A peach essence and a preparation method thereof
Patent Information
- Application Number
- CN202411037645.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-31
- Publication Date
- 2026-09-22
- Estimated Expiration
- 2044-07-31
AI Technical Summary
现有的水蜜桃香精中,通常直接桃醛来调配水蜜桃的气味及口味,但桃醛调配得到的水蜜桃香精,桃子的气味较弱,口味并不会纯正
化学合成的香精经过复配虽然可以接近蜜桃果香,但是其味道不纯正,且复配难度大,往往限制了其应用。本发明采用直接以水蜜桃果肉为原料,通过复合酶酶解,在纤维素酶和无花果蛋白酶的协同作用下,果肉细胞壁破裂,使得大部分香气组分、多糖、蛋白等均溶出进入溶液中,进一步在枯草芽孢杆菌和干酪乳杆菌的发酵作用下,难溶的大分子化合物经过发酵转化为了丰富的芳香组分,包括α-松油醇、蒲勒酮、乙酸苯乙酯、二氢香芹酮、邻苯二甲酸二异丁酯、β-紫罗兰酮等活性香气组分,从而使得水蜜桃中产生了丰富浓郁的芳香组分。
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Abstract
Description
Technical Field
[0001] This invention relates to the field of fragrance technology, specifically to a peach fragrance and its preparation method. Background Technology
[0002] Peaches are mild in flavor, juicy, delicious, and nutritious, with a unique aroma that makes them highly popular among consumers. As a typical climacteric stone fruit, peaches are harvested during the hot season, and after harvesting, they rapidly reach a respiratory peak at room temperature, accelerating the ripening and senescence process. Their thin skin makes them easily damaged during harvesting and transportation. Furthermore, their high water and sugar content makes them highly susceptible to microbial contamination and spoilage, making long-distance storage and preservation difficult. Besides being eaten fresh, peaches can be processed into peach jam, peach juice, and canned peaches. However, processing diminishes or even eliminates the characteristic aroma of fresh peaches, making it difficult for consumers to experience the true flavor of fresh peaches. With my country's annual peach production showing an increasing trend, to improve the quality and sales volume of peach products and increase farmers' income, appropriate addition of peach flavoring can be used to modify and compensate for any deficiencies, further enhancing the quality of processed products.
[0003] Compared to other aromatic plants, the aromatic characteristics of peach fruit are more complex, with rich variations in content and significant variability. Furthermore, the analysis of trace or unstable aromatic substances in peach fruit places higher demands on precise detection technologies. These factors all contribute to the challenges in developing natural peach flavorings. Currently, peach aldehyde is typically used directly to blend the aroma and flavor of peaches. However, peach aldehyde-blended peach flavorings have a weaker peach aroma and lack a pure flavor. Summary of the Invention
[0004] The purpose of this invention is to propose a peach flavoring and its preparation method, which has a rich flavor, pure and delicate aroma, sustained release, and improved resistance to breakage. It enhances the aroma retention, persistence and stability, increases its applicability, improves the storage stability of microcapsule products, and extends their shelf life, thus having broad application prospects.
[0005] The technical solution of this invention is implemented as follows: This invention provides a method for preparing peach flavoring. The peach flesh is dried, enzymatically hydrolyzed, fermented and filtered, and the extract is purified by supercritical fluid extraction. The product obtained by reacting carboxylated chitosan with silk fibroin peptides is fixed to form a preservation and aroma-locking cage. After the first layer of β-cyclodextrin is embedded, the second layer of β-cyclodextrin is embedded by the coagulation method to obtain β-cyclodextrin.
[0006] As a further improvement to the present invention, the following steps are included: S1. Enzymatic hydrolysis: Peel and pit the peaches, dry them, and crush them to obtain peach powder. Add water, add a compound enzyme, hydrolyze, and inactivate the enzyme to obtain the enzymatic hydrolysis product. S2. Fermentation: Sterilize the enzymatic hydrolysis product from step S1, inoculate with Bacillus subtilis and Lactobacillus casei, ferment and culture, filter, dry the filtrate, and obtain the fermentation product; S3. Supercritical fluid extraction: The fermentation product from step S2 is subjected to supercritical fluid extraction to obtain an extract; S4. Molecular distillation: Add the extract obtained in step S3 into a molecular distillation apparatus, heat to a first temperature to remove the distillate, heat to a second temperature, and collect the distillate; S5. Preparation of the fresh-keeping and fragrance-locking cage: Carboxylated chitosan was dissolved in water, N-hydroxysuccinimide and 1-ethyl-(3-dimethylaminopropyl)carbodiimide were added for activation, silk fibroin peptides were added, the reaction was stirred, the distillate from step S4 was added, and the mixture was freeze-dried to obtain the fresh-keeping and fragrance-locking cage. S6. Double-layer encapsulation: Dissolve β-cyclodextrin in water, add the preservative and lecithin obtained in step S5, heat and stir to react, centrifuge, freeze dry to obtain a layer of encapsulated particles, add the obtained layer of encapsulated particles, gelatin, silk fibroin peptide, pore-forming agent to water, add vitamin E and lipophilic emulsifier, homogenize, adjust the pH of the solution to 4-4.5, stir to react, then adjust the pH of the solution to 6.4-6.7, add transglutaminase, stir to react, centrifuge, wash, dry to obtain peach flavoring.
[0007] As a further improvement of the present invention, in step S1, the solid-liquid ratio of the peach powder to water is 1:7-10 g / mL, the mass ratio of the peach powder to the compound enzyme is 10:0.5-1, and the compound enzyme is selected from at least two of cellulase, pectinase, α-amylase, β-amylase, neutral protease, papain, and fig protease. Preferably, it is a mixture of cellulase and fig protease with a mass ratio of 10:3-5. The enzymatic hydrolysis temperature is 40-50℃ and the time is 1-3 h.
