Efficient production process for extracting anthocyanidin from zanthoxylum bungeanum

Abstract

The present invention relates to the technical field of the chemical extraction of plants, and relates to an efficient production process for extracting anthocyanidin from Zanthoxylum bungeanum. The process comprises: first subjecting dried Zanthoxylum bungeanum to winnowing, pulverization and enzymatic hydrolysis, so as to obtain an enzymatic hydrolysate, wherein in this step, an alkali treatment is replaced with the mild enzymatic hydrolysis to reduce corrosion to a device and the loss of the numbing flavor; adding the enzymatic hydrolysate to an acidic mixed solvent formulated from ethanol, pure water and citric acid, and performing ultrasonic extraction, wherein an acidic environment can stabilize anthocyanidin, and the ultrasonic treatment can accelerate mass transfer, thereby further improving the extraction efficiency and purity; after extraction, performing centrifugal separation and collecting an anthocyanidin-containing clear liquid, which can avoid extraction with organic solvents multiple times; then performing purification by using a macroporous adsorption resin, wherein by means of sample loading at a specific flow rate, rinsing with purified water and elution with ethanol, the anthocyanidin can be effectively separated, and the entire process flow is simplified; and finally, treating same by means of a vacuum freeze-drying technique, which can maximally retain the active ingredients of anthocyanidin, thereby ensuring the efficient and stable progress of the process flow, and achieving the retention of high-purity and high-activity anthocyanin.

Description

A highly efficient production process for extracting anthocyanins from Sichuan pepper. Technical Field

[0001] This invention relates to the field of plant chemical extraction technology, specifically to an efficient production process for extracting anthocyanins from Sichuan pepper. Background Technology

[0002] Traditional processes for extracting anthocyanins from Sichuan pepper have several limitations. Firstly, the raw material pretreatment is often simplistic and crude, failing to adequately consider the removal of impurities and the impact of cell wall structure on anthocyanin release. While strong alkali treatment can disrupt cell walls to some extent, it easily leads to equipment corrosion, loss of numbing components, and an inability to precisely control the impact on anthocyanin activity, thus limiting subsequent extraction efficiency and introducing more impurities. Secondly, during extraction, traditional methods rely heavily on multiple extractions with organic solvents, resulting in large solvent consumption, long extraction times, and difficulty in stabilizing anthocyanins while minimizing the introduction of lipid-soluble impurities. This is energy-intensive and environmentally unfriendly. Furthermore, during purification, traditional alkaline treatments and membrane separation methods are cumbersome, pose a risk of equipment corrosion from strong alkalis, or fail to effectively improve anthocyanin purity due to the selectivity limitations of membrane separation, potentially affecting its activity. Finally, in the final concentration and drying stage, conventional evaporation and hot air drying methods easily degrade anthocyanins due to the high-temperature environment, leading to decreased product purity and activity retention, failing to meet the demands of high-quality anthocyanin production. Given the shortcomings of these traditional processes, it is urgent to develop a more efficient, lower-cost production process that can guarantee the quality of anthocyanins. Summary of the Invention

[0003] (a) Technical problems to be solved

[0004] To address the shortcomings of existing technologies, this invention provides a highly efficient production process for extracting anthocyanins from Sichuan pepper. This process offers advantages such as mild and efficient raw material pretreatment, precise and stable extraction, simple and highly selective purification, and low-temperature concentration and drying to preserve anthocyanins. It solves the problems of equipment corrosion and loss of numbing flavor caused by strong alkali treatment, large amount of extraction solvent used and long extraction time, complex purification operation with poor results, and easy degradation of anthocyanins during the drying process in traditional processes.

