Method for preparing emulsion gels using phycocyanin-starch complex emulsifiers

Abstract

The present application relates to the technical field of emulsion gel preparation, in particular to a method for preparing emulsion gel by using phycocyanin-starch composite emulsifier, comprising the following steps: preparing phycocyanin, starch, distilled water and soybean oil; adding phycocyanin and starch into distilled water, stirring at room temperature to obtain a mixed solution; heating the mixed solution in a water bath, and cooling to room temperature to obtain phycocyanin-starch composite emulsifier; finally, adding soybean oil and shearing homogeneously at high speed to obtain emulsion gel. The present application provides a method for preparing emulsion gel by using phycocyanin as raw material, which has the characteristics of environmental protection, sustainability, natural source, high nutritional value and antioxidant activity. The application range of protein is expanded, and phycocyanin and starch are compounded through hydrogen bond and hydrophobic interaction. The emulsion gel has excellent storage stability and environmental stress resistance, and is edible. The preparation method is novel and simple, and easy to realize industrial production, which is suitable for food industry.

Description

TECHNICAL FIELD

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

[0002] An emulsion gel is a semi-solid substance formed by the dispersion of droplets in a three-dimensional network structure, with excellent rheological properties and thermodynamic stability, and is widely used in food and drug delivery systems. The preparation of emulsion gel usually requires emulsifiers and stabilizers to ensure uniform dispersion of droplets and structural stability.

[0003] Phycocyanin, as a natural pigment and protein, has attracted much attention due to its antioxidant, anti-inflammatory and immunomodulatory activities, as well as its safety and sustainability, and has become a potential animal-derived protein substitute, widely used in food, cosmetics and pharmaceuticals. Starch is a cheap and abundant natural polysaccharide with good biocompatibility and biodegradability, widely used in food and pharmaceuticals.

[0004] However, the existing technology in preparing gels, at present, the commonly used preparation method of emulsion gel includes adding crosslinking agent in water phase or preparing emulsion first and then secondary gel, but these processes are usually more cumbersome, and the emulsion stabilized by phycocyanin and starch alone often has limitations, is easily affected by external environmental factors such as high temperature, pH value and high ionic strength, and the gel strength is not high. SUMMARY

[0005] The purpose of the present application is to provide a method for preparing an emulsion gel using phycocyanin-starch complex emulsifier, to solve the problems of cumbersome preparation process, easy influence by external environmental factors such as high temperature, pH value and high ionic strength, and low gel strength.

[0006] To achieve the above-mentioned purpose, the present application provides the following technical scheme: a method for preparing an emulsion gel using phycocyanin-starch complex emulsifier, comprising the following steps:

[0007] S1, material preparation: preparing phycocyanin, starch, distilled water and soybean oil, wherein the starch includes but is not limited to tapioca starch, corn starch and potato starch;

[0008] S2, preparation of mixed solution: adding phycocyanin and starch in step S1 into distilled water, and performing magnetic stirring at room temperature to make the solids completely hydrated, to obtain a mixed solution;

[0009] S3, water bath heating: heating the mixed solution obtained in step S2 in a water bath, while stirring by a magnetic stirrer, and then cooling the solution after water bath heating to room temperature to obtain a phycocyanin-starch mixed solution;

[0010] S4, preparing emulsion gel: adding soybean oil into the phycocyanin-starch mixture in step S3, and homogenizing the phycocyanin-starch mixture with soybean oil by using a homogenizer to obtain an emulsion gel.

[0011] Preferably, the total solid content of phycocyanin and starch in step S2 is 3-5% of the mixture, and the content of phycocyanin is 5%-40% of the total solid content in the mixture.

[0012] Preferably, the temperature of water bath heating in step S3 is 70-90°C, the heating time is 10-40 min, the stirring rate of the magnetic stirrer in step S3 is 300-500 rpm, and the cooling time is 0.5-2 h.

[0013] Preferably, the high-speed shearing rate of the homogenizer in step S4 is 9000-15000 r / min, and the time is 2-4 min.

[0014] Preferably, the volume ratio of phycocyanin-starch mixture to soybean oil in step S4 includes but is not limited to 8:2, 7:3, 6:4, 5:5, 4:6, 3:7 and 2:8.

[0015] Compared with the prior art, the present application has the following advantages:

[0016] 1. The present application uses phycocyanin as raw material and provides a preparation method of emulsion gel, which has the characteristics of environmental protection, natural source, high nutritional value, bright color and antioxidant activity, and expands the application range of protein. The phycocyanin and starch are compounded by hydrogen bond and hydrophobic interaction, the prepared emulsion gel has excellent storage stability and environmental stress stability, and is edible. The preparation method is novel and simple, easy to realize industrialized production, and suitable for food industry. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 The figure shows the stable emulsion droplet particle size of the composite emulsifier prepared in the present application comparative example one, comparative example two and example one. DETAILED DESCRIPTION

[0018] The technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.