[0008] As a further improvement of the present invention, the inoculation amounts of Bacillus subtilis and Lactobacillus casei seed solutions in step S2 are 1-2 v / v% and 0.5-1.5 v / v%, respectively, and the fermentation conditions are 36-40℃, 100-200 r / min, and fermentation culture for 24-36 h.
[0009] As a further improvement of the present invention, the supercritical fluid extraction conditions in step S3 are: CO2 flow rate of 25-32 L / h, extraction pressure of 30-35 MPa, extraction temperature of 40-50℃, desorption pressure of 9.5-10.5 MPa, desorption temperature of 50-60℃, time of 1-2 h, entrainer is ethanol, and the amount of entrainer added is 1-2%.
[0010] As a further improvement of the present invention, in step S4, the first temperature is 50-60°C and the second temperature is 115-135°C.
[0011] As a further improvement of the present invention, the mass ratio of carboxylated chitosan, N-hydroxysuccinimide, 1-ethyl-(3-dimethylaminopropyl)carbodiimide, silk fibroin peptide, and distillate in step S5 is 10-12:3-5:4-6:7-10:5-7, the activation conditions are room temperature and the time is 1-2 h, and the stirring reaction time is 10-12 h.
[0012] As a further improvement of the present invention, the mass ratio of β-cyclodextrin, preservative, and lecithin in step S6 is 15-20:7-10:0.5-1; the heating and stirring reaction temperature is 45-55℃ and the time is 2-4 hours; the mass ratio of the layer-embedded particles, gelatin, silk fibroin peptide, pore-forming agent, vitamin E, lipophilic emulsifier, and transglutaminase is 15-20:17-22:2-3:0.5-1:1-2:0.5-1:3-5; the lipophilic emulsifier is selected from at least one of Span-20, Span-40, Span-60, Span-80, and Span-85; the homogenization speed is 10000-12000 r / min and the time is 10-20 min; and the pore-forming agent is selected from at least one of hexadecyltrimethylammonium chloride, hexadecyltrimethylsodium chloride, and hexadecyldimethylbenzylsodium chloride.
[0013] As a further improvement to the present invention, the specific steps include: S1. Enzymatic hydrolysis: Peel and pit the peaches, freeze-dry them, pulverize them to obtain peach powder, add water, the solid-liquid ratio of the peach powder to water is 1:7-10 g / mL, add a compound enzyme, the mass ratio of the peach powder to the compound enzyme is 10:0.5-1, enzymatic hydrolysis is carried out at 40-50℃ for 1-3 hours, enzyme is inactivated, and the enzymatic hydrolysis product is obtained; The complex enzyme is a mixture of cellulase and fig protease in a mass ratio of 10:3-5. S2. Fermentation: Sterilize the enzymatic hydrolysis product from step S1, inoculate with Bacillus subtilis and Lactobacillus casei seed culture at inoculation amounts of 1-2 v / v% and 0.5-1.5 v / v%, respectively, at 36-40℃ and 100-200 r / min, ferment for 24-36 h, filter, dry the filtrate, and obtain the fermentation product; S3. Supercritical fluid extraction: The fermentation product from step S2 is subjected to supercritical fluid extraction to obtain an extract; The supercritical fluid extraction conditions are: CO2 flow rate of 25-32 L / h, extraction pressure of 30-35 MPa, extraction temperature of 40-50℃, desorption pressure of 9.5-10.5 MPa, desorption temperature of 50-60℃, extraction time of 1-2 h, and ethanol as the entrainer, with an addition amount of 1-2%. S4. Molecular distillation: Add the extract obtained in step S3 into a molecular distillation apparatus, heat to 50-60℃ to remove the distillate, heat to 115-135℃, and collect the distillate; S5. Preparation of the fresh-keeping and fragrance-locking cage: Dissolve 10-12 parts by weight of carboxylated chitosan in water, add 3-5 parts by weight of N-hydroxysuccinimide and 4-6 parts by weight of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, stir and activate at room temperature for 1-2 hours, add 7-10 parts by weight of silk fibroin peptide, stir and react for 10-12 hours, add 5-7 parts by weight of the distillate from step S4, freeze-dry to obtain the fresh-keeping and fragrance-locking cage; S6. Double-layer embedding: Dissolve 15-20 parts by weight of β-cyclodextrin in 100 parts by weight of water, add 7-10 parts by weight of the preservative and fragrance-locking agent obtained in step S5 and 0.5-1 parts by weight of lecithin, heat to 45-55℃, stir and react for 2-4 hours, centrifuge, freeze dry to obtain a single-layer embedded particle. Add 15-20 parts by weight of the single-layer embedded particle, 17-22 parts by weight of gelatin, 2-3 parts by weight of silk fibroin peptide, and 0.5-1 parts by weight of pore-forming agent. Add 200 parts by weight of water, 1-2 parts by weight of vitamin E and 0.5-1 parts by weight of lipophilic emulsifier, homogenize at 10000-12000 r / min for 10-20 min, adjust the pH of the solution to 4-4.5, stir for 20-40 min, then adjust the pH of the solution to 6.4-6.7, add 3-5 parts by weight of transglutaminase, stir for 2-4 h, centrifuge, wash, and dry to obtain peach flavoring.
[0014] This invention further protects a peach flavoring prepared by the above-described preparation method.
[0015] This invention further protects the application of the above-mentioned peach flavoring in the food, textile, and feed industries.