[0005] (II) Technical Solution

[0006] To achieve the above objectives, the present invention provides the following technical solution: a highly efficient production process for extracting anthocyanins from Sichuan pepper, comprising the following steps:

[0007] Step 1: Raw material pretreatment: The dried Sichuan peppercorns are winnowed, crushed and enzymatically hydrolyzed to obtain enzymatic hydrolysate;

[0008] Step 2: Selecting a solvent: Prepare an acidic mixed solvent with a pH of 2-4 using ethanol, pure water, and citric acid. Add the enzymatic hydrolysate to the acidic mixed solvent and perform ultrasonic extraction.

[0009] Step 3, solid-liquid separation: Place the enzymatic hydrolysate after extraction into a centrifuge tube, centrifuge under the set conditions of the centrifuge, let it stand for 1 to 2 hours, and collect the anthocyanin-containing clear liquid at the top of the centrifuge tube.

[0010] Step 4: Purification: The anthocyanin solution was purified using an AB-8 macroporous adsorption resin column. The collected anthocyanin solution was passed through a pre-activated AB-8 macroporous adsorption resin column at a flow rate of 0.8–1 mL / min. After loading, the solution was rinsed 1–3 times with 95–100 mL of pure water, and then eluted with 40–50 mL of ethanol solution at a flow rate of 0.9–1 mL / min to obtain an anthocyanin ethanol solution.

[0011] Step 5, Concentration and Drying: Using vacuum freeze-drying technology, the anthocyanin ethanol solution obtained by elution is pre-frozen at a temperature of -55 to -50°C for 2 to 3 hours, then transferred to a freeze dryer, and sublimation drying is carried out after the temperature is raised and the set conditions are met to obtain anthocyanins.

[0012] Preferably, in step one, the dried Sichuan peppercorns are air-separated, and after air separation, the dried Sichuan peppercorns are pulverized in an environment with a temperature ≤10℃, and the particle size is controlled at 80-100 mesh.

[0013] Preferably, in step one, the pulverized dried Sichuan peppercorns are added to a citric acid-sodium citrate buffer solution with a pH of 4.5-5.5 at a material-to-liquid ratio of 1:8-1:10, and then 0.5% to 2.0% of a compound enzyme preparation based on the total mass of the Sichuan peppercorn powder is added. The mixture is stirred and enzymatically hydrolyzed at a temperature of 50-55°C for 2 to 3 hours.

[0014] Preferably, the ratio of pectinase to cellulase in the compound enzyme preparation is 1:1 to 2:1.

[0015] Preferably, the acidic mixed solvent in step two is prepared by mixing ethanol, pure water and citric acid in a volume ratio of 5:5:1, wherein the concentration of ethanol is 90% to 95% and the concentration of citric acid is 10% to 15%.

[0016] Preferably, the solvent extraction conditions in step two are: ultrasonic power of 300-400W, frequency of 40-50kHz, temperature of 45-50℃, and extraction time of 30-60 minutes.

[0017] Preferably, the solid-liquid separation conditions in step three are: centrifugation at a speed of 3500-4000 r / min for 10-15 minutes.

[0018] Preferably, the pre-activation treatment step of the AB-8 macroporous adsorption resin column in step four is as follows:

[0019] S1.1 Soak the AB-8 macroporous adsorption resin column in anhydrous ethanol for 2 to 4 hours;

[0020] S1.2. Rinse the resin column with 2-3 column volumes of anhydrous ethanol at a flow rate of 1-3 mL / min.

[0021] S1.3 Rinse the resin column with pure water until the rinsing solution has no ethanol smell, so that the resin becomes hydrophilic.

[0022] S1.4 Rinse the resin column with a 0.1-0.2 mol / L hydrochloric acid solution until the pH value is between 7 and 8. Finally, rinse the resin column with pure water until the pH value of the rinsing solution stabilizes at 6.5-7.5 and the resin column reaches equilibrium.

[0023] Preferably, the concentration of the ethanol solution in step four of the purification process is 65% to 70%.

[0024] Preferably, the drying conditions in step five are: a vacuum degree of 5-10 Pa, a temperature of 15-20°C, and a sublimation drying time of 12-14 hours.

