Method for preparing emulsion gel easy to swallow by using phycocyanin nanoparticle-starch nanocrystal compound

Abstract

The invention relates to the technical field of emulsion gel preparation, in particular to a method for preparing easy-to-swallow emulsion gel by using a phycocyanin nanoparticle-starch nanocrystal compound, which comprises the following steps: preparing phycocyanin, starch, distilled water and soybean oil, dissolving the phycocyanin in the distilled water, then quickly injecting into absolute ethyl alcohol, and stirring to obtain a solution A; removing ethanol through rotary evaporation to obtain a phycocyanin nanoparticle solution A; adding starch into a concentrated sulfuric acid solution, heating in a water bath and magnetically stirring for reaction to obtain a starch nanocrystal solution B; mixing the solution A and the solution B to obtain a mixed solution C; and adding soybean oil into the mixed solution C, and performing high-speed shearing and homogenizing to obtain the emulsion gel. The emulsion gel prepared from the phycocyanin nanoparticle and starch nanocrystal compound is obviously improved in stability, soft and smooth in texture, controllable in fluidity, easy to swallow, natural and edible in material, high in biological activity and simple and convenient in preparation process, and is suitable for functional food development of old people and people with dysphagia.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of emulsion gel preparation, in particular to a method for preparing easy-to-swallow emulsion gel by using phycocyanin nanoparticle-starch nanocrystal complex. BACKGROUND

[0002] Developing soft and easy-to-swallow food suitable for dysphagia population has become an important direction in the field of functional food. Emulsion gel, which combines the good dispersibility of emulsion and the network structure of gel, becomes an ideal carrier system and is widely used in nutrient delivery and texture control.

[0003] In recent years, Pickering emulsion gel based on natural polymer materials has attracted attention. The complex system of protein and polysaccharide particles shows significant advantages due to strong interfacial activity, adjustable structure and good biocompatibility. Phycocyanin, as a natural colorant and antioxidant protein, has good biological activity and nutritional value; starch nanocrystals have high stability and food-grade safety.

[0004] However, existing emulsions have problems such as poor structural stability, weak environmental adaptability, too sticky or loose texture, etc., which are difficult to meet the eating needs of dysphagia population. SUMMARY

[0005] The purpose of the present application is to provide a method for preparing easy-to-swallow emulsion gel by using phycocyanin nanoparticle-starch nanocrystal complex, to solve the problems of poor structural stability, weak environmental adaptability, too sticky or loose texture, etc. of emulsion, which is difficult to meet the eating needs of dysphagia population.

[0006] To achieve the above purpose, the present application provides the following technical scheme: a method for preparing easy-to-swallow emulsion gel by using phycocyanin nanoparticle-starch nanocrystal complex, comprising the following steps:

[0007] S1, material preparation: preparing phycocyanin, starch, distilled water and soybean oil, the starch including cassava starch, corn starch and potato starch;

[0008] S2, preparing phycocyanin nanoparticle A: dissolving phycocyanin in distilled water in step S1, then quickly injecting the solution into anhydrous ethanol to obtain a phycocyanin nanoparticle solution;

[0009] The phycocyanin nanoparticle solution is rotary evaporated to remove ethanol, and a phycocyanin nanoparticle solution A is obtained;

[0010] S3, preparing starch nanocrystal B: adding starch in step S1 into concentrated sulfuric acid solution, heating in water bath and magnetically stirring the reaction;

[0011] After the reaction was completed, the precipitate was centrifuged and washed with distilled water to obtain starch nanocrystal solution B.

[0012] S4. Preparation of mixture C: Add solution A from step S2 to solution B from step S3 to obtain phycocyanin nanoparticle-starch nanocrystal mixture C;

[0013] S5. Obtaining emulsion gel: Add soybean oil to the mixture C in step S4, and homogenize the mixture C with added soybean oil using a homogenizer at high speed to obtain emulsion gel.

[0014] Preferably, in step S2:

[0015] The concentration of the phycocyanin solution is 0.5%–3% (w / v);

[0016] The volume ratio of phycocyanin solution to anhydrous ethanol is 1:3 to 1:10.

