Fish gelatin cake and method of making same
Patent Information
- Application Number
- CN202611455054.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-09-18
- Publication Date
- 2026-10-30
AI Technical Summary
[0004]然而上述现有技术在高温高压下处理存在不稳定因素,比如鱼鳔中的胶原蛋白易发生过度热变性,同时蛋白质还可能与还原糖(如天然鱼鳔胶中所含有的葡萄糖、果糖等或在酶解过程中多糖水解产生的葡萄糖、果糖等)发生美拉德反应而产生明显的腥味、焦苦味等异味,并且鱼鳔本身固有的腥味也较难去除,不良口感影响患者体验,依从性较差
(1)本发明采用“溶剂提取+酶解”相结合的工艺,在保证鱼鳔胶原蛋白提取率的同时,改善了鱼鳔胶的风味、口感等,还提高了有效成分的稳定性;
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of health food technology and provides a fish gelatin cake and its preparation method. Background Technology
[0002] Fish maw glue, also known as fish glue or fish belly glue, is a traditional gelatinous product made from the swim bladders of large fish (such as yellow croaker, sturgeon, large yellow croaker, and beluga sturgeon) through processes including cleaning, drying, boiling, concentration, and molding. Fish maw glue is sweet in taste and neutral in nature, entering the kidney and liver meridians. It has the effects of tonifying the kidneys and replenishing essence, nourishing yin and blood, stopping bleeding and dispersing blood stasis, and consolidating essence and reducing urination. It is one of the important medicinal materials for nourishing yin and blood in traditional Chinese medicine. Modern nutritional and medical research has further confirmed that fish maw glue is rich in collagen, various amino acids, vitamins, and minerals such as iron, calcium, and phosphorus. These nutrients give it a unique advantage in the field of blood replenishment. In addition to its blood replenishment effects, fish maw glue also has multiple effects such as tonifying the kidneys and replenishing essence, moistening the lungs and relieving cough, and promoting wound healing. It is often combined with longan, red dates, and walnuts to make a winter tonic, occupying an important position in the field of health preservation.
[0003] Chinese invention patent CN116746668B discloses a compound fish maw gelatin and its preparation method. The raw materials include: dried fish maw gelatin, angelica sinensis, rehmannia glutinosa, chuanxiong rhizome, astragalus membranaceus, white peony root, codonopsis pilosula, longan pulp, jujube, wolfberry, and licorice. First, the dried fish maw gelatin is soaked, boiled, and then soaked in acetic acid solution. After washing and high-temperature, high-pressure treatment, it is homogenized, high-pressure homogenized, filtered, and centrifuged to obtain the fish maw gelatin. The remaining components are used as excipients, mixed, boiled, filtered, and then mixed with the fish maw gelatin. The mixture is evaporated, concentrated, and dried to obtain the compound fish maw gelatin. This compound fish maw gelatin product is rich in protein and polysaccharides, has a good taste and iron chelating activity, can significantly increase the body weight of anemic rats, restore hemoglobin levels, and improve symptoms of hepatic sinusoidal disorders and blurred hepatocyte boundaries.
[0004] However, the aforementioned existing technologies have instability factors when processed under high temperature and pressure. For example, the collagen in fish maw is prone to excessive heat denaturation. Simultaneously, proteins may undergo Maillard reactions with reducing sugars (such as glucose and fructose contained in natural fish maw gelatin or glucose and fructose produced during polysaccharide hydrolysis during enzymatic hydrolysis), producing noticeable fishy, burnt, or bitter odors. Furthermore, the inherent fishy smell of fish maw itself is difficult to remove, and the unpleasant taste affects patient experience and reduces compliance. Heat-sensitive components in fish maw, such as hemolymph-replenishing polypeptides, sulfated polysaccharides, and iron-binding proteins, are largely inactivated during traditional high-temperature, long-term boiling, thus affecting their hemolymph-replenishing effects.
[0005] Considering the various defects of existing fish maw glue products, such as poor odor or sensory evaluation, inactivation of effective components during preparation, and insufficient blood-replenishing function, it is still necessary to optimize the preparation process of fish maw glue or improve the compounding of components to improve the overall performance of fish maw glue products. Summary of the Invention
[0006] To address the problems existing in the prior art, this invention provides a fish gelatin cake and its preparation method. The fish gelatin cake has the characteristics of good taste and good stability. In addition, when combined with jujube, longan, sunflower seed kernels, pumpkin seed kernels, etc., it has significant blood-nourishing effects and excellent comprehensive performance.
[0007] Terminology Explanation: Unless otherwise defined, all technical terms used herein have the same meanings as commonly understood by one of ordinary skill in the art to which this subject matter pertains. Unless otherwise stated, all patents, patent inventions, and disclosures cited throughout this document are incorporated herein by reference in their entirety. Where multiple definitions exist for terms herein, the definitions provided in this chapter shall prevail.
[0008] It should be understood that the above brief description and the following detailed description are exemplary and for illustrative purposes only, and do not limit the subject matter of the invention in any way. In this invention, the singular is used in conjunction with the plural unless otherwise specifically stated. It should also be noted that, unless otherwise stated, the use of “or” or “or” means “and / or”. Furthermore, the use of the term “comprising” and other forms such as “including,” “containing,” and “contains” are not limiting.
[0009] Unless otherwise stated, conventional methods within the scope of the art shall be used.