[0016] The present invention has the following beneficial effects: While chemically synthesized flavorings can approximate the aroma of peaches through blending, their taste is not pure, and blending them is difficult, often limiting their application. This invention uses peach pulp directly as raw material. Through enzymatic hydrolysis with a complex enzyme, the cell walls of the pulp rupture under the synergistic action of cellulase and fig protease, allowing most aroma components, polysaccharides, and proteins to dissolve into the solution. Further fermentation by Bacillus subtilis and Lactobacillus casei transforms insoluble macromolecular compounds into rich aromatic components, including α-terpineol, purée, phenethyl acetate, dihydrocarvone, diisobutyl phthalate, and β-ionone, resulting in a rich and intense aromatic composition in the peach.
[0017] Supercritical fluid extraction offers advantages such as high extraction efficiency, no solvent residue, and mild operating conditions, overcoming the drawbacks of traditional extraction processes and effectively preserving the characteristics of natural active substances. However, the extract obtained from supercritical CO2 fluid extraction has a complex aroma. Due to the lack of selective separation of aroma-producing components, it contains some substances detrimental to the peach aroma, leading to unpleasant fragrance, increased roughness, and dryness. Therefore, this invention further employs molecular distillation technology to purify the extract, avoiding thermal decomposition, precise distillation, reducing the loss of important components, and greatly preserving the molecular structure of the original active substances. This removes low-boiling-point aromatic components and retains complex fragrance components with higher purity, thereby improving the fineness of the resulting peach flavoring, making it sweeter, with a purer fruity aroma, free from roughness and dryness, and more appealing to consumers. However, the directly obtained distillate is volatile, lacks sustained-release properties, cannot retain its aroma for a long time, has poor stability, and cannot be stored for extended periods.
[0018] This invention modifies chitosan by carboxylation to obtain carboxyl-containing chitosan. After activation with N-hydroxysuccinimide and 1-ethyl-(3-dimethylaminopropyl)carbodiimide, it condenses with the amino groups on the surface of silk fibroin peptides to obtain a cage-like complex. This complex facilitates the adsorption and fixation of different aroma molecules in the distillate, improving its sustained-release properties and aroma persistence. However, since silk fibroin peptides are protein-based substances, they are prone to bacterial growth, leading to a spoiled odor. This invention uses chitosan for the complex. Chitosan has excellent antibacterial properties, which can significantly inhibit bacterial growth, extend shelf life, and improve the structural stability of the resulting aroma-locking cage, thereby enhancing its sustained-release properties.
[0019] Fragrances have calming, hypnotic, and mood-enhancing effects, but because they are mostly alcohols, ethers, and aldehydes, they have low boiling points and are easily volatile. Microcapsules utilize film-forming materials to encapsulate substances like fragrances that are easily affected by the environment or are volatile, forming tiny particles that effectively protect the shelf life and usability of the core material. Although microcapsule technology can reduce the volatilization of active ingredients in fragrances, facilitate storage, and prevent oxidation, thus improving their retention, in practical use, microcapsules have problems such as poor flexibility and easy breakage, resulting in a short fragrance retention time.
[0020] This invention uses double-walled microcapsules. Because they have two layers of walls, the physicochemical properties of each layer can complement each other, synergistically improving the quality of the microcapsules, increasing their applicability, improving the mechanical strength and resistance to breakage of the microcapsules, significantly improving the sustained-release properties of the fragrance, and enhancing the aroma retention, persistence and stability.
[0021] The first layer wall material, β-cyclodextrin, has excellent encapsulation properties, allowing for the production of well-shaped microcapsules with uniform particle size distribution at room temperature. These microcapsules exhibit high-temperature resistance, prolonged aroma retention time, and improved sustained-release performance. This invention employs a coagulation method under the action of a porogen in the preparation of the outer capsule wall. Two or more linear, random polymer materials with opposite charges are used as wall materials. Changing the pH of the system causes electrostatic attraction between the oppositely charged polymers, reducing their solubility and resulting in phase separation, thus achieving encapsulation. Under the action of the porogen, the outer wall material forms a porous structure, thereby improving the sustained-release performance of the fragrance, enabling it to slowly release aroma, enhancing the storage stability of the microcapsule product, and extending its shelf life.
[0022] The peach flavoring prepared by this invention has a rich flavor, pure and delicate aroma, sustained release, and improved resistance to breakage. It enhances the aroma retention, persistence and stability, increases its applicability, improves the storage stability of microcapsule products, and extends their shelf life, thus having broad application prospects. Detailed Implementation
[0023] The technical solutions in the embodiments of the present invention will be clearly and completely described below. 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.
[0024] Bacillus subtilis, 20 billion CFU / g, purchased from Shandong Zhenyi Development Chemical Co., Ltd.; Lactobacillus casei, 10 billion CFU / g, purchased from Guangdong Mingtong Biotechnology Co., Ltd.
[0025] Preparation of Bacillus subtilis seed culture: Bacillus subtilis was inoculated into LB medium and activated at 50℃ and 100 r / min for 24 h to obtain a bacterial count of 10. 8 -10 9 CFU / mL bacterial seed solution.
[0026] Preparation of Lactobacillus casei seed culture: Lactobacillus casei was inoculated into slant agar medium and activated at 37℃ under anaerobic conditions at 100 r / min for 24 h to obtain a culture with a bacterial count of 10. 8 -10 9 CFU / mL bacterial seed solution.
[0027] Cellulase, 50,000 U / g, transglutaminase, 1,000 U / g, purchased from Xiasheng (Beijing) Biotechnology Development Co., Ltd. Fig protease, 10,000 U / g, purchased from Hebei Pengyu Biotechnology Co., Ltd.