[0019] In the embodiments of the present application, the test methods for the properties of the composite emulsifier and the physicochemical properties of the emulsion gel are as follows:

[0020] Droplet size measurement method: The emulsion droplet size and distribution were measured by a laser particle size analyzer (Mastersizer 3000, Malvern Instruments Ltd., UK) with a refractive index of 1.095. The samples were diluted to 1 wt% concentration with distilled water at the corresponding pH value and measured immediately after preparation. The droplet size measurement was calculated as the mean volume diameter value (D 4,3 ).

[0021] Anti-environmental stress test: ion strength, during the preparation of the emulsion gel, different molar concentrations of sodium chloride (50 mM, 100 mM, 200 mM, 300 mM and 500 mM) were added to the aqueous phase; pH, before the preparation of the emulsion gel, the pH of the aqueous phase was adjusted to 3.0, 5.0, 7.0, 9.0 and 11.0; high temperature, the prepared emulsion was heated in a water bath at 50℃, 60℃, 70℃, 80℃ and 90℃, respectively.

[0022] Example one

[0023] See Figure 1 , the present application provides a technical solution: using phycocyanin-starch complex emulsifier to prepare emulsion gel, comprising the following steps:

[0024] S1, material preparation: prepare phycocyanin, cassava starch, distilled water and soybean oil;

[0025] S2, preparation of mixed solution: phycocyanin and cassava starch are added to distilled water, and magnetic stirring is carried out at room temperature for 10 min to make the solid completely hydrated, and the mixed solution is obtained, wherein the total solid content of phycocyanin and cassava starch is 5% of the mixed solution, and the content of phycocyanin accounts for 40% of the total solid content in the mixed solution;

[0026] S3, water bath heating: the mixed solution obtained in step S2 is heated in a water bath, the temperature is 90℃, the heating time is 30 min, at the same time, the magnetic stirrer is stirred, and the stirring rate is 300 rpm, then the solution after water bath heating is cooled to room temperature for 1h, and the phycocyanin-starch mixed solution is obtained;

[0027] S4, preparation of emulsion gel: soybean oil is added to the phycocyanin-starch mixed solution in step S3, the volume ratio of phycocyanin-starch mixed solution to soybean oil is 3:7, and the phycocyanin-starch mixed solution with soybean oil is treated by high-speed shearing homogenizer to obtain emulsion gel, the shearing rate is 13000r / min, and the time is 3min.

[0028] The emulsion gel prepared by the example one has the emulsion particle size test result that the droplet particle size of the emulsion gel prepared by using the phycocyanin-starch composite emulsifier of the example is 108 μm, and the particle size distribution is uniform, the emulsion stability is high, and the emulsion still maintains the gel state after being stored for 42 days.

[0029] Example two

[0030] Different from the example one is that:

[0031] S2, preparing a mixed solution: the content of phycocyanin accounts for 10% of the total solid content in the mixed solution.

[0032] The emulsion gel prepared by the example two has the emulsion particle size test result that the droplet particle size of the emulsion gel prepared by using the phycocyanin-starch composite emulsifier of the example is 178 μm, and the particle size distribution is uniform, the emulsion stability is slightly high, and the emulsion loses the gel characteristics after being stored for 42 days.

[0033] Example three

[0034] Different from the example one is that:

[0035] S2, preparing a mixed solution: the content of phycocyanin accounts for 5% of the total solid content in the mixed solution.

[0036] S4, preparing an emulsion gel: the volume ratio of the phycocyanin-starch mixed solution to soybean oil is 4:6.

[0037] The emulsion gel prepared by the example three has the emulsion particle size test result that the droplet particle size of the emulsion gel prepared by using the phycocyanin-starch composite emulsifier of the example is 406 μm, and the particle size distribution is uniform, the emulsion stability is poor, the emulsifier is insufficient to cover the oil-water interface, and the stratification phenomenon appears after being stored.

[0038] Example four

[0039] Different from the example one is that:

[0040] Including the following steps:

[0041] S1, material preparation: preparing phycocyanin, corn starch, distilled water and soybean oil;

[0042] S2, preparing a mixed solution: adding phycocyanin and corn starch into distilled water, and performing magnetic stirring for 10 min at room temperature to make the solids completely hydrated, to obtain a mixed solution, wherein the total solid content of phycocyanin and corn starch is 3% of the mixed solution, and the content of phycocyanin accounts for 40% of the total solid content in the mixed solution;

[0043] S3, water bath heating: the mixed solution obtained in step S2 is subjected to water bath heating, the temperature is 70℃, the heating time is 20 min, at the same time, the magnetic stirrer is stirred, and the stirring rate is 300 rpm, then the solution after water bath heating is cooled to room temperature for 1 h, to obtain a phycocyanin-starch mixed solution;

[0044] S4, preparing emulsion gel: soybean oil is added to the phycocyanin-starch mixed solution in step S3, the volume ratio of the phycocyanin-starch mixed solution to the soybean oil is 3:7, and the phycocyanin-starch mixed solution with the added soybean oil is subjected to high-speed shearing homogenization treatment by a homogenizer to obtain an emulsion gel, the shearing rate is 13000 r / min, and the time is 3 min.

