CN109206529B - Processing method of high water-holding carrageenan - Google Patents
Processing method of high water-holding carrageenan Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0036—Galactans; Derivatives thereof
- C08B37/0042—Carragenan or carragen, i.e. D-galactose and 3,6-anhydro-D-galactose, both partially sulfated, e.g. from red algae Chondrus crispus or Gigantia stellata; kappa-Carragenan; iota-Carragenan; lambda-Carragenan; Derivatives thereof
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Abstract
The invention discloses a processing method of high water-holding carrageenan, belonging to the field of food processing. The high water-holding carrageenan is prepared by taking kappa-carrageenan as a raw material and crushing after alkali treatment, three times of ultrahigh pressure assisted carboxymethylation reaction, neutralization, washing, freeze drying. The invention has mild process conditions and high efficiency, and the prepared high water-holding carrageenan has high water-holding rate and high gel strength. The invention has reasonable technology, good product application prospect and good expected economic and social benefits.
Description
Technical Field
The invention belongs to the field of food processing, and particularly relates to a processing method of high water-holding carrageenan.
Background
Carrageenan (Carrageenan), also known as Carrageenan, is generally extracted from red algae of the genus Chondrus or Eucheuma. Kappa-carrageenan is mainly composed of repetitive disaccharide units such as alpha (1 → 3) -D-galactose-4-sulfate and beta (1 → 4) -3, 6-anhydro-D-galactose, can be used as fillers, emulsifiers, gelling agents, thickeners and the like, and is widely applied to the fields of food, chemical industry, medicine and the like.
Because the gel of the kappa-carrageenan has brittleness and bleeding property (namely poor water retention property), the quality of the gel product is seriously influenced. At present, the method for solving the problem of poor gel water retention of kappa-carrageenan mainly improves the gel stability by compounding other colloids or macromolecular materials so as to avoid the occurrence of bleeding phenomenon, but the process is more complex and the adaptability is poor.
The structure of the polysaccharide can be improved by carboxymethylation, thereby improving the solubility and the gel property of the polysaccharide. The modified starch is mainly used for preparing carboxymethyl starch at present, and the viscosity, the ageing resistance and the water retention property of the modified starch are all obviously improved. However, the modification of non-starch polysaccharides, particularly carrageenan, using conventional carboxymethylation methods results in a reduction in gel strength. After only adopting carboxymethylation to process the carrageenan, the gel strength is reduced to 460 g/cm2And the water retention rate is 95.7 percent. After one-time ultrahigh pressure auxiliary carboxymethylation reaction treatment, the gel strength and the water retention rate are improved to 820 g/cm respectively2And 96.6%, but coagulatedThe glue strength and the water holding rate are still low, and the commodity value is influenced.
Disclosure of Invention
The invention aims to provide a processing method of high water-holding carrageenan aiming at the defects of the prior art, and the obtained modified carrageenan not only has excellent water holding capacity, but also has higher gel strength.
In order to achieve the purpose, the invention adopts the following technical scheme:
(1) alkali treatment: dispersing kappa-carrageenan powder into 80-95 wt% propanol solution according to the mass ratio of 1: 10-1: 15, and adding 20wt% NaOH solution to ensure that the mass ratio of NaOH to kappa-carrageenan powder in the system is 10-30: 100, fully stirring, and keeping the temperature of 10-35 ℃ for 1-2 h;
(2) three times of ultrahigh pressure assisted carboxymethylation reaction: adding chloroacetic acid into the reaction system in the step (1) to enable the mass ratio of the chloroacetic acid to the carrageenan powder to be 6.5-19.5: 100, packaging the mixture in a plastic bag, sealing, placing the plastic bag in a static ultrahigh pressure machine, treating the mixture at 800 MPa-1200 MPa and 25-45 ℃ for 20-60 min, reducing the pressure to normal pressure and keeping the pressure for 5min, treating the mixture at 200 MPa-400 MPa and 25-45 ℃ for 10 min-20 min, reducing the pressure to normal pressure and keeping the pressure for 5min, and finally treating the mixture at 100 MPa-200 MPa and 25-45 ℃ for 5 min-10 min, and reducing the pressure to normal pressure and keeping the pressure for 5 min;
(3) neutralizing: after the carboxymethylation reaction is finished, gradually adding 1mol/L acetic acid solution into the reaction system until the pH value of the reaction system is 7;
(4) washing: suction-filtering the carboxymethylation reaction product obtained in the step (3), and washing a filter cake for 3 times by using an ethanol solution with the concentration of 80-95 wt%;
(5) freeze drying and crushing: and (4) placing the washed filter cake into a vacuum freeze dryer, drying, crushing, and sieving by a 80-mesh sieve to obtain a sieved substance, namely a finished product.