[0017] The rotary evaporator was operated at a temperature of 30°C and a rotation speed of 150 rpm.

[0018] The concentration of the phycocyanin nanoparticle solution A is 0.5% to 4.0% (w / v).

[0019] Preferably, in step S3:

[0020] The concentration of the concentrated sulfuric acid solution is 1–3.16 M, and the mass-to-volume ratio of starch to concentrated sulfuric acid solution is 1:5–1:20 (g / mL).

[0021] The water bath heating temperature is 30℃~50℃, the reaction time is 3~5 days, and the magnetic stirring speed is 100~500rpm.

[0022] Preferably, in step S3:

[0023] The centrifugation speed is 8000-12000 rpm, and the centrifugation time is 10-20 minutes;

[0024] The precipitate is washed with distilled water 5 to 20 times.

[0025] The concentration of starch nanocrystal solution B is 0.5%–4.0% (w / v).

[0026] Preferably, the volume ratio of solution A to solution B in step S4 is 4:1 to 1:3.

[0027] Preferably, in step S5, the high-speed shearing rate of the homogenizer is 9000-15000 rpm, and the time is 2-4 min.

[0028] Preferably, the volume fraction of soybean oil in step S5 includes 20%, 30%, 40%, 50%, 60%, 70%, 75%, and 80%.

[0029] Compared with the prior art, the beneficial effects of the present invention are:

[0030] This invention provides a method for preparing an emulsion gel based on a phycocyanin nanoparticle and starch nanocrystal complex, achieving a synergistic improvement in emulsion stability and gel structural strength, significantly enhancing the stability of the emulsion gel under storage, heating, acid-base changes, and ionic environments. Simultaneously, the complex forms a dense adsorption layer at the oil-water interface, effectively inhibiting oil droplet aggregation and oxidative degradation of active ingredients. The resulting emulsion gel is soft and lubricating, meeting the structural requirements of people with swallowing disorders for "smooth, easy-to-swallow, and low-irritation" foods. Furthermore, the materials used are natural, edible, and highly bioactive, and the preparation process is simple and controllable, showing promising prospects for industrial applications. Attached Figure Description

[0031] Figure 1 This is a schematic diagram of the droplet size of the composite stabilized emulsions prepared in Comparative Example 1, Comparative Example 2 and Example 1 of the present invention.

[0032] Figure 2 This is a schematic diagram showing the rheological test results of storage modulus and loss modulus in Embodiment 1 and Comparative Example 3 of the present invention. Detailed Implementation

[0033] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0034] Existing emulsions suffer from poor structural stability, weak environmental adaptability (such as sensitivity to temperature, acidity, alkali, and ions), and excessively viscous or loose texture. Therefore, this invention constructs an emulsion gel structure with good lubricity and oral adaptability based on the electrostatic and hydrogen bonding interactions between phycocyanin nanoparticles and starch nanocrystals. This provides a safe, nutritious, and texture-controllable food solution for people with swallowing disorders and has significant research and application value.

[0035] The methods for testing the properties of the complex and the physicochemical characteristics of the emulsion gel in the embodiments of the present invention are as follows:

[0036] Method for determining the droplet size of emulsions: The droplet size and distribution were determined using a laser particle size analyzer (Mastersizer 3000, Malvern Instruments Ltd., UK). The refractive indices of water and soybean oil were set to 1.33 and 1.45, respectively. Samples were diluted with distilled water to appropriate concentrations at the corresponding pH values, and measurements were taken immediately after dilution. Droplet size is expressed as volume average diameter (D). 4,3 )express.

[0037] Emulsion rheology determination method: using Kinexus Pro + The rheometer (Malvern Instruments Ltd.) is used to characterize rheological properties. Equipped with a 20mm parallel plate, a 1mm measurement gap, and frequency sweep testing (0.1-10 rad / s), it measures the storage modulus (G') and loss modulus (G") of the sample.

