Preparation method of chaozhou flavor old medicine orange essence

Abstract

The application belongs to the technical field of essence, and specifically discloses a preparation method of a Chaozhou-flavor old medicine orange essence. The old medicine orange is subjected to enzymatic hydrolysis treatment by using a composite enzyme system of cellulase, pectinase, amylase and flavor protease. The composite enzyme can break the cell wall structure of the old medicine orange, degrade starch and protein impurities, avoid the target components from being adsorbed and wrapped by macromolecular matrix, maximize the release of aroma components combined with macromolecules under mild conditions, effectively improve the dissolution effect of aroma components, and improve the softness of aroma. The diatomite is used to adsorb insoluble impurities such as residual undecomposed peel fragments, protein precipitates and colloids. The 0.22-0.45 μm filter membrane is used to intercept large-particle impurities. The water vapor distillation is used to realize the separation of aroma components from water phase and non-volatile impurities. Then, the dichloromethane extraction is used to effectively enrich the components with aged aroma and medicine aroma in the old medicine orange, so that the essence flavor is more full and the layering is stronger.

Description

Technical Field

[0001] This invention relates to the field of flavor technology, specifically to a method for preparing Chaoshan-style aged tangerine flavor. Background Technology

[0002] Aged medicinal kumquat is a traditional pickled food from the Chaoshan region, made from kumquats and aged with salt, sugar, licorice, fritillaria, and other ingredients. It possesses a unique complex flavor profile, combining aged, citrus, medicinal, and sweet notes. Its aroma components are complex, including terpenes, aldehydes, ketones, glycyrrhizic acid, and polysaccharide derivatives. The market demand for natural aged medicinal kumquat flavoring as a flavoring additive in food, beverages, and tobacco products is growing.

[0003] The current preparation of natural aged tangerine flavorings mostly adopts a single alcohol extraction or water extraction process, which has the following problems: First, the peel of aged tangerines is rich in cellulose and pectin, and the pulp contains starch and protein substances. Single extraction is difficult to release the aroma components encapsulated in the macromolecular structure, resulting in a weak aroma of the flavoring; Second, the extraction process is not targeted enough and it is difficult to enrich the aroma components at the same time, resulting in poor flavor harmony.

[0004] Therefore, this application is submitted. Summary of the Invention

[0005] This invention provides a method for preparing Chaoshan-style aged tangerine flavoring. The method obtained in this application can effectively enrich the components with aged aroma and medicinal aroma in aged tangerines, making the flavoring more full-bodied and more layered.

[0006] The present invention solves its technical problem by adopting the following technical solution: A method for preparing a traditional Chinese medicine citrus flavoring includes the following steps: (1) Pulverize old tangerine peel to obtain old tangerine peel powder, add compound enzyme and old tangerine peel powder to water, enzymatically hydrolyze to obtain enzymatic hydrolysate, add diatomaceous earth, stir evenly, filter with a 0.22~0.45μm filter membrane to obtain impurity-removed solution; (2) Steam distill the purified liquid and collect the distillate; (3) Extract the distillate with dichloromethane to obtain the extract; (4) The extract was filtered through an ultrafiltration membrane with a molecular weight cutoff of 2 kDa and concentrated to obtain old citrus flavoring.

[0007] As an embodiment of this application, the particle size of the old medicinal orange powder is 50-500 mesh.

[0008] As an embodiment of this application, the complex enzyme comprises cellulase, pectinase, amylase and flavor protease in a mass ratio of 1:(0.8~1.2):(0.6~0.8):(0.4~0.6).

[0009] As an embodiment of this application, the mass ratio of the compound enzyme, aged tangerine powder, and water is (0.02~0.05):1:(8~20).

[0010] As an embodiment of this application, the enzymatic hydrolysis temperature is 42~48℃ and the time is 2~6h.

[0011] As an embodiment of this application, the mass ratio of the enzymatic hydrolysate to diatomaceous earth is 1:(0.02~0.05).

[0012] As an embodiment of this application, the particle size of the diatomaceous earth is 200-600 mesh.

[0013] As an embodiment of this application, the temperature of the steam distillation is 90~98℃ and the time is 2~8h.

[0014] As an embodiment of this application, the volume ratio of the distillate to dichloromethane is 1:(0.8~5).