[0025] Compared with existing technologies, this invention provides a highly efficient production process for extracting anthocyanins from Sichuan pepper, which has the following beneficial effects:

[0026] 1. This invention optimizes raw material pretreatment by combining air separation, low-temperature pulverization, and enzymatic hydrolysis. This achieves the beneficial effects of reducing impurity interference, improving anthocyanin extraction efficiency, and enhancing product quality. Air separation effectively removes impurities from Sichuan peppercorns, reducing the burden on subsequent extraction. Low-temperature pulverization, conducted in a low-temperature environment, effectively avoids the impact of high temperatures on the active components of anthocyanins while increasing the contact area between the solvent and the raw material. Enzymatic hydrolysis, through a gentle chemical reaction, destroys pectin and cellulose in the cell walls, promoting the release of anthocyanins. This pretreatment method not only solves the problem of low extraction efficiency caused by excessive impurities in traditional processes but also promotes the release of anthocyanins by destroying cell walls through enzymatic hydrolysis, while avoiding equipment corrosion and loss of numbing flavor components caused by strong alkali treatment.

[0027] 2. This invention achieves the beneficial effects of reducing solvent consumption, shortening extraction time, and reducing energy consumption by employing an acidic mixed solvent ultrasonic extraction technology. The acidic environment helps stabilize anthocyanins, while ultrasonic-assisted extraction accelerates the mass transfer process, thereby further improving extraction efficiency and selectivity. While ensuring the extraction rate and purity of anthocyanins, it can effectively reduce production costs and reduce environmental impact.

[0028] 3. This invention achieves the beneficial effects of simplifying the process and improving the purity and activity retention rate of anthocyanins by applying macroporous adsorption resin purification and vacuum freeze-drying technology. Macroporous adsorption resin can specifically adsorb anthocyanins, achieving effective separation and avoiding the complex operation and strong alkali corrosion problems of traditional alkaline treatment and membrane separation. Vacuum freeze-drying technology is carried out at low temperature, which maximizes the preservation of the active ingredients of anthocyanins, thereby avoiding degradation caused by high-temperature drying and improving the stability and quality of the product. Attached Figure Description

[0029] Figure 1 is a process flow diagram of the present invention. Detailed Implementation

[0030] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. 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.

[0031] Please refer to Figure 1. A highly efficient production process for extracting anthocyanins from Sichuan pepper includes the following steps:

[0032] Step 1, Raw material pretreatment: The dried peppercorns are air-selected, crushed and enzymatically hydrolyzed to obtain enzymatic hydrolysate. This step combines air-selection, crushing and enzymatic hydrolysis into an enhanced pretreatment. The introduction of mild and efficient enzymatic hydrolysis replaces the strong alkali treatment in the traditional process, thereby solving the problems of corrosion, loss of numbing flavor and some impurities, and improving extraction efficiency.

[0033] Step 2, Solvent Selection: Prepare an acidic mixed solvent with a pH of 2-4 using ethanol, pure water, and citric acid. Add the enzymatic hydrolysate to the acidic mixed solvent and perform ultrasonic extraction. This step helps stabilize anthocyanins under acidic conditions. At the same time, the selective dissolution effect of ethanol and pure water can reduce the mixing of lipid-soluble impurities, thereby improving the extraction efficiency and purity of anthocyanins. Furthermore, the use of citric acid instead of strong alkali can significantly reduce equipment corrosion.

[0034] Step 3, solid-liquid separation: Place the enzymatic hydrolysate after extraction into a centrifuge tube and centrifuge under the set conditions of the centrifuge. After standing for 1 to 2 hours, collect the anthocyanin-containing clear liquid at the top of the centrifuge tube. This aqueous system can effectively avoid the multiple extraction operations of traditional organic solvent extraction, and the assistance of ultrasound can accelerate the mass transfer process, thereby reducing extraction time and solvent consumption, improving extraction efficiency and selectivity, and reducing energy consumption and environmental pollution.