[0038] Example 1

[0039] Please see Figure 1 and 2 ,in Figure 1 D 4,3 "This represents the volume-average diameter of the milk droplets." Figure 2 The horizontal axis "angular frequency" is in "rad / s", and the vertical axis "G'" and "G" represent storage modulus and loss modulus (unit: Pa), respectively. This invention provides a technical solution: a method for preparing an easily swallowable emulsion gel using a phycocyanin nanoparticle-starch nanocrystal composite, comprising the following steps:

[0040] S1. Material preparation: Prepare phycocyanin, tapioca starch, distilled water and soybean oil;

[0041] S2. Preparation of phycocyanin nanoparticles A: Dissolve the phycocyanin from step S1 in distilled water to prepare a 2% (w / v) phycocyanin solution, and then quickly inject the solution into anhydrous ethanol, wherein the volume ratio of phycocyanin solution to anhydrous ethanol is 1:4 to obtain a phycocyanin nanoparticle solution.

[0042] Ethanol was removed by rotary evaporation of phycocyanin nanoparticle solution at a temperature of 30°C and a rotation speed of 150 rpm, resulting in a 2% (w / v) phycocyanin nanoparticle solution A.

[0043] S3. Preparation of starch nanocrystals B: The cassava starch from step S1 was added to a 3.16M concentrated sulfuric acid solution. The mass-to-volume ratio of cassava starch to concentrated sulfuric acid solution was 1:5 (g / mL). The reaction was carried out in a water bath with magnetic stirring. The water bath temperature was 40℃, the reaction time was 5 days, and the magnetic stirring speed was 200 rpm.

[0044] After the reaction was completed, the mixture was centrifuged at 8000 rpm for 10 minutes. The resulting precipitate was washed 10 times with distilled water to obtain a 2% (w / v) starch nanocrystal solution B.

[0045] S4. Preparation of mixed solution C: Add solution A from step S2 to solution B from step S3, with a volume ratio of solution A to B of 2:1, to obtain phycocyanin nanoparticle-starch nanocrystal mixed solution C.

[0046] S5. Obtaining the emulsion gel: Add soybean oil to the mixture C from step S4, with the soybean oil accounting for 75% of the total volume, and homogenize the mixture C with added soybean oil using a homogenizer with high-speed shearing. The high-speed shearing rate of the homogenizer is 13000 rpm, and the time is 3 min, to obtain the emulsion gel.

[0047] The emulsion prepared in Example 1 was gel-like. Droplet size testing results showed that the droplet size of the emulsion gel prepared using the phycocyanin nanoparticle-starch nanocrystal composite in this example was 34 μm. The emulsion gel was soft and smooth, exhibiting high stability, especially maintaining its gel-like state even after 14 days of storage. Its rheological test results (…) Figure 2 This indicates that the emulsion gel strength of this embodiment is significantly higher than that of the phycocyanin-starch emulsion gel prepared in Comparative Example 3. For example, the G' value of the emulsion gel in Example 1 is 500 Pa, while the G' value of the emulsion gel in Comparative Example 3 is 100 Pa.

[0048] Example 2

[0049] The difference from Example 1 is:

[0050] S2. Preparation of phycocyanin nanoparticles A: The concentration of solution A is 0.5% (w / v).

[0051] S3. Preparation of starch nanocrystals B: The concentration of solution B is 0.5% (w / v).

[0052] The emulsion prepared in Example 2 was in a fluid state. Droplet size testing results showed that the droplet size of the emulsion prepared using the phycocyanin nanoparticle-starch nanocrystal composite in this example was 84 μm, and the emulsion exhibited poor stability, showing severe stratification after 14 days of storage.

[0053] Example 3

[0054] The difference from Example 1 is:

[0055] S5. Prepare an emulsion gel: soybean oil accounts for 20% of the total volume.

[0056] The emulsion prepared in Example 3 was in a fluid state. Droplet size testing results showed that the droplet size of the emulsion prepared using the phycocyanin nanoparticle-starch nanocrystal composite in this example was 84 μm, and the emulsion exhibited extremely poor stability, showing stratification both fresh and after 14 days of storage.