The invention has the following remarkable advantages:
(1) adopting a kappa-carrageenan, chloroacetic acid, NaOH and propanol solution system to carry out carboxymethylation reaction, and obviously improving the hydrophilicity of the carrageenan through carboxymethylation;
(2) the carboxymethylation reaction is assisted by the ultrahigh pressure with three-level pressure decreasing, so that the carboxymethylation reaction efficiency can be improved, the carrageenan crosslinking degree can be increased, and the internal stress can be eliminated, thereby ensuring higher gel strength and excellent water retention.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
(1) Alkali treatment: dispersing kappa-carrageenan powder into a propanol solution with a concentration of 80wt% according to a mass ratio of 1:10, adding a NaOH solution with a concentration of 20wt% to ensure that the mass ratio of NaOH to the kappa-carrageenan powder in the system is 10:100, fully stirring, and keeping at 10 ℃ for 2 hours;
(2) three times of ultrahigh pressure assisted carboxymethylation reaction: adding chloroacetic acid into the reaction system in the step (1) to enable the mass ratio of the chloroacetic acid to the carrageenan powder to be 6.5:100, packaging the mixture in a plastic bag, sealing, placing in a static ultrahigh pressure machine, treating at 800MPa and 45 ℃ for 60min, reducing to normal pressure and keeping for 5min, treating at 200MPa and 45 ℃ for 20min, reducing to normal pressure and keeping for 5min, and finally treating at 100MPa and 45 ℃ for 10min, reducing to normal pressure and keeping for 5 min;
(3) neutralizing: after the carboxymethylation reaction is finished, gradually adding 1mol/L acetic acid solution into the reaction system until the pH value of the reaction system is 7;
(4) washing: carrying out suction filtration on the carboxymethylation reaction product obtained in the step (3), and washing a filter cake for 3 times by using an ethanol solution with the concentration of 80 wt%;
(5) freeze drying and crushing: and (4) placing the washed filter cake into a vacuum freeze dryer, drying, crushing, and sieving by a 80-mesh sieve to obtain a sieved substance, namely a finished product.
Example 2
(1) Alkali treatment: dispersing kappa-carrageenan powder into a propanol solution with the concentration of 90wt% according to the mass ratio of 1:12, adding a NaOH solution with the concentration of 20wt% to ensure that the mass ratio of NaOH to the kappa-carrageenan powder in a system is 20:100, fully stirring, and keeping the temperature at 20 ℃ for 1.5 hours;
(2) three times of ultrahigh pressure assisted carboxymethylation reaction: adding chloroacetic acid into the reaction system in the step (1) to enable the mass ratio of the chloroacetic acid to the carrageenan powder to be 13:100, packaging the mixture in a plastic bag, sealing, placing in a static ultrahigh pressure machine, treating at 1000MPa and 35 ℃ for 40min, reducing to normal pressure and keeping for 5min, treating at 300MPa and 35 ℃ for 15min, reducing to normal pressure and keeping for 5min, treating at 150MPa and 35 ℃ for 7min, and reducing to normal pressure and keeping for 5 min;
(3) neutralizing: after the carboxymethylation reaction is finished, gradually adding 1mol/L acetic acid solution into the reaction system until the pH value of the reaction system is 7;
(4) washing: carrying out suction filtration on the carboxymethylation reaction product obtained in the step (3), and washing a filter cake for 3 times by using an ethanol solution with the concentration of 90 wt%;
(5) freeze drying and crushing: and (4) placing the washed filter cake into a vacuum freeze dryer, drying, crushing, and sieving by a 80-mesh sieve to obtain a sieved substance, namely a finished product.
Example 3
(1) Alkali treatment: dispersing kappa-carrageenan powder into a propanol solution with the concentration of 95wt% according to the mass ratio of 1:15, adding a NaOH solution with the concentration of 20wt% to ensure that the mass ratio of NaOH to the kappa-carrageenan powder in a system is 30:100, fully stirring, and keeping at 35 ℃ for 1 h;
(2) three times of ultrahigh pressure assisted carboxymethylation reaction: adding chloroacetic acid into the reaction system in the step (1) to enable the mass ratio of the chloroacetic acid to the carrageenan powder to be 19.5:100, packaging the mixture in a plastic bag, sealing, placing in a static ultrahigh pressure machine, treating at 1200MPa and 25 ℃ for 20min, reducing to normal pressure and keeping for 5min, treating at 400MPa and 25 ℃ for 10min, reducing to normal pressure and keeping for 5min, and finally treating at 200MPa and 25 ℃ for 5min, and reducing to normal pressure and keeping for 5 min;
(3) neutralizing: after the carboxymethylation reaction is finished, gradually adding 1mol/L acetic acid solution into the reaction system until the pH value of the reaction system is 7;
(4) washing: carrying out suction filtration on the carboxymethylation reaction product obtained in the step (3), and washing a filter cake for 3 times by using an ethanol solution with the concentration of 95 wt%;
(5) freeze drying and crushing: and (4) placing the washed filter cake into a vacuum freeze dryer, drying, crushing, and sieving by a 80-mesh sieve to obtain a sieved substance, namely a finished product.