[0010] Unless specifically defined herein, the use of all commercially available products herein employs standard techniques. For example, it may be carried out using the manufacturer's instructions for use with the kit, or in accordance with methods known in the art or the description of this invention. The techniques and methods described herein can generally be implemented according to conventional methods well known in the art, based on the descriptions in the various summary and more specific documents cited and discussed in this specification.
[0011] The terms “optional / arbitrary” or “optionally / arbitrarily” mean that the event or situation described below may or may not occur, including both the occurrence and non-occurrence of the event or situation.
[0012] In a first aspect, the present invention provides: A type of fish maw cake, the raw materials for which the fish maw cake is prepared include: fish maw glue, jujubes, longan, sunflower seeds, and pumpkin seeds; the preparation method of the fish maw glue is as follows: Step 1: Take the raw fish swim bladder and add it to a eutectic solvent for extraction to obtain the extract; Step 2, enzymatic hydrolysis: Add a compound enzyme to the extract for enzymatic hydrolysis. After the hydrolysis is completed, sterilize, centrifuge and filter to obtain the enzymatic hydrolysate. Step 3, Purification: Sodium chloride is added to the enzymatic hydrolysate to precipitate the precipitate. After centrifugation and filtration, the precipitate is dissolved in acetic acid solution and then dialyzed with acetic acid solution and water in sequence. The dialysate is concentrated and then freeze-dried to obtain the fish maw gel. The eutectic solvent is menthol, citric acid, and water; the complex enzyme is β-glucanase, collagenase, and flavor protease.
[0013] The molar ratio of menthol, citric acid and water is 1-5:1-5:1-2, including but not limited to: 1:5:1, 1:4:1, 1:3:1, 1:2:1, 1:1:1, 2:1:1, 3:1:1, 4:1:1, 5:1:1, 1:5:2, 1:4:2, 1:3:2, 1:2:2, 1:1:2, 2:1:2, 3:1:2, 4:1:2, 5:1:2 or any molar ratio within this range.
[0014] In step one, the mass-to-volume ratio of the raw fish swim bladder to the eutectic solvent is 1:20-24 g / mL, including but not limited to 1:20 g / mL, 1:21 g / mL, 1:22 g / mL, 1:23 g / mL, 1:24 g / mL, or any mass-to-volume ratio within this range; the extraction temperature is 60-80℃, including but not limited to 60℃, 65℃, 70℃, 75℃, 80℃, or any temperature value within this range or any suitable temperature range; the number of extractions is 1-3 times, for example: 1 time, 2 times, or 3 times; each extraction lasts 10-20 minutes, including but not limited to 10 minutes, 12 minutes, 14 minutes, 16 minutes, 18 minutes, 20 minutes, or any time within this time range.
[0015] The mass ratio of β-glucanase, collagenase, and flavor protease is 1:0.2-0.6:2-8, including but not limited to: 1:0.2:2, 1:0.3:2, 1:0.4:2, 1:0.5:2, 1:0.6:2, 1:0.2:3, 1:0.3:3, 1:0.4:3, 1:0.5:3, 1:0.6:3, 1:0.2:4, 1:0.3:4, 1:0.4:4, 1:0.5:4, 1:0.6:4, 1:0.2:5, 1:0.3:5, 1:0.4:5, 1:0.5:5, 1:0.6:5, 1:0.2:6, 1:0.3:6, 1:0.4:6, 1:0.5:6, 1:0.6:6, or any mass ratio within this range.
[0016] In step two, the amount of the compound enzyme added is 0.1-0.5 wt% of the raw fish swim bladder, including but not limited to: 0.1 wt%, 0.2 wt%, 0.3 wt%, 0.4 wt%, 0.5 wt%, or any mass percentage within this range; the enzymatic hydrolysis temperature is 45-55℃, including but not limited to 45℃, 46℃, 47℃, 48℃, 49℃, 50℃, 51℃, 52℃, 53℃, 54℃, 55℃, or any temperature value or any suitable temperature range within this range; the pH value is 4.0-6.5, including but not limited to 4.0, 4.5, 5.0, 5.5, 6.0, 6.5, or any pH value or any suitable pH range within this range; the enzymatic hydrolysis time is 2-5 h, including but not limited to 2 h, 3 h, 4 h, 5 h, or any time within this range.
[0017] In step three, the concentration of NaCl in the solution during the precipitation process is 1-3 wt%, including but not limited to 1 wt%, 2 wt%, 3 wt%, or any concentration within this range.
[0018] In step three, the concentration of the acetic acid solution during the dissolution process is 0.3-0.5 mol / L, including but not limited to 0.3 mol / L, 0.35 mol / L, 0.4 mol / L, 0.45 mol / L, 0.5 mol / L, or any concentration within this range; and the volume-to-mass ratio of the acetic acid solution to the raw fish swim bladder is 5-10 mL / g, including but not limited to 5 mL / g, 6 mL / g, 7 mL / g, 8 mL / g, 9 mL / g, 10 mL / g, or any volume-to-mass ratio within this range.
[0019] In step three, the concentration of the acetic acid solution during dialysis is 0.1-0.2 mol / L, including but not limited to 0.1 mol / L, 0.15 mol / L, 0.2 mol / L, or any concentration within this range; the volume-to-mass ratio of the acetic acid solution to the raw fish swim bladder is 5-10 mL / g, including but not limited to 5 mL / g, 6 mL / g, 7 mL / g, 8 mL / g, 9 mL / g, 10 mL / g, or any volume-to-mass ratio within this range; and the dialysis time is 6-10 h, including but not limited to 6 h, 7 h, 8 h, 9 h, 10 h, or any time within this range.
