The invention has the advantages that: the microcapsule prepared by the invention aims at reducing the toxicity of azo pigments, and the biodegradable polylactic acid material is selected as the wall material to prepare the pigment microcapsule with biodegradability, so that the possibility of the pigments contacting human organs can be reduced or avoided, the reduction and degradation of azo pigments in organ tissues and intestinal tracts can be reduced or even completely avoided, and the safety of the edible pigments is greatly improved.
Detailed Description
The first embodiment is as follows:
a preparation method of biodegradable food pigment microcapsules comprises the following steps:
(1) weighing 1g of polylactic acid and 50mL of dichloromethane, mixing, putting into a reaction vessel, starting stirring, then putting the reaction vessel into a water bath, heating to 50 ℃, and then adding 2g of polyvinylpyrrolidone and 0.75g of triton X-100 to obtain an oil phase system;
(2) weighing 8mL of methacryloyloxyethyl trimethyl ammonium chloride, 10mL of deionized water, 0.05g of potassium persulfate and 0.12g of sodium bisulfite, mixing, introducing argon for 30min, heating to 30 ℃, keeping the temperature for 5h, adding 0.5g of carmine, uniformly mixing, and putting into the reactor in the step (1); finally, stirring uniformly at the rotating speed of 400r/min to enable the water phase to form uniform liquid drops to be dispersed in the oil phase system, and obtaining a W/O internal water phase system;
(3) weighing 2.5g of polyvinyl alcohol, 800.6 g of Tween and 250mL of deionized water, mixing, and uniformly stirring at a rotating speed of 400r/min to obtain an external water phase system; adding the W/O internal aqueous phase system obtained in the step (2) into an external aqueous phase system to obtain a W/O/W reversed-phase suspension polymerization system;
(4) continuously stirring the W/O/W reversed phase suspension polymer system at the rotating speed of 450r/min until the system is stable, keeping the temperature of the system at 30 ℃ for 1h, heating to 50 ℃, keeping the temperature for 5h, cooling to 20 ℃, filtering to obtain spheres, leaching the spheres with water at 85 ℃, and drying in vacuum to obtain the colored polymer microspheres, namely the biodegradable food pigment microcapsules.
Example two:
a preparation method of biodegradable food pigment microcapsules comprises the following steps:
(1) weighing 1g of polylactic acid and 50mL of dichloromethane, mixing, putting into a reaction vessel, starting stirring, then putting the reaction vessel into a water bath, heating to 50 ℃, and then adding 2g of polyvinylpyrrolidone and 0.75g of triton X-100 to obtain an oil phase system;
(2) weighing 5mL of methacryloyloxyethyl trimethyl ammonium chloride, 10mL of deionized water, 0.06g of potassium persulfate and 0.12g of sodium bisulfite, mixing, introducing argon for 30min, heating to 30 ℃, keeping the temperature for 5h, adding 0.5g of carmine, uniformly mixing, and putting into the reactor in the step (1); finally, stirring uniformly at the rotating speed of 400r/min to enable the water phase to form uniform liquid drops to be dispersed in the oil phase system, and obtaining a W/O internal water phase system;
(3) weighing 2.5g of polyvinyl alcohol, 800.6 g of Tween and 250mL of deionized water, mixing, and uniformly stirring at a rotating speed of 400r/min to obtain an external water phase system; adding the W/O internal aqueous phase system obtained in the step (2) into an external aqueous phase system to obtain a W/O/W reversed-phase suspension polymerization system;
(4) continuously stirring the W/O/W reversed phase suspension polymer system at the rotating speed of 450r/min until the system is stable, keeping the temperature of the system at 30 ℃ for 1h, heating to 50 ℃, keeping the temperature for 5h, cooling to 20 ℃, filtering to obtain spheres, leaching the spheres with water at 85 ℃, and drying in vacuum to obtain the colored polymer microspheres, namely the biodegradable food pigment microcapsules.