[0015] This application also provides a traditional Chinese medicine orange flavoring, which is prepared using the preparation method described above.

[0016] The beneficial effects of this invention are as follows: This application uses a complex enzyme system of cellulase, pectinase, amylase and flavor protease to enzymatically hydrolyze aged tangerines. The complex enzymes can synergistically break down the cell wall structure of aged tangerines, degrade starch and protein impurities, and prevent the target components from being adsorbed and encapsulated by the macromolecular matrix. Under mild conditions, the aroma components bound to macromolecules are released to the maximum extent, effectively improving the dissolution effect of aroma components and enhancing the mellowness of the aroma. Diatomaceous earth adsorbs residual incompletely decomposed peel fragments, protein precipitates, colloids and other insoluble impurities. A 0.22~0.45μm filter membrane is used to retain large particulate impurities. Steam distillation is used to separate the aroma components from the aqueous phase and non-volatile impurities (such as small molecule sugars and residual salts produced by enzymatic hydrolysis). Then, dichloromethane extraction is used to effectively enrich the components with aged aroma and medicinal aroma in aged tangerines, making the flavor fuller and more layered. Detailed Implementation

[0017] 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 some embodiments of the present invention, 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.

[0018] In this invention, the technical features described in an open-ended manner include both closed-ended technical solutions composed of the listed features and open-ended technical solutions that include the listed features.

[0019] In this invention, numerical ranges are involved. Unless otherwise specified, the numerical ranges are considered continuous and include the minimum and maximum values ​​of the range, as well as every value between the minimum and maximum values. Furthermore, when the range refers to integers, it includes every integer between the minimum and maximum values ​​of the range. Additionally, when multiple ranges are provided to describe features or characteristics, the ranges may be merged. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all subranges to which they are included.

[0020] In this invention, there are no particular limitations on the specific dispersion and stirring methods.

[0021] Unless otherwise specified, all reagents or instruments used in this invention are commercially available conventional products. Unless otherwise specified, the raw materials used in each comparative example and the parallel experiments of each embodiment are the same commercially available products.

[0022] This application provides a method for preparing aged citrus flavoring, comprising the following steps: (1) Pulverize old tangerine peel to obtain old tangerine peel powder, add compound enzyme and old tangerine peel powder to water, enzymatically hydrolyze to obtain enzymatic hydrolysate, add diatomaceous earth, stir evenly, filter with a 0.22~0.45μm filter membrane to obtain impurity-removed solution; (2) Steam distill the purified liquid and collect the distillate; (3) Extract the distillate with dichloromethane to obtain the extract; (4) The extract was filtered through an ultrafiltration membrane with a molecular weight cutoff of 2 kDa and concentrated to obtain old citrus flavoring.

[0023] The inventors of this application have discovered that the characteristic aroma of *Citrus reticulata*, a traditional food and medicine source, is composed of various volatile and semi-volatile organic compounds, mainly including terpenes (such as myrcene and limonene), alcohols (such as linalool and citronellol), phenols (such as eugenol and maltol), esters (ethyl linoleate and ethyl linoleate), and fatty acids. These components collectively endow *Citrus reticulata* with its unique flavor and excellent antibacterial activity. The cell walls of *Citrus reticulata* have a cellulose framework and pectin as a filling matrix. Some aroma components are tightly bound to large molecules such as polysaccharides and proteins in the cell wall structure and are encapsulated within the plant cells. Simultaneously, *Citrus reticulata* contains a certain amount of starch molecules, which easily gelatinize in the extraction system to form colloids. These starch molecules adsorb and encapsulate some aroma components, reducing their dissolution rate in the solvent and increasing the difficulty of subsequent separation and purification.

[0024] This application employs a complex enzyme system of cellulase, pectinase, amylase, and flavor protease to enzymatically hydrolyze aged tangerines. The complex enzymes synergistically break down the cell wall structure of aged tangerines, degrade starch and protein impurities, and prevent the target components from being adsorbed and encapsulated by the macromolecular matrix. Under mild conditions, it maximizes the release of aroma components bound to macromolecules, effectively improving the dissolution effect of aroma components and enhancing the mellowness of the aroma. Diatomaceous earth adsorbs residual incompletely decomposed peel fragments, protein precipitates, colloids, and other insoluble impurities. A 0.22~0.45μm filter membrane is used to retain large particulate impurities. Steam distillation is used to separate aroma components from the aqueous phase and non-volatile impurities (such as small molecule sugars and residual salts produced by enzymatic hydrolysis). Then, dichloromethane extraction is used to effectively enrich the components with aged and medicinal aroma in aged tangerines, making the flavor fuller and more layered.