[0020] During the dialysis process, the volume-to-mass ratio of water to raw fish swim bladder is 5-10 mL / g, including but not limited to: 5 mL / g, 6 mL / g, 7 mL / g, 8 mL / g, 9 mL / g, 10 mL / g or any volume-to-mass ratio within this range; the dialysis time is 6-10 h, including but not limited to 6 h, 7 h, 8 h, 9 h, 10 h or any time within this range.
[0021] Preferably, the raw materials of the fish maw cake, by weight, include: 47-55 parts fish maw glue, 48-52 parts jujubes, 48-52 parts longan, 48-52 parts sunflower seeds, and 48-52 parts pumpkin seeds.
[0022] More preferably, the raw material composition of the fish maw cake, by weight, includes: 51 parts fish maw glue, 50 parts jujubes, 50 parts longan, 50 parts sunflower seeds, and 50 parts pumpkin seeds.
[0023] As some preferred technical solutions of the present invention, the raw materials for preparing the fish gelatin cake also include: 18-22 parts of mulberry and 24-28 parts of wolfberry.
[0024] Secondly, the present invention also provides: The above-mentioned method for preparing fish gelatin cake includes the following steps: (1) Melting: Add fish maw glue to part of rice wine, heat and stir until completely melted, then add yellow rock sugar, continue stirring until completely melted, then add the remaining rice wine and yellow rock sugar in batches and continue stirring to obtain fish maw glue liquid; (2) Mixing raw materials: Take jujubes, longan, sunflower seeds and pumpkin seeds, chop them, stir and add them to fish glue liquid in turn to cook, and then cool and shape them to obtain the cake.
[0025] Furthermore, in step (1), the mass ratio of fish maw glue, rice wine and yellow rock sugar is 1:0.8-1.2:0.8-1.2.
[0026] Further, in step (1), the heating and stirring temperature is 60-80℃ and the time is 3-6 h; and / or in step (2), the cooking temperature is 40-60℃ and the time is 2-5 h.
[0027] Compared with the prior art, the present invention has the following beneficial effects: (1) The present invention adopts a process combining solvent extraction and enzymatic hydrolysis, which improves the flavor and taste of fish maw collagen while ensuring the extraction rate of fish maw collagen, and also improves the stability of the active ingredients. (2) The fish maw gel prepared by the specific process of this invention, when combined with jujube, longan, sunflower seed kernel and pumpkin seed kernel, has a significant blood-nourishing effect and is especially suitable for people with irregular menstruation, dull skin, long-term insomnia, menopause and other conditions. (3) The preparation method of the present invention is simple. By adding yellow rice wine in batches, the viscosity of fish maw glue is effectively improved, and the processing performance such as sticking to the pot during the preparation process is avoided. Detailed Implementation
[0028] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. 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.
[0029] β-glucanase, flavor protease, fig protease, and cellulase were all purchased from Shandong Pingju Biotechnology Co., Ltd.; collagenase (type II) was purchased from Hebei Runbu Biotechnology Co., Ltd.
[0030] Example 1 A type of fish maw cake is prepared using the following ingredients: 47 parts fish maw glue, 48 parts jujubes, 52 parts longan, 52 parts sunflower seeds, and 52 parts pumpkin seeds; the preparation method of the fish maw glue is as follows: Step 1: Take the raw fish swim bladder and add the fish swim bladder gelatin to a eutectic solvent (mix menthol, citric acid and water in a molar ratio of 1:1:1, heat to 35℃ under nitrogen protection and stir until there is no obvious layering, and sonicate for 2 hours to obtain the eutectic solvent) at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 15 minutes. Filter and add the filter residue to the aforementioned eutectic solvent at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 10 minutes. Combine the filtrates to obtain the extract. Step 2: Add 0.3 wt% of a complex enzyme (β-glucanase, collagenase, and flavor protease in a mass ratio of 1:0.4:4) to the extract and ferment at 50±2℃ and pH 5.0±0.2 for 4 hours. Then, remove unreacted enzymes and macromolecular impurities by inactivating the enzymes and centrifuging (5000 rpm for 5 min) to obtain the enzymatic hydrolysate. Step 3: Add sodium chloride to the enzymatic hydrolysate until the sodium chloride concentration is 3 wt%. After centrifugation (1000 rpm for 3 min), filter to collect the precipitate. Dissolve the precipitate with 0.4 mol / L acetic acid solution, then dialyze with 0.2 mol / L acetic acid solution for 8 h, and then dialyze with water for 8 h. After concentrating the dialysate, freeze dry to obtain fish swim bladder gel.
[0031] The preparation method of fish gelatin cake is as follows: (1) Take the amount of fish maw glue in the formula, add it to an appropriate amount of rice wine, heat it to 80℃ and stir until it melts; then add an appropriate amount of yellow rock sugar and continue stirring until the yellow rock sugar is completely melted. Then add the remaining rice wine and yellow rock sugar in 3 portions (the mass ratio of fish maw glue, rice wine and yellow rock sugar is 1:1:1) and stir until completely melted. Keep the temperature and continue to cook for 5 hours until it reaches the state of hanging flag, and obtain fish maw glue liquid. (2) Take the formula amount of jujube, longan, sunflower seed kernel and pumpkin seed kernel respectively, chop them, stir and add them to the fish maw glue liquid in sequence, cook at 50℃ for 3 hours to obtain paste, cool, shape and package to obtain fish glue cake product.