Example three:
a preparation method of biodegradable food pigment microcapsules comprises the following steps:
(1) weighing 1g of polylactic acid and 50mL of dichloromethane, mixing, putting into a reaction vessel, starting stirring, then putting the reaction vessel into a water bath, heating to 50 ℃, and then adding 2g of polyvinylpyrrolidone and 0.75g of triton X-100 to obtain an oil phase system;
(2) weighing 5mL of methacryloyloxyethyl trimethyl ammonium chloride, 10mL of deionized water, 0.06g of potassium persulfate and 0.12g of sodium bisulfite, mixing, introducing argon for 30min, heating to 30 ℃, keeping the temperature for 5h, adding 0.5g of carmine, uniformly mixing, and putting into the reactor in the step (1); finally, stirring uniformly at the rotating speed of 400r/min to enable the water phase to form uniform liquid drops to be dispersed in the oil phase system, and obtaining a W/O internal water phase system;
(3) weighing 3g of polyvinyl alcohol, 800.6 g of Tween and 250mL of deionized water, mixing, and uniformly stirring at a rotating speed of 400r/min to obtain an external water phase system; adding the W/O internal aqueous phase system obtained in the step (2) into an external aqueous phase system to obtain a W/O/W reversed-phase suspension polymerization system;
(4) continuously stirring the W/O/W reversed phase suspension polymer system at the rotating speed of 450r/min until the system is stable, keeping the temperature of the system at 30 ℃ for 1h, heating to 50 ℃, keeping the temperature for 5h, cooling to 20 ℃, filtering to obtain spheres, leaching the spheres with water at 85 ℃, and drying in vacuum to obtain the colored polymer microspheres, namely the biodegradable food pigment microcapsules.
Example four:
a preparation method of biodegradable food pigment microcapsules comprises the following steps:
(1) weighing 1g of polylactic acid and 50mL of dichloromethane, mixing, putting into a reaction vessel, starting stirring, then putting the reaction vessel into a water bath, heating to 50 ℃, and then adding 2g of polyvinylpyrrolidone and 0.75g of triton X-100 to obtain an oil phase system;
(2) weighing 5mL of methacryloyloxyethyl trimethyl ammonium chloride, 10mL of deionized water, 0.06g of potassium persulfate and 0.12g of sodium bisulfite, mixing, introducing argon for 30min, heating to 30 ℃, keeping the temperature for 5h, adding 0.5g of carmine, uniformly mixing, and putting into the reactor in the step (1); finally, stirring uniformly at the rotating speed of 400r/min to enable the water phase to form uniform liquid drops to be dispersed in the oil phase system, and obtaining a W/O internal water phase system;
(3) weighing 3g of polyvinyl alcohol, 3g of Tween-800.4 g and 250mL of deionized water, and uniformly stirring at a rotating speed of 400r/min to obtain an external water phase system; adding the W/O internal aqueous phase system obtained in the step (2) into an external aqueous phase system to obtain a W/O/W reversed-phase suspension polymerization system;
(4) continuously stirring the W/O/W reversed phase suspension polymer system at the rotating speed of 450r/min until the system is stable, keeping the temperature of the system at 30 ℃ for 1h, heating to 50 ℃, keeping the temperature for 5h, cooling to 20 ℃, filtering to obtain spheres, leaching the spheres with water at 85 ℃, and drying in vacuum to obtain the colored polymer microspheres, namely the biodegradable food pigment microcapsules.
Example five:
a preparation method of biodegradable food pigment microcapsules comprises the following steps:
(1) weighing 0.8g of polylactic acid and 50mL of dichloromethane, mixing, putting into a reaction vessel, starting stirring, then putting the reaction vessel into a water bath, heating to 50 ℃, and then adding 2g of polyvinylpyrrolidone and 0.75g of triton X-100 to obtain an oil phase system;
(2) weighing 4mL of methacryloyloxyethyl trimethyl ammonium chloride, 7mL of deionized water, 0.03g of potassium persulfate and 0.06g of sodium bisulfite, mixing, introducing argon for 30min, heating to 30 ℃, keeping the temperature for 5h, adding 0.25g of carmine, uniformly mixing, and putting into the reactor in the step (1); finally, stirring uniformly at the rotating speed of 400r/min to enable the water phase to form uniform liquid drops to be dispersed in the oil phase system, and obtaining a W/O internal water phase system;
(3) weighing 2.5g of polyvinyl alcohol, 2. 800.5 g of Tween and 200mL of deionized water, mixing, and stirring uniformly at a rotating speed of 400r/min to obtain an external water phase system; adding the W/O internal aqueous phase system obtained in the step (2) into an external aqueous phase system to obtain a W/O/W reversed-phase suspension polymerization system;
(4) continuously stirring the W/O/W reversed phase suspension polymer system at the rotating speed of 450r/min until the system is stable, keeping the temperature of the system at 25 ℃ for 1h, heating to 50 ℃, keeping the temperature for 5h, cooling to 20 ℃, filtering to obtain spheres, leaching the spheres with water at 85 ℃, and drying in vacuum to obtain the colored polymer microspheres, namely the biodegradable food pigment microcapsules.
