The invention content is as follows:
in order to solve the technical problems, the invention provides a composite hydrogel containing rose residue modified dietary fiber and gelatin, wherein the content of the rose residue modified dietary fiber is 0.1-2% (w/w, mass ratio to water), and the content of the gelatin is 5-10% (w/w, mass ratio to water);
the mass ratio of SDF to IDF in the rose residue modified dietary fiber is 1:3-1: 6;
preferably, the rose residue modified dietary fiber is a composite enzyme modified dietary fiber;
preferably, the content of the rose residue modified dietary fiber is 0.67%;
preferably, the gelatin content is 6.67%;
the invention also provides a preparation method of the composite hydrogel containing the rose residue modified dietary fiber and the gelatin, which comprises the following specific steps:
fully soaking gelatin in water, and dissolving in a heat insulation manner to prepare a gelatin solution of 5-10% (w/w, mass ratio of gelatin to water); adding 0.1-2% (w/w, mass ratio of water) of rose residue modified dietary fiber; uniformly mixing the rose residue modified dietary fiber-gelatin suspension, pouring the mixture into a container for cooling, and storing the mixture overnight to obtain solid rose residue modified dietary fiber-gelatin hydrogel;
the preparation method of the rose residue modified dietary fiber comprises the following steps:
(1) pretreatment: drying rose dregs and then crushing;
(2) preparing a rose dreg suspension: adding 25-50 times (w/w) of water into the rose residue powder, and adjusting pH to 6.5-8.5;
(3) enzymolysis: adding 30-300U of high temperature resistant amylase into each gram of rose residue powder, and stirring and performing enzymolysis for 15-45 minutes at 80-95 ℃; then cooling to 50-65 ℃, adding 3000-15000U protease per gram of rose residue powder, stirring and carrying out enzymolysis for 15-45 minutes; then adjusting the pH of the suspension to 4.0-6.0, adding 30-300U of amyloglucosidase into each gram of rose residue powder, and stirring for enzymolysis for 15-45 minutes; adding 200-300U cellulase and 500-900U xylanase into each gram of rose residue powder for enzymolysis for 1-2.5 hours for modification;
(4) separation: centrifuging the suspension after enzymolysis, washing the precipitate with water, 75-90% ethanol, 90-99% ethanol and acetone in sequence, filtering, and drying the filter residue to obtain IDF;
(5) alcohol precipitation: adding 90-99% ethanol into the supernatant after centrifugal separation, standing overnight, centrifuging, and drying the precipitate to obtain SDF;
and mixing the obtained IDF and SDF to obtain the rose residue modified dietary fiber.
Has the advantages that:
(1) the modified dietary fiber used in the invention has a looser space network structure (see figure 6), is remarkably improved in expansibility, specific surface area, water absorption and oil absorption capacity, is more beneficial to discharge waste in intestinal tracts, slows down absorption of glucose, cholesterol and the like, and can strengthen the effect of regulating intestinal flora.
(2) The gelatin and the modified dietary fiber mixed with the gelatin can improve the crosslinking degree and the microscopic form of gelatin molecules, and obviously improve the rheological and textural quality of the gelatin.
(3) The rose dregs are creatively used as the source of dietary fiber, and are modified to be used for preparing the composite gel, so that the rose fruit gel has proper hardness, elasticity and mouthfeel, and can be used as a raw and auxiliary material of food with certain processing strength.
The specific implementation mode is as follows:
in order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present patent and are not intended to limit the present invention.
Example 1 preparation method of rose residue modified dietary fiber
The preparation method comprises the following steps:
(1) pretreatment: drying rose dregs and then crushing;
(2) preparing a rose dreg suspension: adding 30 times (w/w) of water into the rose residue powder, and adjusting the pH to 7.0;
(3) enzymolysis: adding 200U of high temperature resistant amylase into each gram of rose residue powder, and stirring and performing enzymolysis for 30 minutes at 85 ℃; then cooling to 50 ℃, adding 6000U protease per gram of rose residue powder, stirring and performing enzymolysis for 30 minutes; then, adjusting the pH of the suspension to 5.0 by using 0.5mol/L hydrochloric acid, adding 100U of amyloglucosidase into each gram of rose residue powder, and stirring for enzymolysis for 30 minutes; adding 250U cellulase and 700U xylanase into each gram of rose residue powder for enzymolysis for 2 hours for modification;
(4) separation: centrifuging the enzymolyzed suspension at 5500r/min at 4 deg.C for 15min, washing precipitate with water, 80% ethanol, 95% ethanol and acetone, filtering, and drying the filter residue to obtain IDF;
(5) alcohol precipitation: adding 4 times volume of 95% ethanol into the supernatant after centrifugal separation, standing overnight, and drying and precipitating after centrifugation to obtain SDF.