[0032] Example 2 A type of fish maw cake is prepared using the following ingredients: 51 parts fish maw glue, 50 parts jujubes, 50 parts longan, 50 parts sunflower seeds, and 50 parts pumpkin seeds; the preparation method of the fish maw glue is as follows: Step 1: Take the raw fish swim bladder and add the fish swim bladder gelatin to a eutectic solvent (take menthol, citric acid and water in a molar ratio of 1:5:1, heat to 30℃ under nitrogen protection and stir until there is no obvious layering, sonicate for 2 hours to obtain the eutectic solvent) at a ratio of 1:22 g / mL. Heat to 65℃ and extract for 20 min. Filter, then add the filter residue to the aforementioned eutectic solvent at a ratio of 1:22 g / mL and heat to 75℃ and extract for 10 min. Combine the filtrates to obtain the extract. Step 2: Add 0.5 wt% of a complex enzyme (β-glucanase, collagenase, and flavor protease in a mass ratio of 1:0.2:8) of the raw fish swim bladder to the extract, and ferment for 3 hours at 50±2℃ and pH 4.5±0.2. Then, remove unreacted enzymes and macromolecular impurities by inactivating the enzymes and centrifuging (5000 rpm for 5 min) to obtain the enzymatic hydrolysate. Step 3: Add sodium chloride to the enzymatic hydrolysate until the sodium chloride concentration is 3 wt%. After centrifugation (1000 rpm for 3 min), filter to collect the precipitate. Dissolve the precipitate with 0.4 mol / L acetic acid solution, then dialyze with 0.2 mol / L acetic acid solution for 8 h, and then dialyze with water for 8 h. After concentrating the dialysate, freeze dry to obtain fish swim bladder gel.
[0033] The preparation method of fish gelatin cake is the same as in Example 1.
[0034] Example 3 A type of fish maw cake is prepared using the following ingredients: 55 parts fish maw glue, 52 parts jujubes, 48 parts longan, 48 parts sunflower seeds, and 48 parts pumpkin seeds; the preparation method of the fish maw glue is as follows: Step 1: Take the raw fish swim bladder and add the fish swim bladder gelatin to a eutectic solvent (mix menthol, citric acid and water in a molar ratio of 5:1:1, heat to 45℃ under nitrogen protection and stir until there is no obvious layering, and sonicate for 2 hours to obtain the eutectic solvent) at a ratio of 1:24 g / mL. Heat to 60℃ and extract for 20 minutes. Filter and add the filter residue to the aforementioned eutectic solvent at a ratio of 1:24 g / mL. Heat to 75℃ and extract for 10 minutes. Combine the filtrates to obtain the extract. Step 2: Add 0.5 wt% of a complex enzyme (β-glucanase, collagenase, and flavor protease in a mass ratio of 1:0.6:2) to the extract and ferment at 50±2℃ and pH 5.5±0.2 for 3.5 h. Then, remove unreacted enzymes and macromolecular impurities by inactivating the enzymes and centrifuging (5000 rpm for 5 min) to obtain the enzymatic hydrolysate. Step 3: Add sodium chloride to the enzymatic hydrolysate until the sodium chloride concentration is 3 wt%. After centrifugation (1000 rpm for 3 min), filter to collect the precipitate. Dissolve the precipitate with 0.4 mol / L acetic acid solution, then dialyze with 0.2 mol / L acetic acid solution for 8 h, and then dialyze with water for 8 h. After concentrating the dialysate, freeze dry to obtain fish swim bladder gel.
[0035] The preparation method of fish gelatin cake is the same as in Example 1.
[0036] Example 4 A type of fish maw cake is prepared using the following ingredients: 47 parts fish maw glue, 48 parts jujubes, 52 parts longan, 52 parts sunflower seeds and 52 parts pumpkin seeds, 20 parts mulberries, and 26 parts wolfberries; wherein the preparation method of the fish maw glue is the same as in Example 1.
[0037] The preparation method of fish gelatin cake is as follows: (1) Take the amount of fish maw glue in the formula, add it to an appropriate amount of rice wine, heat it to 80℃ and stir until it melts; then add an appropriate amount of yellow rock sugar and continue stirring until the yellow rock sugar is completely melted. Then add the remaining rice wine and yellow rock sugar in 3 portions (the mass ratio of fish maw glue, rice wine and yellow rock sugar is 1:1:1) and stir until completely melted. Keep the temperature and continue to cook for 5 hours until it reaches the state of hanging flag, and obtain fish maw glue liquid. (2) Take the formula amount of jujube, longan, sunflower seed kernel, pumpkin seed kernel, mulberry and wolfberry respectively, chop them, stir and add them to the fish maw glue solution in sequence, cook at 50℃ for 3 hours to obtain paste, cool, shape and package to obtain fish glue cake product.