Comparative example 1
(1) Alkali treatment: dispersing kappa-carrageenan powder into a propanol solution with the concentration of 90wt% according to the mass ratio of 1:12, adding a NaOH solution with the concentration of 20wt% to ensure that the mass ratio of NaOH to the kappa-carrageenan powder in a system is 20:100, fully stirring, and keeping the temperature at 20 ℃ for 1.5 hours;
(2) one-time ultrahigh pressure assisted carboxymethylation reaction: adding chloroacetic acid into the reaction system in the step (1) to enable the mass ratio of the chloroacetic acid to the carrageenan powder to be 13:100, packaging the mixture in a plastic bag, sealing, placing in a static ultrahigh pressure machine, treating at 1000MPa and 35 ℃ for 40min, and reducing the pressure to normal pressure to keep for 5 min;
(3) neutralizing: after the carboxymethylation reaction is finished, gradually adding 1mol/L acetic acid solution into the reaction system until the pH value of the reaction system is 7;
(4) washing: carrying out suction filtration on the carboxymethylation reaction product obtained in the step (3), and washing a filter cake for 3 times by using an ethanol solution with the concentration of 90 wt%;
(5) freeze drying and crushing: and (3) placing the washed filter cake into a vacuum freeze dryer, drying, crushing, and sieving with a 80-mesh sieve to obtain the undersize product, namely the carrageenan subjected to the primary ultrahigh pressure treatment.
The performance of kappa-carrageenan, the carrageenan prepared in comparative example 1 and once ultra-high pressure treatment and the high water-holding carrageenan prepared in example 2 of the present invention were tested and the results are shown in table 1. It can be seen that by applying the technology and parameters of the invention, the prepared modified carrageenan has gel strength close to that of unmodified carrageenan, the water retention rate is greatly improved, and the total performance is high strength and strong water retention capacity.
TABLE 1 comparison of kappa-carrageenan Performance with different treatment-derived carrageenans
The above description is only an embodiment utilizing the technical content of the present disclosure, and any modification and variation made by those skilled in the art can be covered by the claims of the present disclosure, and not limited to the embodiments disclosed.
Claims (3)
1. A processing method of high water-holding carrageenan is characterized by comprising the following steps: the method comprises the following steps:
(1) alkali treatment: dispersing kappa-carrageenan powder into 80-95 wt% propanol solution according to the mass ratio of 1: 10-1: 15, adding 20wt% NaOH solution to enable the mass ratio of NaOH to the kappa-carrageenan powder in the system to be 10-30: 100, fully stirring, and keeping the temperature of 10-35 ℃ for 1-2 hours;
(2) three times of ultrahigh pressure assisted carboxymethylation reaction: adding chloroacetic acid into the reaction system in the step (1), packaging the mixture in a plastic bag, sealing, and carrying out carboxymethylation reaction under the assistance of three times of ultrahigh pressure;
(3) neutralizing: after the carboxymethylation reaction is finished, gradually adding 1mol/L acetic acid solution into the reaction system until the pH value of the reaction system is 7;
(4) washing: suction-filtering the carboxymethylation reaction product obtained in the step (3), and washing a filter cake for 3 times by using an ethanol solution with the concentration of 80-95 wt%;
(5) freeze drying and crushing: placing the washed filter cake in a vacuum freeze dryer, drying, crushing, and sieving with a 80-mesh sieve to obtain a product below the sieve;
in the step (2), the three times of ultrahigh pressure is processed at the temperature of 25-45 ℃ under the pressure of 800 MPa-1200 MPa for 20-60 min, and is reduced to normal pressure for 5min, then is processed at the temperature of 25-45 ℃ under the pressure of 200 MPa-400 MPa for 10 min-20 min, and is reduced to normal pressure for 5min, and finally is processed at the temperature of 25-45 ℃ under the pressure of 100 MPa-200 MPa for 5 min-10 min, and is reduced to normal pressure for 5 min.
2. The method for processing high water-holding carrageenan according to claim 1, wherein the method comprises the following steps: in the step (2), the mass ratio of the chloroacetic acid to the kappa-carrageenan powder is 6.5-19.5: 100.
3. The high water-holding carrageenan made by the process of claim 1.
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