[0025] In some embodiments, the particle size of the aged tangerine powder is 50 to 500 mesh, for example, it can be 50 mesh, 100 mesh, 150 mesh, 200 mesh, 300 mesh, 400 mesh, 500 mesh or any two of these values.

[0026] In some embodiments, the complex enzyme comprises cellulase, pectinase, amylase, and flavor protease in a mass ratio of 1:(0.8~1.2):(0.6~0.8):(0.4~0.6). For example, the ratio can be 1:0.8:0.6:0.4, 1:1:0.7:0.5, 1:1.2:0.8:0.6, 1:0.8:0.8:0.4, 1:0.8:0.6:0.6, 1:0.8:0.8:0.6, 1:1.2:0.6:0.4, 1:1.2:0.8:0.6, or any two of these values. By controlling the proportion of the complex enzyme within this range, the dissolution effect of aroma components can be effectively improved.

[0027] In some embodiments, the mass ratio of the compound enzyme, aged tangerine powder, and water is (0.02~0.05):1:(8~20), for example, it can be 0.02:1:8, 0.03:1:10, 0.04:1:15, 0.05:1:20, 0.02:1:20, 0.05:1:8, or any two of these values.

[0028] In some embodiments, the enzymatic hydrolysis temperature is 42~48°C, for example, it can be 42°C, 43°C, 44°C, 45°C, 46°C, 47°C, 48°C or any two of these values.

[0029] In some embodiments, the enzymatic hydrolysis time is 2 to 6 hours, for example, it can be 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours, 5.5 hours, 6 hours or any two of these values.

[0030] In some embodiments, the mass ratio of the enzymatic hydrolysate to diatomaceous earth is 1:(0.02~0.05), for example, it can be 1:0.02.

[0031] In some embodiments, the diatomaceous earth has a particle size of 200 to 600 mesh, for example, it can be 200 mesh, 300 mesh, 400 mesh, 500 mesh, 600 mesh or any two of these values.

[0032] In some embodiments, the temperature of the steam distillation is 90~98°C, for example, it can be 90°C, 91°C, 92°C, 93°C, 94°C, 95°C, 96°C, 97°C, 98°C, 99°C or any two of these values.

[0033] In some embodiments, the steam distillation time is 2 to 8 hours, for example, it can be 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours, 5.5 hours, 6 hours, 6.5 hours, 7 hours, 7.5 hours, 8 hours or any two of these values.

[0034] In some embodiments, the volume ratio of the distillate to dichloromethane is 1:(0.8~5), for example, it can be 1:0.8, 1:1, 1:2, 1:3, 1:4, 1:5 or any two of these values.

[0035] In some embodiments, the aged tangerine peel conforms to the requirements of T / CZBXBZ 013-2023 "Three Treasures of Chaozhou (Preserved Fruits)".

[0036] This application also provides a traditional Chinese medicine orange flavoring, which is prepared using the preparation method described above.

[0037] The present application will be described in detail below through embodiments.

[0038] Example 1 A method for preparing a traditional Chinese medicine citrus flavoring includes the following steps: (1) Clean the old medicinal oranges (old medicinal oranges that have been pickled for one year), dry them in an oven at 70℃ for 4 hours, and pulverize them to 200 mesh to obtain old medicinal orange powder.

[0039] The compound enzyme and aged tangerine powder were added to water and stirred at 100 rpm for 10 minutes. The temperature was raised to 46°C and enzymatically hydrolyzed at 46°C for 3 hours to obtain the enzymatic hydrolysate. Diatomaceous earth with a particle size of 325 mesh was added to the enzymatic hydrolysate and stirred at 100 rpm for 1 hour. The solution was then filtered through a 0.22 μm filter membrane to obtain the purified solution.