[0035] Step 4: Purification: The anthocyanin solution is purified using an AB-8 macroporous adsorption resin column. The collected anthocyanin solution is passed through a pre-activated AB-8 macroporous adsorption resin column at a flow rate of 0.8–1 mL / min. After loading, the solution is rinsed 1–3 times with 95–100 mL of pure water to remove small molecule impurities. Then, the anthocyanins in the solution are eluted with 40–50 mL of ethanol solution at a flow rate of 0.9–1 mL / min. The resulting anthocyanin ethanol solution is obtained. Since the macroporous adsorption resin can specifically adsorb anthocyanins, effective separation can be achieved through water washing and ethanol elution, thus replacing traditional alkaline treatment and membrane separation. This simplifies the process and avoids the corrosion of equipment by strong alkali and the loss of numbing components, while ensuring a high purification effect.

[0036] Step 5, Concentration and Drying: Using vacuum freeze-drying technology, the anthocyanin ethanol solution obtained by elution is pre-frozen at a temperature of -55 to -50°C for 2 to 3 hours, and then transferred to a freeze dryer. After setting the temperature, sublimation drying is carried out to obtain anthocyanins. Since vacuum freeze-drying is carried out at low temperature in this step, the active ingredients of anthocyanins can be preserved to the greatest extent, thereby avoiding the degradation of anthocyanins caused by high temperature in traditional concentration and drying, improving product purity and stability, and eliminating solvent residue problems.

[0037] The advantages are: through the close connection, technical synergy, and precise parameter matching between steps one and five, this process method possesses the advantages of mild and efficient raw material pretreatment, precise and stable extraction process, simple and highly selective purification, and low-temperature preservation through concentration and drying. Specifically, the raw material pretreatment combines air classification, low-temperature pulverization, and enzymatic hydrolysis to remove impurities and disrupt cell walls, providing a high-quality raw material foundation for subsequent extraction. During ultrasonic extraction, the acidic mixed solvent is well-matched with the enzymatically hydrolyzed raw material, stabilizing anthocyanins while accelerating extraction. Solid-liquid separation quickly obtains the clear liquid, macroporous adsorption resin provides precise purification and separation, and vacuum freeze-drying achieves low-temperature sublimation drying. The results of each step lay the groundwork for the next efficient step, forming a tightly integrated process chain. Enzymatic hydrolysis replaces strong alkali treatment, avoiding equipment corrosion and loss of numbing flavor. The synergistic use of acidic mixed solvent ultrasonic extraction technology reduces damage to anthocyanins, while macroporous adsorption resin purification technology replaces traditional alkaline treatment and membrane separation, simplifying the process and improving selectivity. Combined with vacuum freeze-drying technology, it further ensures the purity and activity of anthocyanins. The parameters of each step are optimized and matched with each other. For example, the temperature and pH of low-temperature pulverization and enzymatic hydrolysis are matched with the temperature and power of ultrasonic extraction. The flow rate, eluent volume and concentration of macroporous adsorption resin purification are coordinated with the pre-freezing temperature, vacuum degree and drying time of vacuum freeze-drying to ensure high purity and high activity retention of anthocyanins. This makes the entire process highly efficient and stable, solving the problems of equipment corrosion and loss of numbing flavor caused by strong alkali treatment, large amount of extraction solvent and long time consumption, complex purification operation and poor effect, and easy degradation of anthocyanins during the drying process in traditional processes.

[0038] Specifically, in step one, the dried peppercorns are air-separated to remove impurities (such as peppercorn seeds and stems) and reduce the burden of subsequent extraction. After air separation, the dried peppercorns are pulverized at a temperature of ≤10℃, and the particle size is controlled at 80-100 mesh to increase the contact area between the solvent and the raw material.

