Preparation method of high-stability and slow-release flavor high-internal-phase emulsion

Abstract

The invention discloses a preparation method of a high-stability and slow-release flavor high-internal-phase emulsion, which comprises the following steps: removing visible fascia on fresh meat to obtain pretreated meat; mincing the pretreated meat, adding ionized water, stirring, centrifuging, and taking supernate, so as to obtain a myofibrillar protein crude extract; dialyzing the myofibrillar protein crude extract to obtain a purified myofibrillar protein solution; performing ultrahigh pressure treatment on the purified myofibrillar protein solution to obtain a target protein solution; preparing a flavor substance solution; mixing the flavor substance solution and the target protein solution according to a preset proportion to obtain a flavor protein emulsion; and mixing the flavor protein emulsion and edible oil according to a ratio, stirring or homogenizing, and fully mixing to obtain the flavor high internal phase emulsion. The high internal phase emulsion disclosed by the invention has good stability and a flavor slow-release function, can keep stable in food processing and storage processes, gradually releases flavor substances, and improves the flavor quality of food.

Description

Technical Field

[0001] This invention relates to the field of food processing technology, and in particular to a method for preparing a highly stable and slow-release flavor emulsion with a high internal phase. Background Technology

[0002] In meat processing, aldehydes, alcohols, ketones, esters, sulfur-containing compounds, and pyrazines are all important flavor components, typically possessing distinctive aromas that enhance the overall flavor quality of meat. However, during storage, the typical aromas of meat products easily dissipate, leading to a decline in product quality.

[0003] In the food industry, emulsions are widely used to improve the texture, mouthfeel, and flavor of food. However, traditional emulsion construction relies heavily on synthetic emulsifiers, which may pose safety risks and do not meet current consumer demands for clean-label foods. Furthermore, traditional emulsions perform poorly in flavor retention, with flavor compounds easily escaping and affecting the final flavor quality of the food.

[0004] High internal phase emulsions (HIPEs), as emulsion systems with an internal phase volume fraction exceeding 74%, possess unique physicochemical properties. However, current HIPE construction still primarily relies on synthetic emulsifiers. Therefore, there is an urgent need for a novel HIPE that does not depend on synthetic additives and possesses excellent flavor sustained-release capabilities. Summary of the Invention

[0005] This invention provides a method for preparing a highly stable and sustained-release flavorful high internal phase emulsion, thereby solving the technical problem of traditional emulsions relying on synthetic emulsifiers.

[0006] To address the aforementioned technical problems, in a first aspect, the present invention provides a method for preparing a highly stable and sustained-release flavor emulsion with a high internal phase, comprising the following steps: Step 1: Select fresh meat and remove the visible fascia from the fresh meat to obtain pre-treated meat; Step 2: After mincing the pre-treated meat with a meat grinder, add deionized water and stir. Then centrifuge and take the supernatant to obtain crude myofibrillar protein extract. Step 3: Dialyze the crude myofibrillar protein extract to remove small molecule impurities and obtain a purified myofibrillar protein solution. Step 4: The purified myofibrillar protein solution is placed into a vacuum packaging bag for vacuum packaging, and then subjected to ultra-high pressure treatment to obtain the target protein solution. Step 5: Dissolve the flavor substance to prepare a flavor substance solution; Step 6: Mix the flavor substance solution and the target protein solution in a preset ratio to obtain a flavor protein emulsion; Step 7: Mix the flavored protein emulsion with edible oil at a ratio of 75% to 90% of the internal phase volume fraction, stir or homogenize, and mix thoroughly to obtain a flavorful internal phase emulsion.

[0007] In some of these embodiments, the fresh meat includes one or more of chicken, pork, and beef.

[0008] In some of the embodiments, step 2 includes: mincing the pre-treated meat with a meat grinder, adding deionized water at a meat-to-water mass ratio of 1:(2~4), stirring and extracting at 2℃~6℃ for 1h~3h, centrifuging at 6000~10000r / min for 15min~30min, taking the supernatant to obtain crude myofibrillar protein extract.

[0009] In some embodiments, step 3 includes: dialyzing the crude myofibrillar protein extract with a NaCl solution of concentration of 0.4 mol / L to 0.8 mol / L for 20 h to 30 h to obtain a purified myofibrillar protein solution.

[0010] In some embodiments, step 4 includes: vacuum packaging the purified myofibrillar protein solution into a vacuum packaging bag, and then treating it under ultra-high pressure at a pressure of 150MPa~450MPa for 10min~20min to obtain the target protein solution.

[0011] In some embodiments, the flavor substances in step 5 include one or more of aldehydes, alcohols, ketones, esters, sulfur-containing compounds, and pyrazine compounds.