[0028] Chitosan, content >99%, purchased from Huantai County Jinhu Chitosan Products Co., Ltd.
[0029] Silk fibroin peptides, with a content >90%, were purchased from Shaanxi Bolin Biotechnology Co., Ltd.
[0030] The preparation method of carboxylated chitosan refers to existing technology (Li Fulan, et al. Synthesis of carboxylated chitosan and its adsorption of heavy metals [J]. Journal of Anhui Normal University (Natural Science Edition), 2016, 39(5): 445-448), specifically as follows: Dissolve 2.00g of chitosan in 60mL of 1% acetic acid aqueous solution, and add 3.20g of... α-Ketoglutaric acid was stirred at 37°C for 24 hours. Then, 0.80 g of sodium borohydride was added to the solution, and the reaction was continued at 37°C for 10 hours. The reaction was terminated with 95% ethanol to obtain a fibrous solid. After filtration, the solid was washed three times with ethanol and ether, and then dried naturally to obtain N-ketoglutaric acid-chitosan. The prepared N-ketoglutaric acid-chitosan (1.00 g) and sodium hydroxide (1.36 g) were added to 40 mL of distilled water and stirred thoroughly at 60°C to alkalize and swell for 1 hour. Then, 10 mL of a solution containing 0.10 g of chloroacetic acid was added, and the reaction was continued at 60°C for 10 hours. After precipitation with acetone, the solid was filtered, washed thoroughly with 95% ethanol, and dried to obtain carboxylated chitosan.
[0031] Example 1 This embodiment provides a method for preparing peach flavoring, including the following steps: S1. Enzymatic hydrolysis: Peel and pit the peaches, freeze-dry them, and pulverize them to obtain peach powder. Add 10g of peach powder to 70mL of water, add 0.5g of compound enzyme, and enzymatically hydrolyze at 40℃ for 1h to inactivate the enzyme and obtain the enzymatic hydrolysis product. The complex enzyme is a mixture of cellulase and fig protease in a mass ratio of 10:3. S2. Fermentation: Sterilize the enzymatic hydrolysis product from step S1, inoculate with seed culture of Bacillus subtilis and Lactobacillus casei, with inoculation amounts of 1 v / v% and 0.5 v / v%, respectively, ferment at 36℃ and 100 r / min for 24 h, filter, dry the filtrate, and obtain the fermentation product; S3. Supercritical fluid extraction: The fermentation product from step S2 is subjected to supercritical fluid extraction to obtain an extract; The supercritical fluid extraction conditions were: CO2 flow rate of 25 L / h, extraction pressure of 30 MPa, extraction temperature of 40 °C, desorption pressure of 9.5 MPa, desorption temperature of 50 °C, extraction time of 1 h, and ethanol as the entrainer at a dosage of 1%. S4. Molecular distillation: Add the extract obtained in step S3 into a molecular distillation apparatus, heat to 50°C to remove the distillate, heat to 115°C, and collect the distillate; S5. Preparation of the fresh-keeping and fragrance-locking cage: Dissolve 10g of carboxylated chitosan in water, add 3g of N-hydroxysuccinimide and 4g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, stir and activate at room temperature for 1h, add 7g of silk fibroin peptide, stir and react for 10h, add 5g of the distillate from step S4, freeze dry, and obtain the fresh-keeping and fragrance-locking cage; S6. Double-layer embedding: Dissolve 15g of β-cyclodextrin in 100mL of water, add 7g of the preservative and fragrance lock from step S5 and 0.5g of lecithin, heat to 45℃, stir and react for 2h, centrifuge, freeze dry to obtain a single-layer embedded particle. Add 15g of the single-layer embedded particle, 17g of gelatin, 2g of silk fibroin peptide, and 0.5g of pore-forming agent cetyltrimethylammonium chloride to 200mL of water, add 1g of vitamin E and 0.5g of Span-80, homogenize at 10000r / min for 10min, adjust the pH of the solution to 4, stir and react for 20min, then adjust the pH of the solution to 6.4, add 3g of transglutaminase, stir and react for 2h, centrifuge, wash, and dry to obtain peach flavoring.
[0032] Example 2 This embodiment provides a method for preparing peach flavoring, including the following steps: S1. Enzymatic hydrolysis: Peel and pit the peaches, freeze-dry them, pulverize them to obtain peach powder. Add 10g of peach powder to 100mL of water, add 1g of compound enzyme, and enzymatically hydrolyze at 50℃ for 3h to inactivate the enzyme and obtain the enzymatic hydrolysis product. The complex enzyme is a mixture of cellulase and fig protease in a mass ratio of 10:5. S2. Fermentation: Sterilize the enzymatic hydrolysis product from step S1, inoculate with seed culture of Bacillus subtilis and Lactobacillus casei, with inoculation amounts of 2 v / v% and 1.5 v / v%, respectively, at 40℃ and 200 r / min, ferment for 36 h, filter, dry the filtrate, and obtain the fermentation product; S3. Supercritical fluid extraction: The fermentation product from step S2 is subjected to supercritical fluid extraction to obtain an extract; The supercritical fluid extraction conditions were: CO2 flow rate of 32 L / h, extraction pressure of 35 MPa, extraction temperature of 50 °C, desorption pressure of 10.5 MPa, desorption temperature of 60 °C, extraction time of 2 h, and ethanol as the entrainer at an addition amount of 2%. S4. Molecular distillation: Add the extract obtained in step S3 into a molecular distillation apparatus, heat to 60°C to remove the distillate, heat to 135°C, and collect the distillate; S5. Preparation of the fresh-keeping and fragrance-locking cage: Dissolve 12g of carboxylated chitosan in water, add 5g of N-hydroxysuccinimide and 6g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, stir and activate at room temperature for 2h, add 10g of silk fibroin peptide, stir and react for 12h, add 7g of the distillate from step S4, freeze dry, and obtain the fresh-keeping and fragrance-locking cage; S6. Double-layer embedding: Dissolve 20g of β-cyclodextrin in 100mL of water, add 10g of the preservative and 1g of lecithin from step S5, heat to 55℃, stir and react for 4h, centrifuge, freeze dry to obtain a single-layer embedded particle. Add 20g of the single-layer embedded particle, 22g of gelatin, 3g of silk fibroin peptide, and 1g of pore-forming agent cetyltrimethylammonium chloride to 200mL of water, add 2g of vitamin E and 1g of Span-60, homogenize at 12000r / min for 20min, adjust the pH of the solution to 4.5, stir and react for 40min, then adjust the pH of the solution to 6.7, add 5g of transglutaminase, stir and react for 4h, centrifuge, wash, and dry to obtain peach flavoring.