[0039] Specifically, in step one, the pulverized dried Sichuan peppercorns are added to a citric acid-sodium citrate buffer solution with a pH of 4.5-5.5 at a material-to-liquid ratio of 1:8 to 1:10. Then, 0.5% to 2.0% of the total mass of the Sichuan peppercorn powder is added as a compound enzyme preparation. The mixture is stirred and enzymatically hydrolyzed at 50-55℃ for 2 to 3 hours. Enzymatic hydrolysis under these conditions can effectively destroy pectin and cellulose in the cell walls, release anthocyanins, and improve the extraction rate. At the same time, the process is gentle to avoid excessive loss of numbing substances and strong alkali corrosion. The pH and temperature must be strictly controlled to maintain enzyme activity.

[0040] Specifically, the ratio of pectinase to cellulase in the compound enzyme preparation is 1:1 to 2:1.

[0041] The advantages are: by optimizing the raw material pretreatment and combining air separation, low-temperature pulverization, and enzymatic hydrolysis, the beneficial effects of reducing impurity interference, improving anthocyanin extraction efficiency, and improving product quality are achieved. Among them, air separation effectively removes impurities from Sichuan pepper, reducing the burden on subsequent extraction. Low-temperature pulverization is carried out in a low-temperature environment, which can effectively avoid the impact of high temperature on the active ingredients of anthocyanins, while increasing the contact area between the solvent and the raw material. Enzymatic hydrolysis destroys pectin and cellulose in the cell wall through a gentle chemical reaction, promoting the release of anthocyanins. This pretreatment method not only solves the problem of low extraction efficiency caused by excessive impurities in traditional processes, but also promotes the release of anthocyanins by destroying the cell wall through enzymatic hydrolysis, while avoiding equipment corrosion and loss of numbing flavor components caused by strong alkali treatment.

[0042] Specifically, in step two, the acidic mixed solvent is prepared by mixing ethanol, pure water and citric acid in a volume ratio of 5:5:1, wherein the concentration of ethanol is 90% to 95% and the concentration of citric acid is 10% to 15%.

[0043] Specifically, the solvent extraction conditions in step two are as follows: ultrasonic power of 300-400W, frequency of 40-50kHz, temperature of 45-50℃, and extraction time of 30-60 minutes.

[0044] Specifically, the solid-liquid separation conditions in step three are: centrifugation at a speed of 3500-4000 r / min for 10-15 minutes.

[0045] The advantages are: by using acidic mixed solvent ultrasonic extraction technology, the beneficial effects of reducing solvent consumption, shortening extraction time and reducing energy consumption are achieved. The acidic environment helps stabilize anthocyanins, while ultrasonic-assisted extraction accelerates the mass transfer process, thereby further improving extraction efficiency and selectivity. While ensuring the extraction rate and purity of anthocyanins, it can effectively reduce production costs and reduce environmental impact.

[0046] Specifically, the pre-activation treatment step of the AB-8 macroporous adsorption resin column in step four is as follows:

[0047] S1.1 Soak the AB-8 macroporous adsorption resin column in anhydrous ethanol for 2 to 4 hours to ensure that the resin is fully swollen before proceeding to the next step.

[0048] S1.2. Use 2-3 column volumes of anhydrous ethanol at a flow rate of 1-3 mL / min to flush the resin column to remove ethanol and expel air bubbles.

[0049] S1.3 Rinse the resin column with pure water until the rinsing solution has no ethanol smell, so that the resin becomes hydrophilic.

[0050] S1.4 Rinse the resin column with a 0.1-0.2 mol / L hydrochloric acid solution until the pH value is between 7 and 8. Finally, rinse the resin column with pure water until the pH value of the rinsing solution stabilizes at 6.5-7.5 and the resin column reaches equilibrium.

[0051] Specifically, the concentration of the ethanol solution in step four, the purification process, is 65%–70%.

[0052] Specifically, the drying conditions in step five are: vacuum degree of 5-10 Pa, temperature of 15-20℃, and sublimation drying time of 12-14 hours.