[0012] In some embodiments, step 5 includes: dissolving the flavor substance in anhydrous ethanol or an aqueous ethanol solution to a concentration of 0.1 mg / mL to 1 mg / mL to obtain a flavor substance solution.

[0013] In some embodiments, step 6 includes: mixing the flavor substance solution and the target protein solution at a volume ratio of 1:(5~20), and stirring at 2℃~6℃ at a stirring speed of 200r / min~500r / min for 12h~36h to obtain a flavor protein emulsion.

[0014] In some embodiments, the edible oil in step 7 includes one or more of soybean oil, corn oil, and sunflower oil.

[0015] In some embodiments, step 7 includes: mixing the flavored protein emulsion with edible oil at a ratio of 75% to 90% of the internal phase volume fraction, stirring at 8000 r / min to 12000 r / min for 3 min to 8 min, or homogenizing at a pressure of 40 MPa to 60 MPa for 2 min to 5 min, to obtain a flavorful internal phase emulsion.

[0016] Compared with the prior art, the present invention has the following beneficial effects: The high-flavor internal phase emulsion obtained by this invention uses myofibrillar protein treated under ultra-high pressure as a natural emulsifier, edible oil as the internal phase, and is directionally loaded with characteristic flavor substances, which makes the emulsion have good stability and flavor sustained-release function. It can remain stable during food processing and storage, and gradually release flavor substances to improve the flavor quality of food. Attached Figure Description

[0017] Figure 1 This is a sample image showing the multidimensional stability analysis results of a sucralose high internal phase emulsion according to an embodiment of the present invention; Figure 2 This is a diagram showing the flavor retention kinetics of furfural high internal phase emulsions according to an embodiment of the present invention; Figure 3 The microstructures and corresponding fluorescence staining images of high internal phase emulsions of 2-methyl-3-furanthiol at different concentrations are shown in the embodiments of the present invention. Figure 4 This is a graph showing the quenching constant results of the binding of 2-methyl-3-furanthiol to myofibrillar protein in an embodiment of the present invention; Figure 5 The diagram shows the thermodynamic parameters of the binding between 2-methyl-3-furanthiol and myofibrillar protein, as illustrated in an embodiment of the present invention. Detailed Implementation

[0018] To make the above-mentioned objects, features, and advantages of the present invention more apparent and understandable, specific embodiments of the present invention are described in detail below. Many specific details are set forth in the following description to provide a thorough understanding of the present invention. However, the present invention can be practiced in many other ways different from those described herein, and those skilled in the art can make similar modifications without departing from the spirit of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0019] As used herein, the terms “prepared from” and “comprising” are synonymous. The terms “comprising,” “including,” “having,” “containing,” or any other variations thereof, as used herein, are intended to cover non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that includes the listed elements is not necessarily limited to those elements, but may include other elements not expressly listed or elements inherent to such composition, step, method, article, or apparatus.

[0020] When a quantity, concentration, or other value or parameter is expressed as a range, a preferred range, or a range defined by a series of upper and lower preferred values, this should be understood as specifically disclosing all ranges formed by any pair of any upper or preferred value with any lower or preferred value, regardless of whether the range is disclosed individually. For example, when the range “1 to 5” is disclosed, the described range should be interpreted as including the ranges “1 to 4”, “1 to 3”, “1 to 2”, “1 to 2 and 4 to 5”, “1 to 3 and 5”, etc. When numerical ranges are described herein, unless otherwise stated, the range is intended to include its endpoints and all integers and fractions within that range.

[0021] Furthermore, the indefinite articles “a” and “an” preceding the elements or components of this invention do not impose any limitation on the quantity requirement (i.e., the number of times) of the elements or components. Therefore, “an” or “a” should be interpreted as including one or at least one, and the singular form of an element or component also includes the plural form, unless the quantity clearly refers to the singular form.

[0022] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0023] Example 1: Preparation of a furfural-flavored high internal phase emulsion Raw material preparation: Select 500g of fresh chicken breast, remove visible tendons and fat, mince it with a meat grinder, add deionized water at a meat-to-water ratio of 1:3, stir and extract at 4℃ for 2h, then centrifuge at 8000r / min for 20min, collect the supernatant to obtain crude myofibrillar protein extract; dialyze the crude myofibrillar protein extract with 0.6mol / L NaCl solution for 24h to obtain purified myofibrillar protein solution; Ultra-high pressure treatment: The purified myofibrillar protein solution was placed into a vacuum packaging bag for vacuum packaging, and then treated with ultra-high pressure at 150 MPa for 20 min to obtain the target protein solution; Preparation of flavor substance solution: using furfural as a flavor substance, it was dissolved in anhydrous ethanol to prepare a flavor substance solution with a concentration of 0.5 mg / mL; Preparation of flavor protein emulsion: The flavor substance solution and the target protein solution were mixed at a volume ratio of 1:18 and stirred at 4℃ for 16 hours at a stirring speed of 200r / min~500r / min to obtain a glucuronid-myofibrillar protein emulsion.

