Method for extracting clovershrub zanthoxylum bungeanum peel

Abstract

A clovershrub zanthoxylum bungeanum peel extraction method belongs to the field of clovershrub zanthoxylum bungeanum peel extraction, and comprises the following steps: 1, washing freshly picked clovershrub zanthoxylum bungeanum, and airing; step 2, drying the Dahongpao pepper cleaned and aired in the step 1; step 3, performing peel and seed separation on the dried Dahongpao pepper; 4, crushing the clovershrub peel obtained in the step 3, and extracting the clovershrub peel through a carbon dioxide supercritical fluid extraction method; 5, after extraction is completed, substances obtained in the step 4 are dissolved, and recrystallization operation is conducted; and 6, after recrystallization is completed, filtering, drying and crushing to obtain the Zanthoxylum bungeanum Maxim peel extract. According to the invention, the zanthoxylum clovershrub peel extracted essential oil obtained by carbon dioxide supercritical fluid extraction is purified by a recrystallization method to obtain a crystalline solid, so that the zanthoxylum clovershrub peel extract is convenient to store and transport while the impurity content is reduced.

Description

Technical Field

[0001] The invention belongs to the field of Dahongpao Zanthoxylum bungeanum peel extraction, in particular to a Dahongpao Zanthoxylum bungeanum peel extraction method. Background Art

[0002] Dahongpao peppercorns are a type of red peppercorns that are warm in nature, spicy, and have a distinct numbing flavor. They are mainly grown in North, Central, and South China, with concentrated plantings in Shanxi, Shaanxi, and Henan. The highest quality Dahongpao peppercorns are produced in Hancheng and Fengxian in Shaanxi, and Longnan and Qin'an in Gansu. Dahongpao peppercorns have the advantages of large spikes, thick skin, plump flesh, a mellow numbing flavor, rich aroma, and a high oil content, so they are widely planted and used.

[0003] At present, the use of Dahongpao pepper extracts in addition to the traditional edible field has also been deeply studied; Dahongpao pepper peel is rich in volatile oils, limonene, cumyl alcohol, geraniol, sterols and unsaturated organic acids, piperine, trace elements and other substances. These substances not only give Dahongpao pepper a unique aroma and numbing taste, but also can play a role in disinfection and sterilization. Therefore, its extract can be used not only in traditional edible fields but also in medicine, cosmetics and biological pesticides. The fields are widely used. However, the extracts obtained after the Dahongpao pepper peel extraction are mostly oily, namely Dahongpao pepper peel essential oil. Since oily substances are not convenient to store and transport, the subsequent storage cost and transportation cost are high. At the same time, the Dahongpao pepper peel essential oil extracted is generally extracted according to the maximum yield to ensure the extraction efficiency. Therefore, a certain amount of impurities may still exist in the Dahongpao pepper peel essential oil obtained, which will affect its quality if not purified. Summary of the Invention

[0004] The invention provides a method for extracting Dahongpao Zanthoxylum bungeanum peel, which is used to solve the defects in the prior art.

[0005] The present invention is achieved through the following technical solutions:

[0006] A method for extracting Dahongpao Zanthoxylum bungeanum peel comprises the following steps:

[0007] Step 1: Wash and dry the freshly picked Dahongpao peppercorns;

[0008] Step 2: Dry the Dahongpao peppercorns washed and dried in step 1;

[0009] Step 3: Separate the peel and seeds of the dried Dahongpao pepper;

[0010] Step 4: crushing the Dahongpao Zanthoxylum bungeanum peel obtained in step 3 and extracting the Dahongpao Zanthoxylum bungeanum peel by supercritical fluid extraction with carbon dioxide;

[0011] Step 5: After the extraction is completed, the material obtained in step 4 is dissolved and then recrystallized;

[0012] Step 6: After recrystallization, filter, dry and crush to obtain Dahongpao Zanthoxylum bungeanum peel extract.