[0033] Example 3 This embodiment provides a method for preparing peach flavoring, including the following steps: S1. Enzymatic hydrolysis: Peel and pit the peaches, freeze-dry them, and pulverize them to obtain peach powder. Add 10g of peach powder to 85mL of water, add 0.7g of compound enzyme, and enzymatically hydrolyze at 45℃ for 2h to inactivate the enzyme and obtain the enzymatic hydrolysis product. The complex enzyme is a mixture of cellulase and fig protease in a mass ratio of 10:4. S2. Fermentation: Sterilize the enzymatic hydrolysis product from step S1, inoculate with seed culture of Bacillus subtilis and Lactobacillus casei, with inoculation amounts of 1.5 v / v% and 1 v / v%, respectively, ferment at 38℃ and 150 r / min for 30 h, filter, dry the filtrate, and obtain the fermentation product; S3. Supercritical fluid extraction: The fermentation product from step S2 is subjected to supercritical fluid extraction to obtain an extract; The supercritical fluid extraction conditions were: CO2 flow rate of 25 L / h, extraction pressure of 32 MPa, extraction temperature of 45 °C, desorption pressure of 10 MPa, desorption temperature of 55 °C, extraction time of 1.5 h, with ethanol as the entrainer and an addition amount of 1.5%. S4. Molecular distillation: Add the extract obtained in step S3 into a molecular distillation apparatus, heat to 55°C to remove the distillate, heat to 125°C, and collect the distillate; S5. Preparation of the fresh-keeping and fragrance-locking cage: Dissolve 11g of carboxylated chitosan in water, add 4g of N-hydroxysuccinimide and 5g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, stir and activate at room temperature for 1.5h, add 8g of silk fibroin peptide, stir and react for 11h, add 6g of the distillate from step S4, freeze dry, and obtain the fresh-keeping and fragrance-locking cage; S6. Double-layer embedding: Dissolve 17g of β-cyclodextrin in 100mL of water, add 8g of the preservative and fragrance lock from step S5 and 0.7g of lecithin, heat to 50℃, stir and react for 3h, centrifuge, freeze dry to obtain a single-layer embedded particle. Add 17g of the single-layer embedded particle, 20g of gelatin, 2.5g of silk fibroin peptide, and 0.7g of pore-forming agent cetyl dimethyl benzyl chloride to 200mL of water, add 1.5g of vitamin E and 0.7g of Span-85, homogenize at 11000r / min for 15min, adjust the pH of the solution to 4.2, stir and react for 30min, then adjust the pH of the solution to 6.5, add 4g of transglutaminase, stir and react for 3h, centrifuge, wash, and dry to obtain peach flavoring.
[0034] Example 4 The difference from Example 3 is that the complex enzyme is replaced by a single cellulase.
[0035] Example 5 The difference from Example 3 is that the complex enzyme is replaced by a single fig protease.
[0036] Comparative Example 1 The difference from Example 3 is that no complex enzyme was added in step S1.
[0037] Specifically as follows: S1. Peel and pit the peaches, freeze-dry them, and pulverize them to obtain peach powder. Add 10g of peach powder to 85mL of water, heat to boiling and extract for 2 hours to obtain the extract.
[0038] Comparative Example 2 The difference from Example 3 is that Bacillus subtilis seed culture was not inoculated in step S2.
[0039] Specifically as follows: S2. Fermentation: Sterilize the enzymatic hydrolysis product from step S1, inoculate with Lactobacillus casei seed culture at an inoculation rate of 2.5 v / v%, ferment at 38℃ and 150 r / min for 30 h, filter, dry the filtrate, and obtain the fermentation product.
[0040] Comparative Example 3 The difference from Example 3 is that no Lactobacillus casei seed solution was inoculated in step S2.
[0041] Specifically as follows: S2. Fermentation: Sterilize the enzymatic hydrolysis product from step S1, inoculate with Bacillus subtilis seed liquid at an inoculation rate of 2.5 v / v%, ferment at 38℃ and 150 r / min for 30 h, filter, dry the filtrate, and obtain the fermentation product.
[0042] Comparative Example 4 The difference from Example 3 is that step S2 was not performed.