[0053] The advantages are: by applying macroporous adsorption resin purification and vacuum freeze-drying technology, the process is simplified and the purity and activity retention rate of anthocyanins are improved. Macroporous adsorption resin can specifically adsorb anthocyanins and achieve effective separation, avoiding the complex operation and strong alkali corrosion problems of traditional alkaline treatment and membrane separation. Vacuum freeze-drying technology is carried out at low temperature, which maximizes the preservation of the active ingredients of anthocyanins, thereby avoiding degradation caused by high temperature drying and improving the stability and quality of the product.

[0054] The process method of the present invention was implemented in a practical case, and a conventional method was used as a reference group to obtain the following examples and comparative examples:

[0055] Example 1 (Optimization and Verification of Raw Material Pretreatment)

[0056] Processing procedure: Take 100g of dried Sichuan peppercorns, remove impurities such as peppercorn seeds and stems by air separation, grind to 80 mesh at 8℃, add the ground Sichuan peppercorns to a citric acid-sodium citrate buffer solution with a pH of 4.5 at a material-liquid ratio of 1:8, add 0.5% of the total mass of Sichuan peppercorn powder and a compound enzyme preparation with a pectinase and cellulase ratio of 1:1, stir and enzymatically hydrolyze at 50℃ for 2 hours to obtain the enzymatic hydrolysate.

[0057] Comparative Example 1

[0058] Processing procedure: Using traditional methods, 100g of dried Sichuan peppercorns are directly pulverized to 80 mesh without air separation or enzymatic hydrolysis. Other steps are the same as in Example 1.

[0059] Example 2 (Optimization and Validation of Solvent Extraction)

[0060] Processing procedure: The enzymatic hydrolysate obtained in Example 1 was added to an acidic mixed solvent prepared by mixing 5:5:1 by volume, 90% ethanol and 10% citric acid. Extraction was carried out for 30 minutes under ultrasonic power of 300W, frequency of 40kHz and temperature of 45℃. After extraction, centrifugation was carried out at 3500r / min for 10 minutes. After standing for 1 hour, the supernatant containing anthocyanins was collected.

[0061] Comparative Example 2

[0062] Processing procedure: The traditional solvent A and B two-stage extraction method was used, with an extraction time of 60 minutes. The amount of solvent used was twice that of Example 2, and the other steps were the same as in Example 2.

[0063] Example 3 (Purification Treatment Optimization and Validation)

[0064] Processing procedure: The anthocyanin solution collected in Example 2 was passed through an AB-8 macroporous adsorption resin column (column diameter 1.5 cm, column height 20 cm, resin bed volume 10 mL) that had been pre-activated according to steps S1.1-S1.4. The sample was loaded at a flow rate of 0.8 mL / min. After loading, the sample was rinsed once with 95 mL of pure water, and then the anthocyanins were eluted with 40 mL of 65% ethanol solution at a flow rate of 0.9 mL / min to obtain anthocyanin ethanol solution.

[0065] Comparative Example 3

[0066] Processing procedure: Purification is carried out using traditional alkaline treatment and membrane separation.

[0067] Example 4 (Optimization and Validation of Concentration and Drying)

[0068] Processing procedure: The anthocyanin ethanol solution obtained in Example 3 was pre-frozen at -55°C for 2 hours, then transferred to a freeze dryer with a vacuum of 5 Pa and a temperature of 15°C for sublimation drying for 12 hours to obtain the anthocyanin product.

[0069] Comparative Example 4

[0070] Processing procedure: Traditional evaporation concentration and hot air drying methods are used, with a drying temperature of 60℃.