[0040] The compound enzyme comprises cellulase, pectinase, amylase, and flavor protease in a mass ratio of 1:0.8:0.8:0.6; the mass ratio of the compound enzyme, aged tangerine powder, and water is 0.03:1:12. The mass ratio of the enzymatic hydrolysate and diatomaceous earth is 1:0.04.

[0041] (2) Add the impurity-removed liquid to the steam distillation equipment, add boiling stones to prevent bumping, and steam distill at 96°C for 5 hours. Then condense to obtain the distillate. (3) Extract the distillate with dichloromethane to obtain an extract; the volume ratio of the distillate to dichloromethane is 1:1.2; (4) The extract was filtered through an ultrafiltration membrane with a molecular weight cutoff of 2 kDa and concentrated at 42°C for 30 min using a rotary evaporator to obtain old citrus flavoring.

[0042] Example 2 A method for preparing a traditional Chinese medicine citrus flavoring includes the following steps: (1) Clean the old medicinal oranges (old medicinal oranges that have been pickled for one year), dry them in an oven at 70℃ for 4 hours, and pulverize them to 200 mesh to obtain old medicinal orange powder.

[0043] The compound enzyme and aged tangerine powder were added to water and stirred at 100 rpm for 10 minutes. The temperature was raised to 46°C and enzymatically hydrolyzed at 46°C for 3 hours to obtain the enzymatic hydrolysate. Diatomaceous earth with a particle size of 325 mesh was added to the enzymatic hydrolysate and stirred at 100 rpm for 1 hour. The solution was then filtered through a 0.22 μm filter membrane to obtain the purified solution.

[0044] The compound enzyme comprises cellulase, pectinase, amylase, and flavor protease in a mass ratio of 1:1.2:0.6:0.4; the mass ratio of the compound enzyme, aged tangerine powder, and water is 0.03:1:12. The mass ratio of the enzymatic hydrolysate and diatomaceous earth is 1:0.04.

[0045] (2) Add the impurity-removed liquid to the steam distillation equipment, add boiling stones to prevent bumping, and steam distill at 96°C for 5 hours. Then condense to obtain the distillate. (3) Extract the distillate with dichloromethane to obtain an extract; the volume ratio of the distillate to dichloromethane is 1:1.2; (4) The extract was filtered through an ultrafiltration membrane with a molecular weight cutoff of 2 kDa and concentrated at 42°C for 30 min using a rotary evaporator to obtain old citrus flavoring.

[0046] Example 3 A method for preparing a traditional Chinese medicine citrus flavoring includes the following steps: (1) Clean the old medicinal oranges (old medicinal oranges that have been pickled for one year), dry them in an oven at 70℃ for 4 hours, and pulverize them to 200 mesh to obtain old medicinal orange powder.

[0047] The compound enzyme and aged tangerine powder were added to water and stirred at 100 rpm for 10 minutes. The temperature was raised to 46°C and enzymatically hydrolyzed at 46°C for 3 hours to obtain the enzymatic hydrolysate. Diatomaceous earth with a particle size of 325 mesh was added to the enzymatic hydrolysate and stirred at 100 rpm for 1 hour. The solution was then filtered through a 0.22 μm filter membrane to obtain the purified solution.

[0048] The compound enzyme comprises cellulase, pectinase, amylase, and flavor protease in a mass ratio of 1:0.8:0.8:0.6; the mass ratio of the compound enzyme, aged tangerine powder, and water is 0.04:1:15. The mass ratio of the enzymatic hydrolysate and diatomaceous earth is 1:0.03.

[0049] (2) Add the impurity-removed liquid to a steam distillation apparatus, add boiling stones to prevent bumping, and steam distill at 95°C for 5 hours. Then condense to obtain the distillate. (3) Extract the distillate with dichloromethane to obtain an extract; the volume ratio of the distillate to dichloromethane is 1:1.5; (4) The extract was filtered through an ultrafiltration membrane with a molecular weight cutoff of 2 kDa and concentrated at 42°C for 30 min using a rotary evaporator to obtain old citrus flavoring.

[0050] Comparative Example 1 A method for preparing a traditional Chinese medicine citrus flavoring includes the following steps: (1) Clean the old medicinal oranges (old medicinal oranges that have been pickled for one year), dry them in an oven at 70℃ for 4 hours, and pulverize them to 200 mesh to obtain old medicinal orange powder.