[0038] Comparative Example 1 The only difference from Example 1 is the type of eutectic solvent used in the preparation of the fish maw glue, as detailed below: Step 1: Take the raw fish swim bladder and add the fish swim bladder gelatin to a eutectic solvent (mix urea and lactic acid in a molar ratio of 1:20 g / mL, heat to 35℃ under nitrogen protection and stir until there is no obvious layering, and sonicate for 2 hours to obtain the eutectic solvent) at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 15 min. Filter and add the filter residue to the aforementioned eutectic solvent at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 10 min. Combine the filtrates to obtain the extract. Step 2: Add 0.3 wt% of a complex enzyme (β-glucanase, collagenase, and flavor protease in a mass ratio of 1:0.4:4) to the extract and ferment at 50±2℃ and pH 5.0±0.2 for 4 hours. Then, remove unreacted enzymes and macromolecular impurities by inactivating the enzymes and centrifuging (5000 rpm for 5 min) to obtain the enzymatic hydrolysate. Step 3: Add sodium chloride to the enzymatic hydrolysate until the sodium chloride concentration is 3 wt%. After centrifugation (1000 rpm for 3 min), filter to collect the precipitate. Dissolve the precipitate with 0.4 mol / L acetic acid solution, then dialyze with 0.2 mol / L acetic acid solution for 8 h, and then dialyze with water for 8 h. After concentrating the dialysate, freeze dry to obtain fish swim bladder gel.
[0039] The fish gelatin cake product was prepared according to the formula and preparation method of Example 1.
[0040] Comparative Example 2 The only difference from Example 1 is the type of eutectic solvent used in the preparation of the fish maw glue, as detailed below: Step 1: Take the raw fish swim bladder and add the fish swim bladder gelatin to a eutectic solvent (mix urea and citric acid in a molar ratio of 1:20 g / mL, heat to 35℃ under nitrogen protection and stir until there is no obvious layering, and sonicate for 2 hours to obtain the eutectic solvent) at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 15 minutes. Filter and add the filter residue to the aforementioned eutectic solvent at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 10 minutes. Combine the filtrates to obtain the extract. Step 2: Add 0.3 wt% of a complex enzyme (β-glucanase, collagenase, and flavor protease in a mass ratio of 1:0.4:4) to the extract and ferment at 50±2℃ and pH 5.0±0.2 for 4 hours. Then, remove unreacted enzymes and macromolecular impurities by inactivating the enzymes and centrifuging (5000 rpm for 5 min) to obtain the enzymatic hydrolysate. Step 3: Add sodium chloride to the enzymatic hydrolysate until the sodium chloride concentration is 3 wt%. After centrifugation (1000 rpm for 3 min), filter to collect the precipitate. Dissolve the precipitate with 0.4 mol / L acetic acid solution, then dialyze with 0.2 mol / L acetic acid solution for 8 h, and then dialyze with water for 8 h. After concentrating the dialysate, freeze dry to obtain fish swim bladder gel.
[0041] The fish gelatin cake product was prepared according to the formula and preparation method of Example 1.
[0042] Comparative Example 3 The only difference from Example 1 is the type of eutectic solvent used in the preparation of the fish maw glue, as detailed below: Step 1: Take the raw fish swim bladder and add the fish swim bladder gelatin to a eutectic solvent (take menthol and citric acid mixed at a molar ratio of 1:20 g / mL, heat to 35℃ under nitrogen protection and stir until there is no obvious layering, sonicate for 2 hours to obtain the eutectic solvent) at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 15 minutes. Filter and add the filter residue to the aforementioned eutectic solvent at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 10 minutes. Combine the filtrates to obtain the extract. Step 2: Add 0.3 wt% of a complex enzyme (β-glucanase, collagenase, and flavor protease in a mass ratio of 1:0.4:4) to the extract and ferment at 50±2℃ and pH 5.0±0.2 for 4 hours. Then, remove unreacted enzymes and macromolecular impurities by inactivating the enzymes and centrifuging (5000 rpm for 5 min) to obtain the enzymatic hydrolysate. Step 3: Add sodium chloride to the enzymatic hydrolysate until the sodium chloride concentration is 3 wt%. After centrifugation (1000 rpm for 3 min), filter to collect the precipitate. Dissolve the precipitate with 0.4 mol / L acetic acid solution, then dialyze with 0.2 mol / L acetic acid solution for 8 h, and then dialyze with water for 8 h. After concentrating the dialysate, freeze dry to obtain fish swim bladder gel.
[0043] The fish gelatin cake product was prepared according to the formula and preparation method of Example 1.
[0044] Comparative Example 4 The only difference from Example 1 is the composition of the complex enzyme in the preparation of fish swim bladder gel, as detailed below: Step 1: Take the raw fish swim bladder and add the fish swim bladder gelatin to a eutectic solvent (mix menthol, citric acid and water in a molar ratio of 1:1:1, heat to 35℃ under nitrogen protection and stir until there is no obvious layering, and sonicate for 2 hours to obtain the eutectic solvent) at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 15 minutes. Filter and add the filter residue to the aforementioned eutectic solvent at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 10 minutes. Combine the filtrates to obtain the extract. Step 2: Add 0.3 wt% of a complex enzyme (β-glucanase, collagenase, and fig protease in a mass ratio of 1:0.4:4) to the extract and ferment at 50±2℃ and pH 5.0±0.2 for 4 hours. Then, remove unreacted enzymes and macromolecular impurities by inactivating the enzymes and centrifuging (5000 rpm for 5 min) to obtain the enzymatic hydrolysate. Step 3: Add sodium chloride to the enzymatic hydrolysate until the sodium chloride concentration is 3 wt%. After centrifugation (1000 rpm for 3 min), filter to collect the precipitate. Dissolve the precipitate with 0.4 mol / L acetic acid solution, then dialyze with 0.2 mol / L acetic acid solution for 8 h, and then dialyze with water for 8 h. After concentrating the dialysate, freeze dry to obtain fish swim bladder gel.