[0043] Specifically as follows: S1. Enzymatic hydrolysis: Peel and pit the peaches, freeze-dry them, and pulverize them to obtain peach powder. Add 10g of peach powder to 85mL of water, add 0.7g of compound enzyme, and enzymatically hydrolyze at 45℃ for 2h to inactivate the enzyme and obtain the enzymatic hydrolysis product. The complex enzyme is a mixture of cellulase and fig protease in a mass ratio of 10:4. S2. Supercritical fluid extraction: The enzymatic hydrolysis product from step S1 is subjected to supercritical fluid extraction to obtain an extract. The supercritical fluid extraction conditions were: CO2 flow rate of 25 L / h, extraction pressure of 32 MPa, extraction temperature of 45 °C, desorption pressure of 10 MPa, desorption temperature of 55 °C, extraction time of 1.5 h, with ethanol as the entrainer and an addition amount of 1.5%. S3. Molecular distillation: Add the extract obtained in step S2 into a molecular distillation apparatus, heat to 55°C to remove the distillate, heat to 125°C, and collect the distillate; S4. Preparation of the fresh-keeping and fragrance-locking cage: Dissolve 11g of carboxylated chitosan in water, add 4g of N-hydroxysuccinimide and 5g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, stir and activate at room temperature for 1.5h, add 8g of silk fibroin peptide, stir and react for 11h, add 6g of the distillate from step S3, freeze dry, and obtain the fresh-keeping and fragrance-locking cage; S5. Double-layer embedding: Dissolve 17g of β-cyclodextrin in 100mL of water, add 8g of the preservative and fragrance lock from step S4 and 0.7g of lecithin, heat to 50℃, stir and react for 3h, centrifuge, freeze dry to obtain a single-layer embedded particle. Add 17g of the single-layer embedded particle, 20g of gelatin, 2.5g of silk fibroin peptide, and 0.7g of pore-forming agent cetyl dimethyl benzyl chloride to 200mL of water, add 1.5g of vitamin E and 0.7g of Span-85, homogenize at 11000r / min for 15min, adjust the pH of the solution to 4.2, stir and react for 30min, then adjust the pH of the solution to 6.5, add 4g of transglutaminase, stir and react for 3h, centrifuge, wash, and dry to obtain peach flavoring.
[0044] Comparative Example 5 The difference from Example 3 is that step S3 was not performed.
[0045] Specifically as follows: S1. Enzymatic hydrolysis: Peel and pit the peaches, freeze-dry them, and pulverize them to obtain peach powder. Add 10g of peach powder to 85mL of water, add 0.7g of compound enzyme, and enzymatically hydrolyze at 45℃ for 2h to inactivate the enzyme and obtain the enzymatic hydrolysis product. The complex enzyme is a mixture of cellulase and fig protease in a mass ratio of 10:4. S2. Fermentation: Sterilize the enzymatic hydrolysis product from step S1, inoculate with Bacillus subtilis and Lactobacillus casei seed culture at inoculation amounts of 1.5 v / v% and 1 v / v%, respectively, at 38℃ and 150 r / min, ferment for 30 h, filter, and the filtrate is the fermentation product; S3. Molecular distillation: Add the fermentation product obtained in step S3 into a molecular distillation apparatus, heat to 55°C to remove the distillate, heat to 125°C, and collect the distillate; S4. Preparation of the fresh-keeping and fragrance-locking cage: Dissolve 11g of carboxylated chitosan in water, add 4g of N-hydroxysuccinimide and 5g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, stir and activate at room temperature for 1.5h, add 8g of silk fibroin peptide, stir and react for 11h, add 6g of the distillate from step S3, freeze dry, and obtain the fresh-keeping and fragrance-locking cage; S5. Double-layer embedding: Dissolve 17g of β-cyclodextrin in 100mL of water, add 8g of the preservative and fragrance lock from step S4 and 0.7g of lecithin, heat to 50℃, stir and react for 3h, centrifuge, freeze dry to obtain a single-layer embedded particle. Add 17g of the single-layer embedded particle, 20g of gelatin, 2.5g of silk fibroin peptide, and 0.7g of pore-forming agent cetyl dimethyl benzyl chloride to 200mL of water, add 1.5g of vitamin E and 0.7g of Span-85, homogenize at 11000r / min for 15min, adjust the pH of the solution to 4.2, stir and react for 30min, then adjust the pH of the solution to 6.5, add 4g of transglutaminase, stir and react for 3h, centrifuge, wash, and dry to obtain peach flavoring.
[0046] Comparative Example 6 The difference from Example 3 is that step S4 was not performed.
[0047] Specifically as follows: S1. Enzymatic hydrolysis: Peel and pit the peaches, freeze-dry them, and pulverize them to obtain peach powder. Add 10g of peach powder to 85mL of water, add 0.7g of compound enzyme, and enzymatically hydrolyze at 45℃ for 2h to inactivate the enzyme and obtain the enzymatic hydrolysis product. The complex enzyme is a mixture of cellulase and fig protease in a mass ratio of 10:4. S2. Fermentation: Sterilize the enzymatic hydrolysis product from step S1, inoculate with seed culture of Bacillus subtilis and Lactobacillus casei, with inoculation amounts of 1.5 v / v% and 1 v / v%, respectively, ferment at 38℃ and 150 r / min for 30 h, filter, dry the filtrate, and obtain the fermentation product; S3. Supercritical fluid extraction: The fermentation product from step S2 is subjected to supercritical fluid extraction to obtain an extract; The supercritical fluid extraction conditions were: CO2 flow rate of 25 L / h, extraction pressure of 32 MPa, extraction temperature of 45 °C, desorption pressure of 10 MPa, desorption temperature of 55 °C, extraction time of 1.5 h, with ethanol as the entrainer and an addition amount of 1.5%. S4. Preparation of the freshness-preserving and fragrance-locking cage: Dissolve 11g of carboxylated chitosan in water, add 4g of N-hydroxysuccinimide and 5g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, stir and activate at room temperature for 1.5h, add 8g of silk fibroin peptide, stir and react for 11h, add 6g of the extract from step S3, freeze dry, and obtain the freshness-preserving and fragrance-locking cage; S5. Double-layer embedding: Dissolve 17g of β-cyclodextrin in 100mL of water, add 8g of the preservative and fragrance lock from step S4 and 0.7g of lecithin, heat to 50℃, stir and react for 3h, centrifuge, freeze dry to obtain a single-layer embedded particle. Add 17g of the single-layer embedded particle, 20g of gelatin, 2.5g of silk fibroin peptide, and 0.7g of pore-forming agent cetyl dimethyl benzyl chloride to 200mL of water, add 1.5g of vitamin E and 0.7g of Span-85, homogenize at 11000r / min for 15min, adjust the pH of the solution to 4.2, stir and react for 30min, then adjust the pH of the solution to 6.5, add 4g of transglutaminase, stir and react for 3h, centrifuge, wash, and dry to obtain peach flavoring.