And mixing the obtained IDF and SDF to obtain the rose residue modified dietary fiber.
And (3) carrying out water holding capacity, swelling capacity, oil holding capacity, cholesterol adsorption capacity, cation exchange capacity and glucose adsorption capacity determination on the obtained modified IDF and the obtained unmodified IDF (the preparation method of the unmodified IDF only removes the cellulase and xylanase enzymolysis steps in the steps, and the rest are the same).
(1) The water holding capacity, swelling capacity and oil holding capacity of IDF before and after modification are shown in FIG. 1.
As can be seen from fig. 1, the water holding capacity, swelling capacity and oil holding capacity of the modified IDF are significantly improved compared to the unmodified IDF, and the modified IDF can be applied to various foods for modifying viscosity and texture, absorbing fat in emulsified products, avoiding dehydration problems (dietary fiber with high water holding capacity can improve food structure and prevent syneresis), and other health-related effects.
(2) In vitro simulation evaluation of the absorption capacity of IDF before and after modification in gastric environment (pH2) and intestinal environment (pH7) is shown in fig. 2.
(3) FIG. 3 shows the trend of the change of the cation exchange of IDF before and after modification, and during the transition of the pH of the suspension from acidic to alkaline, the volume of NaOH required by the modified IDF is more at the same pH, which shows that the modified IDF can combine more ions and has stronger cation exchange capacity.
(4) Fig. 4 shows that the modification treatment significantly increased the amount of glucose adsorbed by IDF at different glucose concentrations.
Example 2A composite hydrogel comprising Rose hips residue modified dietary fiber and gelatin
A composite hydrogel comprising rose residue modified dietary fiber and gelatin, wherein the content of the rose residue modified dietary fiber is 0.67% (w/w, mass ratio to water), and the content of the gelatin is 6.67% (w/w, mass ratio to water);
fully soaking gelatin in water, and dissolving under heat insulation to obtain 6.67% (w/w) gelatin solution; adding 0.67% (w/w) of rose residue modified dietary fiber; uniformly mixing the rose residue modified dietary fiber-gelatin suspension by using a magnetic stirrer, pouring the mixture into a container for cooling, and storing at 4 ℃ overnight to obtain solid rose residue modified dietary fiber-gelatin hydrogel;
the preparation method of the rose residue modified dietary fiber comprises the following steps:
(1) pretreatment: drying rose dregs and then crushing;
(2) preparing a rose dreg suspension: adding 25 times (w/w) of water into the rose residue powder, and adjusting the pH to 8.0;
(3) enzymolysis: adding 30U of high temperature resistant amylase into each gram of rose residue powder, and stirring and performing enzymolysis for 30 minutes at 80 ℃; then cooling to 60 ℃, adding 5000U protease per gram of rose residue powder, stirring and performing enzymolysis for 30 minutes; then, adjusting the pH of the suspension to 4.0 by using 0.6mol/L hydrochloric acid, adding 30U of amyloglucosidase into each gram of rose residue powder, and stirring for enzymolysis for 30 minutes; adding 200U cellulase and 500U xylanase into each gram of rose residue powder for enzymolysis for 1 hour for modification;
(4) separation: centrifuging the suspension after enzymolysis, washing precipitates with water, 85% ethanol, 90% ethanol and acetone in sequence, then performing suction filtration, and drying filter residues to obtain IDF;
(5) alcohol precipitation: adding 90% ethanol into the supernatant after centrifugal separation, standing overnight, and drying the precipitate after centrifugation to obtain SDF.
And mixing the obtained SDF and IDF according to the mass ratio of 1:4 to obtain the rose residue modified dietary fiber.