[0045] The fish gelatin cake product was prepared according to the formula and preparation method of Example 1.
[0046] Comparative Example 5 The only difference from Example 1 is the composition of the complex enzyme in the preparation of fish swim bladder gel, as detailed below: Step 1: Take the raw fish swim bladder and add the fish swim bladder gelatin to a eutectic solvent (mix menthol, citric acid and water in a molar ratio of 1:1:1, heat to 35℃ under nitrogen protection and stir until there is no obvious layering, and sonicate for 2 hours to obtain the eutectic solvent) at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 15 minutes. Filter and add the filter residue to the aforementioned eutectic solvent at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 10 minutes. Combine the filtrates to obtain the extract. Step 2: Add 0.3 wt% of a complex enzyme (β-glucanase, cellulase, and flavor protease in a mass ratio of 1:0.4:4) to the extract and ferment for 4 hours at 50±2℃ and pH 5.0±0.2. Then, remove unreacted enzymes and macromolecular impurities by inactivating the enzymes and centrifuging (5000 rpm for 5 min) to obtain the enzymatic hydrolysate. Step 3: Add sodium chloride to the enzymatic hydrolysate until the sodium chloride concentration is 3 wt%. After centrifugation (1000 rpm for 3 min), filter to collect the precipitate. Dissolve the precipitate with 0.4 mol / L acetic acid solution, then dialyze with 0.2 mol / L acetic acid solution for 8 h, and then dialyze with water for 8 h. After concentrating the dialysate, freeze dry to obtain fish swim bladder gel.
[0047] The fish gelatin cake product was prepared according to the formula and preparation method of Example 1.
[0048] Comparative Example 6 The only difference from Example 1 is the composition of the complex enzyme in the preparation of fish swim bladder gel, as detailed below: Step 1: Take the raw fish swim bladder and add the fish swim bladder gelatin to a eutectic solvent (mix menthol, citric acid and water in a molar ratio of 1:1:1, heat to 35℃ under nitrogen protection and stir until there is no obvious layering, and sonicate for 2 hours to obtain the eutectic solvent) at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 15 minutes. Filter and add the filter residue to the aforementioned eutectic solvent at a ratio of 1:20 g / mL. Heat to 75℃ and extract for 10 minutes. Combine the filtrates to obtain the extract. Step 2: Add 0.3 wt% of a complex enzyme (β-glucanase, cellulase, and fig protease in a mass ratio of 1:0.4:4) to the extract and ferment at 50±2℃ and pH 5.0±0.2 for 4 hours. Then, remove unreacted enzymes and macromolecular impurities by inactivating the enzymes and centrifuging (5000 rpm for 5 min) to obtain the enzymatic hydrolysate. Step 3: Add sodium chloride to the enzymatic hydrolysate until the sodium chloride concentration is 3 wt%. After centrifugation (1000 rpm for 3 min), filter to collect the precipitate. Dissolve the precipitate with 0.4 mol / L acetic acid solution, then dialyze with 0.2 mol / L acetic acid solution for 8 h, and then dialyze with water for 8 h. After concentrating the dialysate, freeze dry to obtain fish swim bladder gel.
[0049] The fish gelatin cake product was prepared according to the formula and preparation method of Example 1.
[0050] Comparative Example 7 The only difference from Example 1 is that the raw material composition is different. Specifically, it consists of 47 parts fish maw glue, 48 parts jujube, 52 parts longan and 104 parts sunflower seed kernels. The preparation method of fish maw glue is the same as in Example 1.
[0051] The preparation method of fish gelatin cake is as follows: (1) Take the amount of fish maw glue in the formula, add it to an appropriate amount of rice wine, heat it to 80℃ and stir until it melts; then add an appropriate amount of yellow rock sugar and continue stirring until the yellow rock sugar is completely melted. Then add the remaining rice wine and yellow rock sugar in 3 portions (the mass ratio of fish maw glue, rice wine and yellow rock sugar is 1:1:1) and stir until completely melted. Keep the temperature and continue to cook for 5 hours until it reaches the state of hanging flag, and obtain fish maw glue liquid. (2) Take the formula amount of jujube, longan and sunflower seeds respectively, chop them, stir and add them to the fish maw glue solution in turn, cook at 50℃ for 3 hours to obtain paste, cool, shape and package to obtain fish maw cake product.
[0052] Comparative Example 8 The only difference from Example 1 is that the raw material composition is different. Specifically, it consists of 47 parts fish maw glue, 48 parts jujube, 52 parts angelica, and 52 parts white peony root. The preparation method of fish maw glue is the same as in Example 1.