[0024] Preparation of flavor-rich internal phase emulsion: Flavor protein emulsion and soybean oil were mixed at an internal phase volume fraction of 85% and stirred at 12000 r / min for 3 min to obtain a sucralose high internal phase emulsion.

[0025] 1.1 Stability characterization: The uronic acid high internal phase emulsion was dispensed into sealed glass bottles and stored at 37°C for 30 days. Samples were taken on days 1, 3, 7, 15, and 30 to evaluate its storage stability (A), centrifugal stability (B), heating stability (C), and freeze-thaw stability (D).

[0026] like Figure 1 As shown in Part A (30-day room temperature storage), no oil phase precipitation or aqueous phase sedimentation occurred in any of the emulsion groups during storage, and the interface integrity remained good. In Part B (centrifugal stability), the liquid column height of each emulsion group remained stable after high-speed centrifugation, and no significant phase separation occurred. In Part C (80℃ heating stability), no flocculation or demulsification occurred in any of the three emulsion groups under high temperature conditions, and the interfacial viscoelasticity was not significantly affected, reflecting that the myofibrillar protein emulsions treated differently all possessed good thermal stability under the conditions. In Part D (-20℃ freeze-thaw cycle), the droplet distribution uniformity of each emulsion group did not change significantly after multiple freeze-thaw cycles. Therefore, the flavorful high internal phase emulsion obtained by this invention exhibits good stability characteristics in long-term storage, mechanical stress, and thermal and low-temperature environments, meeting the basic requirements of the food industry for the stability of emulsion products.

[0027] 1.2 Characterization of sustained release: The concentration of free uronic acid in the sealed glass bottle high internal phase emulsion was collected by headspace solid phase microextraction-gas chromatography-mass spectrometry on days 0, 7, 15 and 30 for quantitative analysis. Flavor kinetics was studied based on flavor binding rate and flavor retention rate.

[0028] like Figure 2 As shown, furfural exhibits excellent binding performance in the high internal phase emulsion during the initial preparation stage, with a binding rate reaching 84.40%. The flavor release of furfural in the system displays a kinetic characteristic of "rapid initial release followed by slower release": in the early storage stage (0-7 days), the flavor retention rate rapidly decreases to 51.60%, and the release rate constant... (Half-life 15.4 days) During the middle of storage (7-15 days), the decline in HIPE flavor retention slowed significantly, with the flavor retention decreasing from 51.60% to 36.72%. During the later stage of storage (15-30 days), the HIPE flavor retention only decreased slightly from 36.72% to 32.89%, indicating that this high internal phase emulsion has a significant flavor sustained-release effect.

[0029] Example 2: Preparation of 2-methyl-3-furanthiol high internal phase emulsion Raw material preparation: Select 500g of fresh pork, remove visible fascia and fat, mince it with a meat grinder, add deionized water at a meat-to-water ratio of 1:2, stir and extract at 4℃ for 3h, then centrifuge at 10000r / min for 10min, collect the supernatant to obtain crude myofibrillar protein extract; dialyze the crude myofibrillar protein extract with 0.6mol / L NaCl solution for 24h to obtain purified myofibrillar protein solution; Ultra-high pressure treatment: The purified myofibrillar protein solution was placed into a vacuum packaging bag for vacuum packaging, and then treated with ultra-high pressure at 300 MPa for 20 min to obtain the target protein solution. Preparation of flavor substance solution: 2-methyl-3-furanthiol was used as the flavor substance and dissolved in anhydrous ethanol to prepare a flavor substance solution with a concentration of 0.4 mg / mL; Preparation of flavor protein emulsion: The flavor substance solution and the target protein solution were mixed at a volume ratio of 1:10 and stirred at 4℃ at a stirring speed of 200r / min~300r / min for 20h to obtain 2-methyl-3-furanthiol-myofibrillar protein emulsion.

[0030] Preparation of flavor-rich internal phase emulsion: Flavor protein emulsion and sunflower seed oil were mixed at an internal phase volume fraction of 80%, and stirred at 10000 r / min for 3 min to obtain 2-methyl-3-furanthiol high internal phase emulsion.