Example six:
a preparation method of biodegradable food pigment microcapsules comprises the following steps:
(1) weighing 1.5g of polylactic acid and 50mL of dichloromethane, mixing, putting into a reaction vessel, starting stirring, then putting the reaction vessel into a water bath, heating to 50 ℃, and then adding 2g of polyvinylpyrrolidone and 0.75g of triton X-100 to obtain an oil phase system;
(2) weighing 10mL of methacryloyloxyethyl trimethyl ammonium chloride, 12.5mL of deionized water, 0.075g of potassium persulfate and 0.15g of sodium bisulfite, mixing, introducing argon for 30min, heating to 30 ℃, keeping the temperature for 5h, adding 0.1g of carmine, uniformly mixing, and putting into the reactor in the step (1); finally, stirring uniformly at the rotating speed of 400r/min to enable the water phase to form uniform liquid drops to be dispersed in the oil phase system, and obtaining a W/O internal water phase system;
(3) weighing 7.5g of polyvinyl alcohol, 300mL of Tween-801.25 g of deionized water, mixing, and stirring uniformly at a rotating speed of 400r/min to obtain an external water phase system; adding the W/O internal aqueous phase system obtained in the step (2) into an external aqueous phase system to obtain a W/O/W reversed-phase suspension polymerization system;
(4) continuously stirring the W/O/W reversed phase suspension polymer system at the rotating speed of 450r/min until the system is stable, keeping the temperature of the system at 40 ℃, keeping the temperature for 1h, heating to 50 ℃, keeping the temperature for 5h, cooling to 20 ℃, filtering to obtain spheres, leaching the spheres with water at 85 ℃, and drying in vacuum to obtain the colored polymer microspheres, namely the biodegradable food pigment microcapsules.
Claims (1)
1. A preparation method of biodegradable food pigment microcapsules is characterized by comprising the following steps:
(1) weighing 0.8-1.5g of polylactic acid and 50mL of dichloromethane, mixing, putting into a reaction vessel, starting stirring, putting the reaction vessel into a water bath, heating to 50 ℃, and then adding 2g of polyvinylpyrrolidone and 0.75g of triton X-100 to obtain an oil phase system;
(2) weighing 4-10mL of methacryloyloxyethyl trimethyl ammonium chloride, 7-12.5mL of deionized water, 0.03-0.075g of potassium persulfate and 0.06-0.15g of sodium bisulfite, mixing, introducing argon for 30min, heating to 30 ℃, keeping the temperature for 5h, adding 0.25-0.1g of carmine, uniformly mixing, and putting into the reactor in the step (1); finally, stirring uniformly at the rotating speed of 400r/min to enable the water phase to form uniform liquid drops to be dispersed in the oil phase system, and obtaining a W/O internal water phase system;
(3) weighing 2.5-7.5g of polyvinyl alcohol, 1.25-1.32 g of Tween-800.5 and 300mL of deionized water, and uniformly stirring at a rotating speed of 400r/min to obtain an external water phase system; adding the W/O internal aqueous phase system obtained in the step (2) into an external aqueous phase system to obtain a W/O/W reversed-phase suspension polymerization system;
(4) continuously stirring the W/O/W reversed phase suspension polymer system at the rotating speed of 450r/min until the system is stable, keeping the temperature of the system at 25-40 ℃, keeping the temperature for 1h, heating to 50 ℃, keeping the temperature for 5h, cooling to room temperature, filtering to obtain spheres, leaching the spheres with water at 85 ℃, and drying in vacuum to obtain the colored polymer microspheres, namely the biodegradable food pigment microcapsules.
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