[0053] The preparation method of fish gelatin cake is as follows: (1) Take the amount of fish maw glue in the formula, add it to an appropriate amount of rice wine, heat it to 80℃ and stir until it melts; then add an appropriate amount of yellow rock sugar and continue stirring until the yellow rock sugar is completely melted. Then add the remaining rice wine and yellow rock sugar in 3 portions (the mass ratio of fish maw glue, rice wine and yellow rock sugar is 1:1:1) and stir until completely melted. Keep the temperature and continue to cook for 5 hours until it reaches the state of hanging flag, and obtain fish maw glue liquid. (2) Take the formula amount of jujube, longan, angelica and white peony, chop them, stir and add them to the fish maw glue solution in sequence, cook at 50℃ for 3 hours to obtain paste, cool, shape and package to obtain fish maw cake product.
[0054] Test Example 1: Sensory Evaluation Test of Fish Gelatin Cake Referring to GB / T 29605—2013 "Sensory Analysis Guidelines for Sensory Quality Control of Food", 10 personnel who have received certain sensory analysis training were selected to evaluate the color, aroma, texture and taste of the fish gelatin cake products prepared in the above examples in proportion. The specific evaluation criteria are shown in Table 1, and the evaluation results are shown in Table 2.
[0055] Table 1 Sensory Evaluation Criteria
[0056] Table 2 Sensory evaluation results of fish gelatin cake (scores)
[0057] As can be seen from Table 2, the fish maw cakes prepared in Examples 1-4 of this invention have high scores in color, odor, texture and taste. The fish maw preparation processes of Comparative Examples 1-6 are different, and the odor and taste scores are slightly lower, which has little impact on the sensory evaluation. However, the raw materials of Comparative Examples 7-8 are changed, and the scores of all aspects of the sensory evaluation change significantly. It can be seen that the raw materials have a significant impact on color, odor, texture and taste.
[0058] Test Example 2: Stability Evaluation Test of Fish Gelatin Cake According to the "Guidelines for Stability Testing of Health Foods", the fish gelatin cakes prepared in the comparative examples above were stored for 3 months at a temperature of 37±2℃, relative humidity of 75%±5% and away from direct light. The moisture content (GB 5009.3-2016) and peroxide value (GB 5009.227-2023) of the fish gelatin cake samples were tested at 0, 1, 2 and 3 months to verify the shelf life of the fish gelatin cakes. The results are shown in Tables 3 and 4.
[0059] Table 3. Results of moisture content determination in fish gelatin cake (%)
[0060] Table 4. Peroxide value test results of fish gelatin cake (g / 100g)
[0061] As shown in Tables 3 and 4, the fish gelatin cakes prepared in Examples 1-4 of this invention have a moisture content between 10-15% and a peroxide value below 0.15g / 100g within 3 months, exhibiting high stability. The fish gelatin cake in Comparative Example 7 has an initial moisture content above 15% after 2 months of storage, indicating a high risk of spoilage. After 3 months, its peroxide value also exceeds 0.15g / 100g, but remains below 0.25g / 100g, showing slight oxidative rancidity of the oil. The moisture content changes of the fish gelatin cakes in other comparative examples are similar to those in the examples, and the peroxide values all show varying degrees of increase (except for Comparative Example 8, where the use of Angelica sinensis and Paeonia lactiflora as raw materials has almost no impact on the product's stability). Overall, the fish gelatin cakes prepared in Examples 1-4 of this invention exhibit the best stability.
[0062] Test Example 3: Experiment on the efficacy of fish gelatin cake in improving anemia I. Experimental Animals and Materials SPF-grade male SD rats, weighing 200±20 g.
[0063] Low-iron feed, purchased from Nantong Trofi Feed Technology Co., Ltd., product code: TP0306; The control feed was purchased from Nantong Trofi Feed Technology Co., Ltd., product code: TP0306C; Ferrous sulfate solution: After adjusting the pH to 2.5 by adding a small amount of dilute sulfuric acid to deionized water, add ferrous sulfate heptahydrate (FeSO4·7H2O) crystals to prepare a solution. Prepare and use immediately.
[0064] II. Experimental Methods: 2.1 Modeling and Drug Administration: SD rats (weighing 200±20g) were randomly divided into 15 groups after one week of acclimatization: normal group, model group, positive control group (administered with ferrous sulfate 27 mg / (kg.bw·d)), and groups of Examples 1-4 and Comparative Examples 1-8 (2 g / (kg.bw·d) of fish gelatin cake prepared in Examples 1-4 and Comparative Examples 1-8, pulverized and dispersed in water), with 10 rats in each group. The normal control group was fed a control diet, while the other groups were fed a low-iron diet. During the experiment, tail clipping and bloodletting were performed twice a week, with 0.5 mL per rat each time. The model group was administered 1 mL of distilled water by gavage daily, while the other groups were administered 1 mL of the corresponding solution by gavage for 4 consecutive weeks.
[0065] 2.2 Evaluation Indicators: After the administration of the drug, blood was collected through the abdominal aorta, and peripheral blood red blood cells (RBC), hemoglobin (HGB), hematocrit (HCT) and other hematological indicators were analyzed using a fully automated modular blood and body fluid analyzer. Serum iron (SI), serum ferritin (SF), total iron-binding capacity (TIBC), and transferrin saturation (TSAT) were measured by colorimetric method, and TSAT (SI / TIBC) was calculated. The results are shown in Tables 5 and 6.
[0066] 2.3 Data Processing: Experimental results are expressed as mean ± standard deviation, and statistical software was used for t-tests and analysis of variance. P <0.05 indicates that the difference is statistically significant.