[0057] Example 4

[0058] The difference from Example 1 is:

[0059] S4. Mixture: Add solution A from step S2 to solution B from step S3 in a volume ratio of 4:1.

[0060] S5. Prepare an emulsion gel: soybean oil accounts for 70% of the total volume.

[0061] The emulsion prepared in Example 4 was gel-like. Droplet size testing showed that the droplet size of the emulsion prepared using the phycocyanin nanoparticle-starch nanocrystal composite in this example was 63 μm, and the emulsion gel was soft, smooth, and easy to swallow. It exhibited good stability, remaining gel-like after 14 days of storage.

[0062] Example 5

[0063] The difference from Example 1 is:

[0064] Includes the following steps:

[0065] S1. Material preparation: Prepare phycocyanin, corn starch, distilled water and soybean oil;

[0066] S2. Preparation of phycocyanin nanoparticles A: Dissolve the phycocyanin from step S1 in distilled water to prepare a 1% (w / v) phycocyanin solution, and then quickly inject the solution into anhydrous ethanol, wherein the volume ratio of phycocyanin solution to anhydrous ethanol is 1:6 to obtain a phycocyanin nanoparticle solution.

[0067] Ethanol was removed from the phycocyanin nanoparticle solution by rotary evaporation at a temperature of 30°C and a rotation speed of 150 rpm, resulting in a 1% (w / v) phycocyanin nanoparticle solution A.

[0068] S3. Preparation of starch nanocrystals B: The corn starch from step S1 is added to a 1M concentrated sulfuric acid solution. The mass-to-volume ratio of corn starch to concentrated sulfuric acid solution is 1:10 (g / mL). The reaction is carried out in a water bath with magnetic stirring. The water bath temperature is 40℃, the reaction time is 4 days, and the magnetic stirring speed is 300 rpm.

[0069] After the reaction was completed, the sample was centrifuged at 9000 rpm for 15 minutes. The resulting precipitate was washed 10 times with distilled water to obtain a 1% (w / v) starch nanocrystal solution B.

[0070] S4. Mixture: Add solution A from step S2 to solution B from step S3, with a volume ratio of 1:1 between solutions A and B, to obtain a phycocyanin nanoparticle-starch nanocrystal mixture C.

[0071] S5. Obtaining the emulsion gel: Add soybean oil to the mixture C from step S4, with the soybean oil accounting for 75% of the total volume, and homogenize the mixture C with added soybean oil using a high-speed shear homogenizer. The high-speed shear rate of the homogenizer is 13000 rpm, and the time is 5 min, to obtain the emulsion gel.

[0072] The emulsion prepared in Example 5 was gel-like. Droplet size testing showed that the emulsion prepared using the phycocyanin nanoparticle-starch nanocrystal composite of this example had a strong gel network, with droplet size of 48 μm. The emulsion gel was soft and smooth, exhibiting high stability, and remained gel-like even after 14 days of storage.

[0073] Example 6

[0074] The difference from Example 1 is:

[0075] Includes the following steps:

[0076] S1. Material preparation: Prepare phycocyanin, potato starch, distilled water and soybean oil;

[0077] S2. Preparation of phycocyanin nanoparticles A: Dissolve the phycocyanin from step S1 in distilled water to prepare a 4% (w / v) phycocyanin solution. Then, quickly inject the solution into anhydrous ethanol, wherein the volume ratio of the phycocyanin solution to anhydrous ethanol is 1:10 to obtain a phycocyanin nanoparticle solution.

[0078] Ethanol was removed by rotary evaporation of the phycocyanin nanoparticle solution at a temperature of 30°C and a rotation speed of 150 rpm, resulting in a 4% (w / v) phycocyanin nanoparticle solution A.

[0079] S3. Preparation of starch nanocrystals B: Add the potato starch from step S1 to a 3M concentrated sulfuric acid solution. The mass-to-volume ratio of potato starch to concentrated sulfuric acid solution is 1:20 (g / mL). Heat the mixture in a water bath and stir it magnetically. The water bath temperature is 40℃, the reaction time is 5 days, and the magnetic stirring speed is 400 rpm.