[0031] 2.1 Characterization of 2-methyl-3-furanthiol high internal phase emulsion: such as Figure 3 As shown, ultra-high pressure treatment has a significant regulatory effect on the Ka and n values ​​of the myofibrillar protein-2-methyl-3-furanthiol system; simultaneously, as Figure 4 As shown, thermodynamic parameters indicate that high internal phase emulsions can achieve stable binding of the 2-methyl-3-furanthiol flavor; such as Figure 5 As shown, this high internal phase emulsion has a good microstructure and obvious boundaries.

[0032] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0033] The specific embodiments described above further illustrate the purpose, technical solution, and beneficial effects of the present invention. It should be understood that the above descriptions are merely specific embodiments of the present invention and are not intended to limit the scope of protection of the present invention. In particular, it should be noted that any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention for those skilled in the art.

Claims

1. A process for the preparation of a high stability and slow release flavor high internal phase emulsion characterized in that, The method comprises the following steps: Step 1, selecting fresh meat and removing visible fascia on the fresh meat to obtain pretreated meat; Step 2, grinding the pretreated meat with a meat grinder, adding ionized water for stirring, and then centrifuging to obtain supernatant to obtain a myofibrillar protein crude extract; Step 3, dialyzing the myofibrillar protein crude extract to remove small molecular impurities to obtain a purified myofibrillar protein solution; Step 4, vacuum packaging the purified myofibrillar protein solution in a vacuum packaging bag, and then performing ultrahigh pressure treatment to obtain a target protein solution; Step 5, dissolving flavoring substances to prepare a flavoring substance solution; Step 6, mixing the flavoring substance solution and the target protein solution according to a preset ratio to obtain a flavoring protein emulsion; Step 7, mixing the flavoring protein emulsion and edible oil according to an inner phase volume fraction of 75% to 90%, stirring or homogenizing, and fully mixing to obtain a flavoring high internal phase emulsion.

2. The process for preparing high stability and slow release flavor high internal phase emulsion according to claim 1, characterized in that, The fresh meat comprises one or more of chicken, pork and beef.

3. The method for preparing a highly stable and sustained-release flavorful high-internal-phase emulsion as described in claim 1, characterized in that, The step 2 comprises the following steps: after the pretreated meat is ground with a meat grinder, deionized water is added in a meat-to-water mass ratio of 1: (2-4), stirring extraction is performed at 2-6 DEG C for 1-3 hours, centrifugation is performed at a speed of 6000-10000 r / min for 15-30 minutes, and the supernatant is taken to obtain the myofibrillar protein crude extract.

4. The process for preparing high stability and slow release flavor high internal phase emulsion according to claim 1, characterized in that, The step 3 comprises the following step: the myofibrillar protein crude extract is dialyzed with a NaCl solution with a concentration of 0.4-0.8 mol / L for 20-30 hours to obtain the purified myofibrillar protein solution.

5. The method for preparing a highly stable and sustained-release flavorful high-internal-phase emulsion as described in claim 1, characterized in that, The step 4 comprises the following steps: the purified myofibrillar protein solution is vacuum packaged in a vacuum packaging bag, and then ultrahigh pressure treatment is performed at a pressure of 150-450 MPa for 10-20 minutes to obtain the target protein solution.

6. The method for preparing a highly stable and sustained-release flavorful high-internal-phase emulsion as described in claim 1, characterized in that, The flavoring substances in the step 5 comprise one or more of aldehydes, alcohols, ketones, esters, sulfur-containing compounds and pyrazine compounds.

7. The process for preparing high stability and slow release flavor high internal phase emulsion according to claim 1, characterized in that, The step 5 comprises the following step: the flavoring substances are dissolved in anhydrous ethanol or an ethanol aqueous solution to a concentration of 0.1-1 mg / mL to obtain the flavoring substance solution.

8. The process for preparing high stability and slow release flavor high internal phase emulsion according to claim 1, characterized in that, The step 6 comprises the following steps: the flavoring substance solution and the target protein solution are mixed according to a volume ratio of 1: (5-20), stirring is performed at a stirring speed of 200-500 r / min at 2-6 DEG C for 12-36 hours to obtain the flavoring protein emulsion.

9. The process for preparing high stability and slow release flavor high internal phase emulsion according to claim 1, characterized in that, The edible oil in the step 7 comprises one or more of soybean oil, corn oil and sunflower seed oil.

10. The process for preparing high stability and slow release flavor high internal phase emulsion according to claim 1, characterized in that, The step 7 comprises the following steps: after the flavoring protein emulsion and the edible oil are mixed according to an inner phase volume fraction of 75% to 90%, stirring is performed at a speed of 8000-12000 r / min for 3-8 minutes or homogenization is performed at a pressure of 40-60 MPa for 2-5 minutes to obtain the flavoring high internal phase emulsion.

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