[0051] The compound enzyme and aged tangerine powder were added to water and stirred at 100 rpm for 10 minutes. The temperature was raised to 46°C and enzymatically hydrolyzed at 46°C for 3 hours to obtain the enzymatic hydrolysate. Diatomaceous earth with a particle size of 325 mesh was added to the enzymatic hydrolysate and stirred at 100 rpm for 1 hour. The solution was then filtered through a 0.22 μm filter membrane to obtain the purified solution.

[0052] The compound enzyme comprises cellulase, pectinase, amylase, and flavor protease in a mass ratio of 1:0.5:1.5:1; the mass ratio of the compound enzyme, aged tangerine powder, and water is 0.03:1:12. The mass ratio of the enzymatic hydrolysate and diatomaceous earth is 1:0.04.

[0053] (2) Add the impurity-removed liquid to the steam distillation equipment, add boiling stones to prevent bumping, and steam distill at 96°C for 5 hours. Then condense to obtain the distillate. (3) Extract the distillate with dichloromethane to obtain an extract; the volume ratio of the distillate to dichloromethane is 1:1.2; (4) The extract was filtered through an ultrafiltration membrane with a molecular weight cutoff of 2 kDa and concentrated at 42°C for 30 min using a rotary evaporator to obtain old citrus flavoring.

[0054] Comparative Example 2 A method for preparing a traditional Chinese medicine citrus flavoring includes the following steps: (1) Clean the old medicinal oranges (old medicinal oranges that have been pickled for one year), dry them in an oven at 70℃ for 4 hours, and pulverize them to 200 mesh to obtain old medicinal orange powder.

[0055] The compound enzyme and aged tangerine powder were added to water and stirred at 100 rpm for 10 minutes. The temperature was raised to 46°C and enzymatically hydrolyzed at 46°C for 3 hours to obtain the enzymatic hydrolysate. Diatomaceous earth with a particle size of 325 mesh was added to the enzymatic hydrolysate and stirred at 100 rpm for 1 hour. The solution was then filtered through a 0.22 μm filter membrane to obtain the purified solution.

[0056] The compound enzyme comprises cellulase, pectinase, amylase, and flavor protease in a mass ratio of 1:2:0.2:0.2; the mass ratio of the compound enzyme, aged tangerine powder, and water is 0.03:1:12. The mass ratio of the enzymatic hydrolysate and diatomaceous earth is 1:0.04.

[0057] (2) Add the impurity-removed liquid to the steam distillation equipment, add boiling stones to prevent bumping, and steam distill at 96°C for 5 hours. Then condense to obtain the distillate. (3) Extract the distillate with dichloromethane to obtain an extract; the volume ratio of the distillate to dichloromethane is 1:1.2; (4) The extract was filtered through an ultrafiltration membrane with a molecular weight cutoff of 2 kDa and concentrated at 42°C for 30 min using a rotary evaporator to obtain old citrus flavoring.

[0058] Comparative Example 3 A method for preparing a traditional Chinese medicine citrus flavoring includes the following steps: (1) Clean the old medicinal oranges (old medicinal oranges that have been pickled for one year), dry them in an oven at 70℃ for 4 hours, and pulverize them to 200 mesh to obtain old medicinal orange powder.

[0059] The compound enzyme and aged tangerine powder were added to water and stirred at 100 rpm for 10 minutes. The temperature was raised to 46°C and enzymatically hydrolyzed at 46°C for 3 hours to obtain the enzymatic hydrolysate. Diatomaceous earth with a particle size of 325 mesh was added to the enzymatic hydrolysate and stirred at 100 rpm for 1 hour. The solution was then filtered through a 0.22 μm filter membrane to obtain the purified solution.

[0060] The compound enzyme comprises cellulase, pectinase, β-glucosidase, and neutral protease in a mass ratio of 1:0.8:0.8:0.6; the mass ratio of the compound enzyme, aged tangerine powder, and water is 0.03:1:12. The mass ratio of the enzymatic hydrolysate and diatomaceous earth is 1:0.04.