[0045] The emulsion gel prepared by Example Four has a droplet size of 208 μm, and the particle size distribution is uniform, and the emulsion stability is high.

[0046] Example Five

[0047] Different from Example One is that:

[0048] comprising the following steps:

[0049] S1, material preparation: preparing phycocyanin, potato starch, distilled water and soybean oil;

[0050] S2, preparing mixed solution: adding phycocyanin and potato starch into distilled water, and stirring by a magnetic stirrer at room temperature for 10 min to make the solids completely hydrated to obtain a mixed solution, wherein the total solid content of phycocyanin and potato starch is 5% of the mixed solution, and the content of phycocyanin accounts for 40% of the total solid content in the mixed solution;

[0051] S3, water bath heating: the mixed solution obtained in step S2 is subjected to water bath heating, the temperature is 70℃, the heating time is 20 min, at the same time, the magnetic stirrer is stirred, and the stirring rate is 300 rpm, then the solution after water bath heating is cooled to room temperature for 1 h, to obtain a phycocyanin-starch mixed solution;

[0052] S4, preparing emulsion gel: soybean oil is added to the phycocyanin-starch mixed solution in step S3, the volume ratio of the phycocyanin-starch mixed solution to the soybean oil is 3:7, and the phycocyanin-starch mixed solution with the added soybean oil is subjected to high-speed shearing homogenization treatment by a homogenizer to obtain an emulsion gel, the shearing rate is 13000 r / min, and the time is 3 min.

[0053] The emulsion gel prepared by the example five has the emulsion particle size test result that the droplet particle size of the emulsion gel prepared by using the phycocyanin-starch composite emulsifier of the example is 191 μm, and the droplet particle size distribution is uniform, and the emulsion stability is high.

[0054] Example six

[0055] The method comprises the following steps:

[0056] S1, material preparation: preparing phycocyanin, cassava starch, distilled water and soybean oil;

[0057] S2, preparation of mixed solution: adding phycocyanin and cassava starch into distilled water, and magnetically stirring at room temperature for 10 min to completely hydrate the solid, to obtain a mixed solution, wherein the total solid content of phycocyanin and cassava starch is 5% of the mixed solution, and the content of phycocyanin accounts for 40% of the total solid content in the mixed solution;

[0058] S3, water bath heating: heating the mixed solution obtained in step S2 in a water bath, the temperature is 90℃, and the heating time is 30 min, while stirring by a magnetic stirrer at a speed of 300 rpm, and then cooling the solution to room temperature for 1 h to obtain a phycocyanin-starch mixed solution;

[0059] S4, preparation of emulsion gel: adding soybean oil into the phycocyanin-starch mixed solution in step S3, and the volume ratio of the phycocyanin-starch mixed solution to the soybean oil is 2:8, and then homogenizing the phycocyanin-starch mixed solution with the added soybean oil by a high-speed shearing homogenizer to obtain an emulsion gel, the shearing speed is 15000 r / min, and the time is 4 min.

[0060] The emulsion gel prepared by the example six has the emulsion particle size test result that the droplet particle size of the emulsion gel prepared by using the phycocyanin-starch composite emulsifier of the example is 134 μm, and the droplet particle size distribution is uniform, and the emulsion stability is higher.

[0061] Comparative example one

[0062] A method for preparing an emulsion by using phycocyanin alone, comprising the following steps:

[0063] Adding phycocyanin into distilled water, and magnetically stirring at room temperature for 10 min to completely hydrate the solid, to obtain a mixed solution, wherein the total solid content of phycocyanin is 5% of the mixed solution;

[0064] Heating the above mixed solution in a water bath, the temperature is 90℃, and the heating time is 30 min, while magnetically stirring at a speed of 300 rpm, and then cooling the solution to room temperature for 1 h to obtain a phycocyanin mixed solution;

[0065] The soybean oil was added to the phycocyanin mixture, and the volume ratio of the water phase of the phycocyanin mixture to the oil phase of the soybean oil was 3:7. The phycocyanin mixture to which the soybean oil was added was subjected to high-speed shearing homogenization treatment by using a homogenizer to obtain an emulsion gel, and the shearing rate was 13000 r / min and the time was 3 min.

[0066] The emulsion gel prepared by Comparative Example 2 had a droplet size of 784 μm, and the droplet size was too large, and the emulsion stability was poor.