[0048] Comparative Example 7 The difference from Example 3 is that step S5 was not performed.
[0049] Specifically as follows: S1. Enzymatic hydrolysis: Peel and pit the peaches, freeze-dry them, and pulverize them to obtain peach powder. Add 10g of peach powder to 85mL of water, add 0.7g of compound enzyme, and enzymatically hydrolyze at 45℃ for 2h to inactivate the enzyme and obtain the enzymatic hydrolysis product. The complex enzyme is a mixture of cellulase and fig protease in a mass ratio of 10:4. S2. Fermentation: Sterilize the enzymatic hydrolysis product from step S1, inoculate with seed culture of Bacillus subtilis and Lactobacillus casei, with inoculation amounts of 1.5 v / v% and 1 v / v%, respectively, ferment at 38℃ and 150 r / min for 30 h, filter, dry the filtrate, and obtain the fermentation product; S3. Supercritical fluid extraction: The fermentation product from step S2 is subjected to supercritical fluid extraction to obtain an extract; The supercritical fluid extraction conditions were: CO2 flow rate of 25 L / h, extraction pressure of 32 MPa, extraction temperature of 45 °C, desorption pressure of 10 MPa, desorption temperature of 55 °C, extraction time of 1.5 h, with ethanol as the entrainer and an addition amount of 1.5%. S4. Molecular distillation: Add the extract obtained in step S3 into a molecular distillation apparatus, heat to 55°C to remove the distillate, heat to 125°C, and collect the distillate; S5. Double-layer embedding: Dissolve 17g of β-cyclodextrin in 100mL of water, add 8g of the distillate from step S4 and 0.7g of lecithin, heat to 50℃, stir for 3h, centrifuge, freeze dry to obtain a single-layer embedded particle. Add 17g of the single-layer embedded particle, 20g of gelatin, 2.5g of silk fibroin peptide, and 0.7g of pore-forming agent cetyl dimethyl benzyl chloride to 200mL of water, add 1.5g of vitamin E and 0.7g of Span-85, homogenize at 11000r / min for 15min, adjust the pH of the solution to 4.2, stir for 30min, then adjust the pH of the solution to 6.5, add 4g of transglutaminase, stir for 3h, centrifuge, wash, and dry to obtain peach flavoring.
[0050] Comparative Example 8 The difference from Example 3 is that step S6 was not performed.
[0051] Specifically as follows: S1. Enzymatic hydrolysis: Peel and pit the peaches, freeze-dry them, and pulverize them to obtain peach powder. Add 10g of peach powder to 85mL of water, add 0.7g of compound enzyme, and enzymatically hydrolyze at 45℃ for 2h to inactivate the enzyme and obtain the enzymatic hydrolysis product. The complex enzyme is a mixture of cellulase and fig protease in a mass ratio of 10:4. S2. Fermentation: Sterilize the enzymatic hydrolysis product from step S1, inoculate with seed culture of Bacillus subtilis and Lactobacillus casei, with inoculation amounts of 1.5 v / v% and 1 v / v%, respectively, ferment at 38℃ and 150 r / min for 30 h, filter, dry the filtrate, and obtain the fermentation product; S3. Supercritical fluid extraction: The fermentation product from step S2 is subjected to supercritical fluid extraction to obtain an extract; The supercritical fluid extraction conditions were: CO2 flow rate of 25 L / h, extraction pressure of 32 MPa, extraction temperature of 45 °C, desorption pressure of 10 MPa, desorption temperature of 55 °C, extraction time of 1.5 h, with ethanol as the entrainer and an addition amount of 1.5%. S4. Molecular distillation: Add the extract obtained in step S3 into a molecular distillation apparatus, heat to 55°C to remove the distillate, heat to 125°C, and collect the distillate; S5. Preparation of the freshness-preserving and fragrance-locking cage: Dissolve 11g of carboxylated chitosan in water, add 4g of N-hydroxysuccinimide and 5g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, stir and activate at room temperature for 1.5h, add 8g of silk fibroin peptide, stir and react for 11h, add 6g of the distillate from step S4, freeze dry to obtain the freshness-preserving and fragrance-locking cage, which is the peach flavoring.
[0052] Test Example 1 The components of the distillates obtained in Examples 1-5 and Comparative Examples 1-5 of the present invention were analyzed by GC / MS.
[0053] Chromatographic column: PE-5MS capillary column (30m×0.25mm×0.25μm); injection port temperature 250℃; carrier gas: high-purity helium; flow rate 1.0 mL / min; injection volume 2μL; split ratio 50:1; temperature program 50℃ (1min) → 5℃ / min → 250℃ (3min).
[0054] Mass spectrometry conditions: EI ion source; ionization energy 70 eV; ion source temperature 190 °C; transfer line temperature 250 °C; scan range 35-450 u. Spectral searches were performed using the WILEY and NIST spectral libraries.