[0071] Table 1: Energy consumption and cost comparison between the examples and comparative examples

[0072] Anthocyanin performance test table 2

[0073] Analysis of Table 1-2 yields the following results:

[0074] (1) In Example 1, the raw material pretreatment method of air separation, low temperature pulverization and enzymatic hydrolysis reduced energy consumption by 0.7 kW·h / kg and cost by 7 yuan / kg compared with Comparative Example 1. The anthocyanin extraction rate increased by 4.7%, the purity increased by 13.3%, and the activity retention rate increased by 12.2%. This shows that the enhanced pretreatment can effectively reduce impurity interference, and the enzymatic hydrolysis can destroy the cell wall to promote the release of anthocyanins, while reducing energy consumption and cost. In contrast, Comparative Example 1 only used traditional pulverization treatment, which had many impurities that affected the subsequent extraction. The energy consumption and cost were high, and the anthocyanin extraction effect was poor.

[0075] (2) Example 2 uses ultrasonic extraction with acidic mixed solvent, which reduces energy consumption by 2.7 kW·h / kg and cost by 20 yuan / kg compared with Comparative Example 2. The extraction rate is increased by 5.5%, the purity is increased by 8.9%, and the activity retention rate is increased by 8.9%. The acidic environment stabilizes anthocyanins, and ultrasound accelerates mass transfer, reducing extraction time and solvent usage. Comparative Example 2 uses the traditional two-stage extraction method, which consumes a lot of solvent and takes a long time, resulting in high energy consumption, high cost, and poor extraction effect.

[0076] (3) Example 3 uses macroporous adsorption resin for purification, which reduces energy consumption by 1.5 kW·h / kg and cost by 15 yuan / kg compared to Comparative Example 3. The purity is increased by 6.7% and the activity retention rate is increased by 6.8%. The macroporous adsorption resin simplifies the process by specific adsorption and avoids strong alkali corrosion and loss of anthocyanin flavor. Comparative Example 3 uses traditional alkaline treatment and membrane separation method, which is complicated to operate, strong alkali corrodes the equipment, affects the quality of anthocyanins, and has higher energy consumption and cost.

[0077] (4) Example 4 uses vacuum freeze drying technology, which reduces energy consumption by 2.5 kW·h / kg and cost by 15 yuan / kg compared to Comparative Example 4. The purity is increased by 10.7% and the activity retention rate is increased by 13.5%. Low temperature drying retains anthocyanin active ingredients to the greatest extent. Comparative Example 4 uses traditional evaporation concentration and hot air drying. High temperature causes anthocyanin degradation, affecting purity and activity, and the energy consumption and cost are also higher.

[0078] In summary, this invention optimizes and innovates the process steps of raw material pretreatment, solvent extraction, purification, and concentration drying, effectively reducing energy consumption and costs in the production process compared to traditional methods. Simultaneously, it significantly improves the extraction rate, purity, and activity retention rate of anthocyanins. By employing mild and efficient enzymatic hydrolysis instead of strong alkali treatment, it avoids equipment corrosion and loss of numbing flavor. The application of acidic mixed solvent ultrasonic extraction, macroporous adsorption resin purification, and vacuum freeze-drying technology simplifies the traditional process and reduces environmental pollution. This achieves efficient, low-cost, and high-quality anthocyanin extraction from Sichuan pepper, demonstrating promising industrial application prospects and economic value.