[0067] Comparative Example 2

[0068] A method for preparing an emulsion using cassava starch alone, comprising the following steps:

[0069] The cassava starch was added to distilled water, and magnetic stirring was performed at room temperature for 10 min to completely hydrate the solid, to obtain a mixture, wherein the total solid content of the cassava starch was 5% of the mixture;

[0070] The above mixture was heated in a water bath, the temperature was 90°C, the heating time was 30 min, and magnetic stirring was performed at the same time, the stirring rate was 300 rpm, and then the solution was cooled to room temperature for 1 h to obtain a cassava starch mixture;

[0071] The soybean oil was added to the cassava starch mixture, and the volume ratio of the water phase of the cassava starch mixture to the oil phase of the soybean oil was 3:7. The cassava starch mixture to which the soybean oil was added was subjected to high-speed shearing homogenization treatment by using a homogenizer to obtain an emulsion gel, and the shearing rate was 13000 r / min and the time was 3 min.

[0072] The emulsion gel prepared by Comparative Example 2 had a droplet size of 784 μm, and the droplet size was too large, and the emulsion stability was poor.

[0073] The emulsion state of Comparative Example 1, Comparative Example 2, Example 1 and Example 2 at different periods is shown in Table 1

[0074] Table 1: Emulsion state of Comparative Example 1, Comparative Example 2, Example 1 and Example 2 at different periods

[0075]

[0076] The emulsion gel prepared by Comparative Example 2 had a droplet size of 784 μm, and the droplet size was too large, and the emulsion stability was poor. Figure 1As shown in Table 1, the phycocyanin-starch complex emulsifier prepared in Example 1 has better performance, and has significant advantages in emulsion stability and particle size control. The emulsion has smaller and uniformly distributed droplet size, which greatly improves the stability of the emulsion or emulsion gel. Therefore, the emulsion gel with smaller emulsion droplet size, simple preparation process and significantly improved storage stability is of great significance for the design and realization of active substance food functionalization. The present application uses phycocyanin as raw material, which has the characteristics of environmental protection, sustainability, natural source, high nutritional value, bright color, antioxidant activity and the like, and expands the application range of protein. The phycocyanin and starch are complexed by hydrogen bond and hydrophobic interaction, which is a safe and non-toxic method for improving the stability of emulsion or emulsion gel.

[0077] The emulsion gel environmental stress resistance test table in Example 6 is shown in Table 2:

[0078] Table 2: Emulsion gel environmental stress resistance test table in Example 6

[0079]

[0080] As shown in Table 2, the phycocyanin-starch complex emulsifier emulsion gel prepared in Example 1 has significantly enhanced stability under environmental stress (such as pH change, high temperature and ionic strength). Its smaller droplet structure enables it to efficiently deliver nutrients and improve the absorption efficiency of hydrophobic bioactive substances. Therefore, the complex emulsifier emulsion gel can be used as a new type of nutrient delivery carrier and widely applied in the fields of nutrient delivery, drug controlled release and bioactive substance stabilization, thereby promoting the application of protein in scientific research and food industry.

[0081] It should be noted that, in this document, relational terms such as first and second and the like can be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises", "comprising", or any other variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but can include other elements not expressly listed or inherent to such process, method, article, or apparatus.

[0082] Although embodiments of the present application have been shown and described, it is to be understood that various modifications, substitutions, replacements and changes can be made to these embodiments without departing from the principles and spirit of the present application, and the scope of the present application is defined by the appended claims and their equivalents.

Claims

1. A method for preparing emulsion gels using phycocyanin-starch composite emulsifiers, characterized in that, Includes the following steps: S1. Material preparation: Prepare phycocyanin, starch, distilled water and soybean oil, where the starch can be tapioca starch, corn starch or potato starch. S2. Preparation of the mixture: Add the phycocyanin and starch from step S1 to distilled water and stir magnetically at room temperature to completely hydrate the solids and obtain the mixture. The total solid content of phycocyanin and starch is 3% to 5% of the mixture, and the content of phycocyanin accounts for 40% of the total solid content in the mixture. S3. Water bath heating: The mixture obtained in step S2 is heated in a water bath at a temperature of 70℃~90℃ for 10~40min, while being stirred with a magnetic stirrer at a speed of 300~500rpm. The cooling time is 0.5~2h. After that, the solution heated in the water bath is cooled to room temperature to obtain a phycocyanin-starch mixture. S4. Obtaining the emulsion gel: Add soybean oil to the phycocyanin-starch mixture in step S3, and homogenize the phycocyanin-starch mixture with added soybean oil using a homogenizer at a high speed of shearing to obtain the emulsion gel. The high speed of shearing in the homogenizer is 9000-15000 r / min, and the time is 2-4 min. The volume ratio of phycocyanin-starch mixture to soybean oil is 8:2, 3:7, or 2:8.

Images