[0055] The results are shown in Table 1.
[0056] Table 1
[0057] As can be seen from the table above, the distillates obtained in Examples 1-3 of the present invention contain abundant active components.
[0058] Test Example 2 The sustained-release performance of the peach flavorings prepared in Examples 1-3 and Comparative Examples 7 and 8 of this invention was tested.
[0059] The sustained-release properties of peach flavoring are described as follows: Remaining flavor fraction w (%) at different times = Remaining flavor fraction m on day t t / Initial mass of fragrance m0 × 100% The results are shown in Table 2.
[0060] Table 2 As can be seen from the table above, the peach flavorings prepared in Examples 1-3 of this invention have good sustained-release properties.
[0061] Test Example 3 Twenty fragrance evaluators were selected to conduct aroma evaluations. Based on GB / T 14454.2-2008 "Methods for Evaluating the Aroma of Fragrances," the evaluators conducted sensory evaluations. Preliminary simulated evaluations showed that the evaluators could distinguish the differences between various peach aroma samples. Simultaneously, a top-quality commercially available peach flavoring was provided to all evaluators as a control sample. Evaluators scored the sample's aroma on a scale of 1-9 based on its similarity to the control sample's peach aroma; higher scores indicated closer similarity, while lower scores indicated off-odors, sharp aromas, or bland aromas. Finally, the evaluators' scores were statistically analyzed, outliers were analyzed and removed using the Q-test, and the average score was calculated.
[0062] The results are shown in Table 3.
[0063] Table 3 Example 1 8.9 Example 2 9.0 Example 3 9.0 Example 4 8.4 Example 5 8.3 Comparative Example 1 7.9 Comparative Example 2 7.2 Comparative Example 3 7.4 Comparative Example 4 6.8 Comparative Example 5 6.1 Comparative Example 6 6.5 Comparative Example 7 7.0 Comparative Example 8 8.1 As can be seen from the table above, the peach flavorings prepared in Examples 1-3 of this invention have high sensory evaluation, rich flavor, and pure and delicate aroma.
[0064] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A method for preparing peach flavoring, characterized in that, Specifically, the following steps are included: S1. Enzymatic hydrolysis: Peel and pit the peaches, freeze-dry them, pulverize them to obtain peach powder, add water, the solid-liquid ratio of the peach powder to water is 1:(7-10), g / mL; add a compound enzyme, the mass ratio of the peach powder to the compound enzyme is 10:0.5-1, enzymatic hydrolysis is carried out at 40-50℃ for 1-3 hours, enzyme is inactivated, and the enzymatic hydrolysis product is obtained; The complex enzyme is a mixture of cellulase and fig protease in a mass ratio of 10:3-5. S2. Fermentation: Sterilize the enzymatic hydrolysis product from step S1, inoculate with Bacillus subtilis and Lactobacillus casei seed culture at inoculation amounts of 1-2 v / v% and 0.5-1.5 v / v%, respectively, at 36-40℃ and 100-200 r / min, ferment for 24-36 h, filter, dry the filtrate, and obtain the fermentation product; S3. Supercritical fluid extraction: The fermentation product from step S2 is subjected to supercritical fluid extraction to obtain an extract; The supercritical fluid extraction conditions are: CO2 flow rate of 25-32 L / h, extraction pressure of 30-35 MPa, extraction temperature of 40-50℃, desorption pressure of 9.5-10.5 MPa, desorption temperature of 50-60℃, extraction time of 1-2 h, and ethanol as the entrainer, with an addition amount of 1-2%. S4. Molecular distillation: Add the extract obtained in step S3 into a molecular distillation apparatus, heat to 50-60℃ to remove the distillate, heat to 115-135℃, and collect the distillate; S5. Preparation of the fresh-keeping and fragrance-locking cage: Dissolve 10-12 parts by weight of carboxylated chitosan in water, add 3-5 parts by weight of N-hydroxysuccinimide and 4-6 parts by weight of 1-ethyl-(3-dimethylaminopropyl)carbodiimide, stir and activate at room temperature for 1-2 hours, add 7-10 parts by weight of silk fibroin peptide, stir and react for 10-12 hours, add 5-7 parts by weight of the distillate from step S4, freeze-dry to obtain the fresh-keeping and fragrance-locking cage; S6. Double-layer embedding: Dissolve 15-20 parts by weight of β-cyclodextrin in 100 parts by weight of water, add 7-10 parts by weight of the preservative and fragrance-locking agent obtained in step S5 and 0.5-1 parts by weight of lecithin, heat to 45-55℃, stir and react for 2-4 hours, centrifuge, freeze dry to obtain a single-layer embedded particle. Add 15-20 parts by weight of the single-layer embedded particle, 17-22 parts by weight of gelatin, 2-3 parts by weight of silk fibroin peptide, and 0.5-1 parts by weight of pore-forming agent to 200 parts by weight of water. Add 1-2 parts by weight of vitamin E and 0.5-1 parts by weight of lipophilic emulsifier, homogenize at 10000-12000 r / min for 10-20 min, adjust the pH of the solution to 4-4.5, stir for 20-40 min, then adjust the pH of the solution to 6.4-6.7, add 3-5 parts by weight of transglutaminase, stir for 2-4 h, centrifuge, wash, and dry to obtain peach flavoring; the pore-forming agent is hexadecyltrimethylammonium chloride.
2. The preparation method according to claim 1, characterized in that, The lipophilic emulsifier mentioned in step S6 is selected from at least one of Span-20, Span-40, Span-60, Span-80, and Span-85.
3. A peach flavoring prepared by the method described in claim 1 or 2.
Citation Information
Patent Citations
Peach fermented product and preparation method thereof
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