Example 3A composite hydrogel comprising Rose hips residue modified dietary fiber and gelatin
A composite hydrogel comprising rose residue modified dietary fiber and gelatin, wherein the content of the rose residue modified dietary fiber is 0.1% (w/w), and the content of the gelatin is 5% (w/w);
the preparation method specifically comprises the following steps:
fully soaking gelatin in water, and dissolving the gelatin in a heat insulation manner to prepare a gelatin solution with the concentration of 5% (w/w); adding 0.1% (w/w) rose residue modified dietary fiber; uniformly mixing the rose residue modified dietary fiber-gelatin suspension by using a magnetic stirrer, pouring the mixture into a container for cooling, and storing at 4 ℃ overnight to obtain solid rose residue modified dietary fiber-gelatin hydrogel;
the preparation method of the rose flower residue modified dietary fiber comprises the following steps:
(1) pretreatment: drying rose dregs and then crushing;
(2) preparing a rose dreg suspension: adding 30 times (w/w) of water into the rose residue powder, and adjusting the pH to 6.5;
(3) enzymolysis: adding 50U of high temperature resistant amylase into each gram of rose residue powder, and stirring and performing enzymolysis for 15 minutes at 85 ℃; then cooling to 55 ℃, adding 3000U protease per gram of rose residue powder, stirring and performing enzymolysis for 15 minutes; then, adjusting the pH of the suspension to 5.0 by using 0.4mol/L hydrochloric acid, adding 50U of amyloglucosidase into each gram of rose residue powder, and stirring for enzymolysis for 15 minutes; adding 200U cellulase and 500U xylanase into each gram of rose residue powder for enzymolysis for 1.5 hours for modification;
(4) separation: centrifuging the suspension after enzymolysis, washing precipitates with water, 75% ethanol, 90% ethanol and acetone in sequence, then performing suction filtration, and drying filter residues to obtain IDF;
(5) alcohol precipitation: adding 95% ethanol into the supernatant after centrifugal separation, standing overnight, centrifuging, and drying the precipitate to obtain SDF;
and mixing the obtained SDF and IDF according to the mass ratio of 1:3 to obtain the rose residue modified dietary fiber.
Example 4A composite hydrogel comprising Rose hips residue modified dietary fiber and gelatin
A composite hydrogel comprising rose residue modified dietary fiber and gelatin, wherein the content of the rose residue modified dietary fiber is 2% (w/w), and the content of the gelatin is 10% (w/w);
the preparation method comprises the following specific steps:
fully soaking gelatin in water, and dissolving the gelatin in a heat insulation manner to prepare a 10% (w/w) gelatin solution; adding 2% (w/w) of rose residue modified dietary fiber; uniformly mixing the rose residue modified dietary fiber-gelatin suspension by using a magnetic stirrer, pouring the mixture into a container for cooling, and storing at 4 ℃ overnight to obtain solid rose residue modified dietary fiber-gelatin hydrogel;
the preparation method of the rose residue modified dietary fiber comprises the following steps:
(1) pretreatment: drying rose dregs and then crushing;
(2) preparing a rose dreg suspension: adding 50 times (w/w) of water into the rose residue powder, and adjusting the pH to 8.5;
(3) enzymolysis: adding 300U of high temperature resistant amylase into each gram of rose residue powder, and stirring and performing enzymolysis for 45 minutes at 95 ℃; then cooling to 65 ℃, adding 15000U protease per gram of rose residue powder, stirring and performing enzymolysis for 45 minutes; then, adjusting the pH of the suspension to 5.5 by using 1mol/L hydrochloric acid, adding 300U of amyloglucosidase into each gram of rose residue powder, and stirring for enzymolysis for 45 minutes; adding 300U cellulase and 900U xylanase into each gram of rose residue powder for enzymolysis for 2.5 hours for modification;
(4) separation: centrifuging the suspension after enzymolysis, washing precipitates with water, 90% ethanol, 99% ethanol and acetone in sequence, then performing suction filtration, and drying filter residues to obtain IDF;
(5) alcohol precipitation: adding 99% ethanol into the supernatant after centrifugal separation, standing overnight, and drying the precipitate after centrifugation to obtain SDF;
and mixing the obtained SDF and IDF according to the mass ratio of 1:6 to obtain the rose residue modified dietary fiber.