[0080] After the reaction was completed, the sample was centrifuged at 12,000 rpm for 20 minutes. The resulting precipitate was washed 10 times with distilled water to obtain a 4% (w / v) starch nanocrystal solution B.

[0081] S4. Mixture: Add solution A from step S2 to solution B from step S3. The volume ratio of solution A to B is 1:3 to obtain a phycocyanin nanoparticle-starch nanocrystal mixture C.

[0082] S5. Obtaining the emulsion gel: Add soybean oil to the mixture C from step S4, with the soybean oil accounting for 80% of the total volume, and homogenize the mixture C with added soybean oil using a homogenizer with high-speed shearing. The high-speed shearing rate of the homogenizer is 15000 rpm, and the time is 2 min, to obtain the emulsion gel.

[0083] The emulsion prepared in Example 6 is gel-like. Droplet size testing results show that the emulsion prepared using the phycocyanin nanoparticle-starch nanocrystal composite of this example has a strong gel network, with droplet size of 38 μm. The emulsion gel is soft and smooth, easy to swallow, and highly stable, maintaining its gel-like state even after 14 days of storage.

[0084] Comparative Example 1

[0085] A method for preparing an emulsion using phycocyanin nanoparticles alone includes the following steps:

[0086] Phycocyanin was dissolved in distilled water, and then the solution was rapidly injected into anhydrous ethanol to obtain a phycocyanin nanoparticle solution. The ethanol was removed by rotary evaporation to obtain a phycocyanin nanoparticle solution with a concentration of 2%.

[0087] Soybean oil was added to the above phycocyanin nanoparticle solution, with the soybean oil accounting for 75% of the total volume. The mixture was then homogenized using a high-speed shear homogenizer to obtain an emulsion gel. The shear rate was 13,000 rpm, and the time was 3 min.

[0088] The emulsion prepared by Comparative Example 1 was gel-like. The droplet size results showed that the droplet size of the emulsion prepared using the phycocyanin nanoparticles in this comparative example was 42 μm, which is still larger than the droplet size in Example 1. The emulsion had poor softness but slightly high stability, and its gel state remained unchanged after 14 days of storage.

[0089] Comparative Example 2

[0090] A method for preparing an emulsion using individual starch nanocrystals includes the following steps:

[0091] Cassava starch was added to a 3.16M concentrated sulfuric acid solution and heated in a 40°C water bath with magnetic stirring at 200 rpm for 5 days. After the reaction was completed, the mixture was centrifuged, and the resulting precipitate was washed multiple times with distilled water to obtain a starch nanocrystal solution with a concentration of 2%.

[0092] Soybean oil was added to the above starch nanocrystal solution, with the oil comprising 75% of the total volume. The mixture was then homogenized using a high-speed shear homogenizer at a shear rate of 13000 rpm for 3 minutes to obtain an emulsion gel.

[0093] The emulsion prepared by Comparative Example 2 was gel-like. The droplet size results showed that the droplet size of the emulsion prepared using the starch nanocrystals in this comparative example was 285 μm. The emulsion exhibited extremely poor stability, showing stratification after 7 days of storage.

[0094] Comparative Example 3

[0095] Materials Preparation: Prepare phycocyanin, tapioca starch, distilled water, and soybean oil; Preparation of Mixture: Add phycocyanin and tapioca starch to distilled water and magnetically stir at room temperature to completely hydrate the solids, obtaining a mixture with phycocyanin content accounting for 40% of the total concentration; Water Bath Heating: Heat the obtained mixture in a water bath while stirring with a magnetic stirrer, then cool the heated solution to room temperature to obtain a phycocyanin-starch mixture; Emulsion Gel Preparation: Add soybean oil to the above phycocyanin-starch mixture at a volume ratio of 3:7, and homogenize the mixture with added soybean oil using a high-speed shear homogenizer to obtain an emulsion gel. The shear rate is 13000 rpm for 3 minutes.