[0067] III. Experimental Results: Table 5. Results of hematological parameters RBC, HGB and HCT in rats of each group
[0068] Note: Compared with the normal group, the model group, P <0.0001; compared with the model group, each drug-treated group # P <0.05, ## P <0.01; ### P <0.001; #### P <0.0001; compared with Example 1 group, each comparative example group &&& P <0.001; &&&& P <0.0001.
[0069] Table 6. Serum SI, TIBC, TSAT and SF levels in each group of rats
[0070] Note: Compared with the normal group, the model group, P <0.0001; compared with the model group, each drug-treated group # P <0.05, ## P <0.01; ### P <0.001;#### P <0.0001; compared with Example 1 group, each comparative example group &&&& P <0.0001.
[0071] As shown in Tables 5 and 6, compared with the normal group, the red blood cell count (RBC), hemoglobin (HGB), and hematocrit (HCT) of the model group rats were significantly reduced. P <0.0001); SI content, TSAT and SF all decreased significantly ( P <0.0001 or P <0.01), while TIBC increased significantly ( P <0.0001), indicating that the iron deficiency anemia model was successfully established.
[0072] Compared with the model group, the positive group and the groups of Examples 1-4 showed that all indicators tended to be at the level of the normal group and were significantly different from the model group. P <0.0001). Comparative Examples 1-8 also showed varying degrees of difference in some indicators. P <0.0001 or P <0.001), but significantly worse than Example Group 1. It can be seen that the specific solvent and enzymatic hydrolysis process in the preparation of fish maw cake of the present invention is more conducive to the release of active ingredients. At the same time, when the fish maw is combined with specific traditional Chinese medicine, it effectively reverses the state of iron deficiency anemia, insufficient red blood cell count and decreased oxygen carrying capacity, and also effectively improves serum iron metabolism.
[0073] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, and is not intended to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions made by those skilled in the art to the technical solution of the present invention do not depart from the essence and scope of the technical solution of the present invention.
Claims
1. A type of fish gelatin cake, characterized in that, The raw materials for preparing the fish maw cake include: fish maw glue, jujubes, longan, sunflower seeds, and pumpkin seeds; the preparation method of the fish maw glue is as follows: Step 1: Take the raw fish swim bladder and add it to a eutectic solvent for extraction to obtain the extract; Step 2, Enzymatic hydrolysis: Add a compound enzyme to the extract for enzymatic hydrolysis. After the hydrolysis is completed, sterilize, centrifuge and filter to obtain the hydrolysate. Step 3, Purification: Sodium chloride is added to the enzymatic hydrolysate to precipitate the precipitate. After centrifugation and filtration, the precipitate is dissolved in acetic acid solution and then dialyzed with acetic acid solution and water in sequence. The dialysate is concentrated and then freeze-dried to obtain the fish maw gel. The eutectic solvent is menthol, citric acid, and water; the complex enzyme is β-glucanase, collagenase, and flavor protease.
2. The fish gelatin cake according to claim 1, characterized in that, The molar ratio of menthol, citric acid and water is 1-5:1-5:1-2.
3. The fish gelatin cake according to claim 1, characterized in that, The mass ratio of β-glucanase, collagenase, and flavor protease is 1-2:0.2-0.6:2-8.
4. The fish gelatin cake according to claim 1, characterized in that, In step one, the extracted process parameters include: The mass-to-volume ratio of the fish swim bladder to the eutectic solvent is 1:20-24 g / mL; The extraction temperature is 60-80℃; Extraction is performed 1-3 times, with each extraction lasting 10-20 minutes.
5. The fish gelatin cake according to claim 1, characterized in that, In step two, the amount of the compound enzyme added is 0.1-0.5 wt% of the raw fish swim bladder. And / or the conditions for the enzymatic hydrolysis include: a temperature of 45-55°C, a pH of 4.0-6.0, and a hydrolysis time of 2-5 h.
6. The fish gelatin cake according to claim 1, characterized in that, The ingredients of the fish maw cake, by weight, include: 47-55 parts fish maw glue, 48-52 parts jujubes, 48-52 parts longan, 48-52 parts sunflower seeds, and 48-52 parts pumpkin seeds.
7. The fish gelatin cake according to claim 6, characterized in that, The raw materials for preparing the fish gelatin cake also include: 18-22 parts of mulberry and 24-28 parts of wolfberry.
8. The method for preparing fish gelatin cake according to any one of claims 1-7, characterized in that, Includes the following steps: (1) Melting: Add fish maw glue to part of rice wine, heat and stir until completely melted, then add yellow rock sugar, continue stirring until completely melted, then add the remaining rice wine and yellow rock sugar in batches and continue stirring to obtain fish maw glue liquid; (2) Mixing raw materials: Take jujubes, longan, sunflower seeds and pumpkin seeds, chop them, stir and add them to fish glue solution in turn to cook, and then cool and shape them to obtain the cake.
9. The preparation method according to claim 8, characterized in that, In step (1), the mass ratio of fish maw glue, rice wine and yellow rock sugar is 1:0.8-1.2:0.8-1.
2.
10. The preparation method according to claim 8, characterized in that, In step (1), the heating and stirring temperature is 60-80℃ and the time is 3-6 h; and / or in step (2), the cooking temperature is 40-60℃ and the time is 2-5 h.
Citation Information
Patent Citations
A kind of composite fish bladder glue and preparation method thereof
CN116746668B