EXAMPLE 5 Effect test
Preparing a composite gel of rose residue dietary fiber (RPDF) and gelatin by adopting the mode of example 2, wherein the addition amount of the RPDF is 0 percent; 0.33% of rose residue modified dietary fiber, 0.67% of rose residue modified dietary fiber and 1% of rose residue modified dietary fiber; 0.33% of rose residue unmodified dietary fiber, 0.67% of rose residue unmodified dietary fiber and 1% of rose residue unmodified dietary fiber;
wherein, the preparation methods of all the modified dietary fibers are the same as the example 2, the preparation methods of all the unmodified dietary fibers only remove the enzymolysis steps of the cellulase and the xylanase in the preparation method of the dietary fibers in the example 2, and the rest are the same.
(1) Dynamic temperature scanning
Subjecting the gel obtained by the above preparation to dynamic temperatureScanning, as shown in fig. 5. Gelation temperature T of RPDF-gelatingAnd melting temperature TmDefined as the temperature at the G' and G "crossover point during the cooling phase and the heating phase, respectively. FIG. 5 shows T of RPDF-gelatin systemgAnd TmThe relationship between the amount of addition and the modification treatment. T of all RPDF-gelatin samplesmT of unmodified RPDF-gelatin higher than that of pure gelatin (25-26℃)mModification of T of RPDF-gelatin at 26-30 deg.CmThe values at 28-30 ℃ increased and then decreased with the RPDF addition, and the values at 0.67% were the highest overall (29.5 ℃). The gel melting point is too low, which causes adverse effects such as difficult shaping, difficult storage, poor chewiness and the like, and has higher requirements on processing conditions, storage environment and sensory evaluation. The addition of the dietary fiber improves the melting point of the gelatin, is beneficial to maintaining morphological characters under a certain temperature condition, can meet higher processing, storage and eating requirements, and has better effect of modifying the dietary fiber. The combination of the dietary fiber and the gelatin not only utilizes the function of the dietary fiber to ensure low calorie intake, but also improves the weakness of the physical property of the gelatin in practical application and expands the development and utilization space of the gelatin.
(2) Effect of RPDF on gel texture Properties
Table 1 shows the effect of different RPDF additions and different treatments of dietary fiber on the gelatin texture properties. The data show that the addition of RPDF significantly improved gel cohesion; the hardness is increased and then reduced along with the increase of the addition amount, and the hardness reaches the maximum at 0.67 percent; after the addition amount of the modified RPDF exceeds 0.67 percent, the gel hardness, the chewiness and the adhesiveness are obviously reduced, while the unmodified RPDF has no obvious influence on the gel texture property at higher addition amount; compared with a pure gelatin sample, the dietary fiber reaches the highest level of hardness, chewiness and adhesiveness when the addition amount of the dietary fiber is 0.67 percent.
TABLE 1 Effect of Rose hips dietary fiber addition on gel texture Properties
(3) RPDF-gelatin microstructure Observation
The RPDF-gelatin freeze-dried sample is observed by a scanning electron microscope (shown in figure 6), and the pure gelatin hydrogel sample has a lamellar structure, a smooth surface and larger pores; the gel added with the RPDF exists in a spongy cluster, and the gaps are in a bundle shape or a channel shape; along with the increase of the RPDF content, the gel structure is gathered into a flocculent honeycomb type, the structure is damaged, the surface is rough, the gaps are gradually reduced to be pit-shaped or circular, and the combination of the IDF and the gelatin is changed from an embedded type to an embedded type. This phenomenon may be due to the water absorption and steric stability of RPDF, which may combine with some components in gelatin, making the microstructure more compact. According to researches, the large-area continuous network structure with uniform pore size distribution, more pores and smaller diameter can ensure that the gel keeps certain resistance under the action of external shear or under the condition of higher temperature, the characteristics of solid objects of the gel are not easy to damage, and the complex system can show higher storage modulus and hardness in rheological and texture property tests. The edible taste and the actual production are considered comprehensively, the addition amount of 0.67 percent of RPDF-gelatin is moderate, and the RPDF-gelatin can be used as a raw material and an auxiliary material of food with certain processing strength.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the patent. It should be noted that, for those skilled in the art, various changes, combinations and improvements can be made in the above embodiments without departing from the patent concept, and all of them belong to the protection scope of the patent. Therefore, the protection scope of this patent shall be subject to the claims.