[0096] The emulsion prepared by Comparative Example 3 was gel-like. Its rheological test results ( Figure 2 The results show that the gel strength of the emulsion prepared using the phycocyanin-starch composite in this comparative example is lower than that of the sample in Example 1. For example, the storage modulus (G') and loss modulus (G") of the emulsion in this comparative example are both lower than those of the emulsion gel prepared from dual nanoparticles in Example 1, indicating that its gel strength is relatively weak. Therefore, compared with amorphous phycocyanin-starch composite emulsifiers, the nanoparticle form of the phycocyanin-starch composite is more conducive to constructing a dense, high-quality gel system, and is more suitable for food processing applications.

[0097] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0098] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for preparing an easily swallowable emulsion gel using a phycocyanin nanoparticle-starch nanocrystal complex, characterized in that: Includes the following steps: S1. Material preparation: Prepare phycocyanin, starch, distilled water and soybean oil, wherein the starch includes tapioca starch, corn starch and potato starch; S2. Preparation of phycocyanin nanoparticles A: Dissolve the phycocyanin from step S1 in distilled water, and then quickly inject the solution into anhydrous ethanol to obtain a phycocyanin nanoparticle solution. Ethanol was removed from the phycocyanin nanoparticle solution by rotary evaporation to obtain phycocyanin nanoparticle solution A; S3. Preparation of starch nanocrystals B: Add the starch from step S1 to a concentrated sulfuric acid solution, heat in a water bath and stir magnetically to react; After the reaction was completed, the precipitate was centrifuged and washed with distilled water to obtain starch nanocrystal solution B. S4. Preparation of mixture C: Add solution A from step S2 to solution B from step S3 to obtain phycocyanin nanoparticle-starch nanocrystal mixture C; S5. Obtaining emulsion gel: Add soybean oil to the mixture C in step S4, and homogenize the mixture C with added soybean oil using a homogenizer at high speed to obtain emulsion gel.

2. The method for preparing an easily swallowable emulsion gel using phycocyanin nanoparticles-starch nanocrystals complex according to claim 1, characterized in that: In step S2: The concentration of the phycocyanin solution is 0.5%–3% (w / v); The volume ratio of phycocyanin solution to anhydrous ethanol is 1:3 to 1:

10. The rotary evaporator was operated at a temperature of 30°C and a rotation speed of 150 rpm. The concentration of the phycocyanin nanoparticle solution A is 0.5% to 4.0% (w / v).

3. The method for preparing an easily swallowable emulsion gel using phycocyanin nanoparticles-starch nanocrystals complex according to claim 1, characterized in that: In step S3: The concentration of the concentrated sulfuric acid solution is 1–3.16 M, and the mass-to-volume ratio of starch to concentrated sulfuric acid solution is 1:5–1:20 (g / mL). The water bath heating temperature is 30℃~50℃, the reaction time is 3~5 days, and the magnetic stirring speed is 100~500rpm.

4. The method for preparing an easily swallowable emulsion gel using phycocyanin nanoparticles-starch nanocrystals complex according to claim 1, characterized in that: In step S3: The centrifugation speed is 8000-12000 rpm, and the centrifugation time is 10-20 minutes; The precipitate is washed with distilled water 5 to 20 times. The concentration of starch nanocrystal solution B is 0.5%–4.0% (w / v).

5. The method for preparing an easily swallowable emulsion gel using phycocyanin nanoparticles-starch nanocrystals complex according to claim 1, characterized in that: In step S4, the volume ratio of solution A to solution B is 4:1 to 1:

3.

6. The method for preparing an easily swallowable emulsion gel using phycocyanin nanoparticles-starch nanocrystals complex according to claim 1, characterized in that: In step S5, the high-speed shearing rate of the homogenizer is 9000-15000 rpm, and the time is 2-4 min.

7. The method for preparing an easily swallowable emulsion gel using phycocyanin nanoparticles-starch nanocrystals complex according to claim 1, characterized in that: In step S5, the volume fraction of soybean oil in the total volume includes 20%, 30%, 40%, 50%, 60%, 70%, 75%, and 80%.

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