[0061] (2) Add the impurity-removed liquid to the steam distillation equipment, add boiling stones to prevent bumping, and steam distill at 96°C for 5 hours. Then condense to obtain the distillate. (3) Extract the distillate with dichloromethane to obtain an extract; the volume ratio of the distillate to dichloromethane is 1:1.2; (4) The extract was filtered through an ultrafiltration membrane with a molecular weight cutoff of 2 kDa and concentrated at 42°C for 30 min using a rotary evaporator to obtain old citrus flavoring.

[0062] Comparative Example 4 A method for preparing a traditional Chinese medicine citrus flavoring includes the following steps: (1) Clean the old medicinal oranges (old medicinal oranges that have been pickled for one year), dry them in an oven at 70℃ for 4 hours, and pulverize them to 200 mesh to obtain old medicinal orange powder.

[0063] The compound enzyme and aged tangerine powder were added to water and stirred at 100 rpm for 10 minutes. The temperature was raised to 46°C and enzymatically hydrolyzed at 46°C for 3 hours to obtain the enzymatic hydrolysate. Diatomaceous earth with a particle size of 325 mesh was added to the enzymatic hydrolysate and stirred at 100 rpm for 1 hour. The solution was then filtered through a 0.22 μm filter membrane to obtain the purified solution.

[0064] The complex enzyme comprises β-glucanase, papain, amylase, and flavor protease in a mass ratio of 1:0.8:0.8:0.6; the mass ratio of the complex enzyme, aged tangerine powder, and water is 0.03:1:12. The mass ratio of the enzymatic hydrolysate and diatomaceous earth is 1:0.04.

[0065] (2) Add the impurity-removed liquid to the steam distillation equipment, add boiling stones to prevent bumping, and steam distill at 96°C for 5 hours. Then condense to obtain the distillate. (3) Extract the distillate with dichloromethane to obtain an extract; the volume ratio of the distillate to dichloromethane is 1:1.2; (4) The extract was filtered through an ultrafiltration membrane with a molecular weight cutoff of 2 kDa and concentrated at 42°C for 30 min using a rotary evaporator to obtain old citrus flavoring.

[0066] Comparative Example 5 A method for preparing a traditional Chinese medicine citrus flavoring includes the following steps: (1) Clean the old medicinal oranges (old medicinal oranges that have been pickled for one year), dry them in an oven at 70℃ for 4 hours, and pulverize them to 200 mesh to obtain old medicinal orange powder.

[0067] The compound enzyme and aged tangerine powder were added to water and stirred at 100 rpm for 10 minutes. The temperature was raised to 46°C and enzymatically hydrolyzed at 46°C for 3 hours to obtain the enzymatic hydrolysate. Diatomaceous earth with a particle size of 325 mesh was added to the enzymatic hydrolysate and stirred at 100 rpm for 1 hour. The solution was then filtered through a 0.22 μm filter membrane to obtain the purified solution.

[0068] The compound enzyme comprises cellulase and pectinase in a mass ratio of 1:0.8; the mass ratio of the compound enzyme, aged tangerine powder, and water is 0.03:1:12. The mass ratio of the enzymatic hydrolysate and diatomaceous earth is 1:0.04.

[0069] (2) Add the impurity-removed liquid to the steam distillation equipment, add boiling stones to prevent bumping, and steam distill at 96°C for 5 hours. Then condense to obtain the distillate. (3) Extract the distillate with dichloromethane to obtain an extract; the volume ratio of the distillate to dichloromethane is 1:1.2; (4) The extract was filtered through an ultrafiltration membrane with a molecular weight cutoff of 2 kDa and concentrated at 42°C for 30 min using a rotary evaporator to obtain old citrus flavoring.

[0070] Comparative Example 6 A method for preparing a traditional Chinese medicine citrus flavoring includes the following steps: (1) Clean the old medicinal oranges (old medicinal oranges that have been pickled for one year), dry them in an oven at 70℃ for 4 hours, and pulverize them to 200 mesh to obtain old medicinal orange powder.

[0071] The compound enzyme and aged tangerine powder were added to water and stirred at 100 rpm for 10 minutes. The temperature was raised to 46°C and enzymatically hydrolyzed at 46°C for 3 hours to obtain the enzymatic hydrolysate. Diatomaceous earth with a particle size of 325 mesh was added to the enzymatic hydrolysate and stirred at 100 rpm for 1 hour. The solution was then filtered through a 0.22 μm filter membrane to obtain the purified solution.