[0079] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A highly efficient production process for extracting anthocyanins from Sichuan pepper, characterized in that, Includes the following steps: Step 1: Raw material pretreatment: The dried Sichuan peppercorns are winnowed, crushed and enzymatically hydrolyzed to obtain enzymatic hydrolysate; Step 2: Selecting a solvent: Prepare an acidic mixed solvent with a pH of 2-4 using ethanol, pure water, and citric acid. Add the enzymatic hydrolysate to the acidic mixed solvent and perform ultrasonic extraction. Step 3, solid-liquid separation: Place the enzymatic hydrolysate after extraction into a centrifuge tube, centrifuge under the set conditions of the centrifuge, let it stand for 1 to 2 hours, and collect the anthocyanin-containing clear liquid at the top of the centrifuge tube. Step 4: Purification: The anthocyanin solution was purified using an AB-8 macroporous adsorption resin column. The collected anthocyanin solution was passed through a pre-activated AB-8 macroporous adsorption resin column at a flow rate of 0.8–1 mL / min. After loading, the solution was rinsed 1–3 times with 95–100 mL of pure water, and then eluted with 40–50 mL of ethanol solution at a flow rate of 0.9–1 mL / min to obtain an anthocyanin ethanol solution. Step 5, Concentration and Drying: Using vacuum freeze-drying technology, the anthocyanin ethanol solution obtained by elution is pre-frozen at a temperature of -55 to -50°C for 2 to 3 hours, then transferred to a freeze dryer, and sublimation drying is carried out after the temperature is raised and the set conditions are met to obtain anthocyanins.

2. The efficient production process for extracting anthocyanins from Sichuan pepper according to claim 1, characterized in that, In step one, the dried Sichuan peppercorns are air-separated, and then pulverized at a temperature ≤10℃, with the particle size controlled at 80-100 mesh.

3. The efficient production process for extracting anthocyanins from Sichuan pepper according to claim 1, characterized in that: In step one, the pulverized dried Sichuan peppercorns are added to a citric acid-sodium citrate buffer solution with a pH of 4.5-5.5 at a material-to-liquid ratio of 1:8-1:

10. Then, 0.5% to 2.0% of the total mass of the Sichuan peppercorn powder is added to a compound enzyme preparation, and the mixture is stirred and enzymatically hydrolyzed at a temperature of 50-55°C for 2 to 3 hours.

4. The efficient production process for extracting anthocyanins from Sichuan pepper according to claim 3, characterized in that: The ratio of pectinase to cellulase in the compound enzyme preparation is 1:1 to 2:

1.

5. The efficient production process for extracting anthocyanins from Sichuan pepper according to claim 1, characterized in that: In step two, the acidic mixed solvent is prepared by mixing ethanol, pure water and citric acid in a volume ratio of 5:5:1, wherein the concentration of ethanol is 90% to 95% and the concentration of citric acid is 10% to 15%.

6. The efficient production process for extracting anthocyanins from Sichuan pepper according to claim 1, characterized in that: The solvent extraction conditions in step two are as follows: ultrasonic power of 300-400W, frequency of 40-50kHz, temperature of 45-50℃, and extraction time of 30-60 minutes.

7. The efficient production process for extracting anthocyanins from Sichuan pepper according to claim 1, characterized in that: The solid-liquid separation conditions in step three are: centrifugation at a speed of 3500-4000 r / min for 10-15 minutes.

8. The efficient production process for extracting anthocyanins from Sichuan pepper according to claim 1, characterized in that: The pre-activation treatment step of the AB-8 macroporous adsorption resin column in step four is as follows: S1.1 Soak the AB-8 macroporous adsorption resin column in anhydrous ethanol for 2 to 4 hours; S1.

2. Rinse the resin column with 2-3 column volumes of anhydrous ethanol at a flow rate of 1-3 mL / min. S1.3 Rinse the resin column with pure water until the rinsing solution has no ethanol smell, so that the resin becomes hydrophilic. S1.4 Rinse the resin column with a 0.1-0.2 mol / L hydrochloric acid solution until the pH value is between 7 and 8. Finally, rinse the resin column with pure water until the pH value of the rinsing solution stabilizes at 6.5-7.5 and the resin column reaches equilibrium.

9. The efficient production process for extracting anthocyanins from Sichuan pepper according to claim 1, characterized in that: In step four, the concentration of the ethanol solution in the purification process is 65%–70%.

10. The efficient production process for extracting anthocyanins from Sichuan pepper according to claim 1, characterized in that: The drying conditions in step five are: vacuum degree of 5-10 Pa, temperature of 15-20℃, and sublimation drying time of 12-14 hours.

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