[0072] The compound enzyme comprises cellulase, pectinase, amylase, and flavor protease in a mass ratio of 1:0.8:0.8:0.6; the mass ratio of the compound enzyme, aged tangerine powder, and water is 0.03:1:12. The mass ratio of the enzymatic hydrolysate and diatomaceous earth is 1:0.04.

[0073] (2) Add the impurity-removed liquid to the steam distillation equipment, add boiling stones to prevent bumping, and steam distill at 96°C for 5 hours. Then condense to obtain the distillate. (3) Extract the distillate with petroleum ether to obtain an extract; the volume ratio of the distillate to dichloromethane is 1:1.2; (4) The extract was filtered through an ultrafiltration membrane with a molecular weight cutoff of 2 kDa and concentrated at 42°C for 30 min using a rotary evaporator to obtain old citrus flavoring.

[0074] Test case 1. Sensory evaluation experiment: Evaluation panel: 10 trained sensory evaluators (no history of fragrance allergy, no odor sensitivity, and familiar with the flavor of old citrus).

[0075] Evaluation indicators: aroma intensity, purity of old tangerine aroma, and a 10-point scoring system (10 points is the best, and the scoring criteria are shown in Table 1).

[0076] Evaluation method: Take 50 μL of fragrance sample and drop it onto filter paper. Place the sample in an olfactory identification bottle. The evaluator smells the sample in an odor-free environment, records the score and describes the aroma characteristics, and calculates the total score. The total score for each item is 100 points.

[0077] Table 1

[0078] 2. Antibacterial activity verification Bacterial strains: Escherichia coli - strain ATCC 25922, Staphylococcus aureus - strain ATCC 6538.

[0079] Test method: Refer to the test method marked in QB / T 2738-2012.

[0080] Table 1

[0081] As can be seen from Table 1, the aged citrus flavoring prepared in this application has excellent aged aroma and medicinal aroma, rich aroma, harmonious flavor and mild taste, and also has excellent antibacterial properties.

[0082] Finally, it should be noted that the above embodiments are used to illustrate the technical solutions of the present invention and not to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A method for preparing aged citrus flavoring, characterized in that, Includes the following steps: (1) Pulverize old tangerine peel to obtain old tangerine peel powder, add compound enzyme and old tangerine peel powder to water, enzymatically hydrolyze to obtain enzymatic hydrolysate, add diatomaceous earth, stir evenly, filter with a 0.22~0.45μm filter membrane to obtain impurity-removed solution; (2) Steam distill the purified liquid and collect the distillate; (3) Extract the distillate with dichloromethane to obtain the extract; (4) The extract was filtered through an ultrafiltration membrane with a molecular weight cutoff of 2 kDa and concentrated to obtain old citrus flavoring.

2. The method for preparing aged citrus flavoring according to claim 1, characterized in that, The particle size of the aged tangerine powder is 50-500 mesh.

3. The method for preparing aged citrus flavoring according to claim 1, characterized in that, The complex enzyme comprises cellulase, pectinase, amylase and flavor protease in a mass ratio of 1:(0.8~1.2):(0.6~0.8):(0.4~0.6).

4. The method for preparing aged citrus flavoring according to claim 1, characterized in that, The mass ratio of the compound enzyme, aged tangerine powder, and water is (0.02~0.05):1:(8~20).

5. The method for preparing aged citrus flavoring according to claim 1, characterized in that, The enzymatic hydrolysis is performed at a temperature of 42-48℃ for 2-6 hours.

6. The method for preparing aged citrus flavoring according to claim 1, characterized in that, The mass ratio of the enzymatic hydrolysate to diatomaceous earth is 1:(0.02~0.05).

7. The method for preparing aged citrus flavoring according to claim 1, characterized in that, The diatomaceous earth has a particle size of 200-600 mesh.

8. The method for preparing aged citrus flavoring according to claim 1, characterized in that, The steam distillation temperature is 90~98℃, and the time is 2~8h.

9. The method for preparing aged citrus flavoring according to claim 1, characterized in that, The volume ratio of the distillate to dichloromethane is 1:(0.8~5).

10. A traditional Chinese medicine citrus flavoring, characterized in that, It is prepared by any one of the preparation methods described in claims 1 to 9.

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