[0013] In the above-mentioned method for extracting Dahongpao pepper peel, the freshly picked Dahongpao pepper in step 1 is washed with clean water for 3 to 5 times and then dried for 18 to 24 hours.

[0014] The method for extracting Dahongpao pepper peel comprises the following steps: in the step 2, the cleaned and dried Dahongpao pepper is placed in a drying oven and dried at a temperature of 40-60° C. for 3-4 hours, and the Dahongpao pepper is turned over as a whole every hour during the drying process to ensure drying efficiency; then the temperature is raised to 70-80° C., and drying is continued for 4-6 hours, and the Dahongpao pepper is turned over as a whole every 2 hours during the drying process to ensure drying efficiency; and after drying is completed, the Dahongpao pepper is cooled to room temperature and taken out.

[0015] In the above-mentioned method for extracting Dahongpao Zanthoxylum bungeanum peel, the moisture content of the Dahongpao Zanthoxylum bungeanum after drying in step 2 is less than 6%.

[0016] In the above-mentioned method for extracting Dahongpao Zanthoxylum bungeanum peel, the peel and seeds of the Zanthoxylum bungeanum are separated in step three by a screening machine.

[0017] According to the above-mentioned method for extracting Dahongpao Zanthoxylum bungeanum peel, in the step 4, the Dahongpao Zanthoxylum bungeanum peel is crushed and passed through a 200-mesh sieve. If there is any material remaining on the sieve, the residue is returned and crushed again until all the material is sieved.

[0018] The method for extracting Dahongpao Zanthoxylum bungeanum peel comprises the following steps: the crushed Dahongpao Zanthoxylum bungeanum peel in the step 4 is placed in a supercritical fluid extraction tank, the extraction temperature is raised to 56-60° C., and the extraction pressure is raised to 35-40 MPa; after stabilization for 2-3 minutes, a carbon dioxide fluid is added for extraction, the carbon dioxide fluid flow rate is 40-50 L / h, the extraction pressure is reduced to 10-15 MPa after extraction for 8-10 minutes, and then the extraction pressure is increased to 40-45 MPa, the extraction temperature is controlled at 58-60° C., and the extraction time is 106-118 minutes. After the extraction is completed, the peel is placed in a separation tank, the pressure in the separation tank is reduced to 3-5 MPa, the temperature is controlled at 40-44° C., and the carbon dioxide fluid is gasified and separated, thereby obtaining the Dahongpao Zanthoxylum bungeanum peel extracted essential oil.

[0019] In the above-mentioned method for extracting Dahongpao Zanthoxylum bungeanum peel, the recrystallization operation in step 5 comprises the following steps:

[0020] Step 1: adding the Dahongpao Zanthoxylum bungeanum peel extract obtained in step 4 to a dissolving solvent, wherein the mass of the dissolving solvent added is 1.5 to 2 times the mass of the Dahongpao Zanthoxylum bungeanum peel extract, and stirring at a temperature of 40 to 50° C. until completely dissolved;

[0021] Step 2: After heating to completely dissolve, stop heating and continue stirring to cool to room temperature, then add ethyl acetate dropwise while stirring, and the mass of petroleum ether added should be 4 to 5 times the mass of the essential oil extracted from the peel of Dahongpao pepper. After the addition is complete, stir in an ice-water bath for 50 to 70 minutes;

[0022] Step 3: Place the solid-liquid mixture from which crystals have precipitated after stirring in an ice-water bath in step 2 in a dedicated refrigerator at -10 to -20°C for 10 to 14 hours.

[0023] In the above-mentioned method for extracting Dahongpao Zanthoxylum bungeanum peel, the dissolving solvent in step 1 is a mixed solvent obtained by mixing ethanol and cyclopropane in a mass ratio of 2:1.

[0024] The method for extracting Dahongpao Zanthoxylum bungeanum peel comprises the following steps: in step 6, separating the solid-liquid mixture obtained by the recrystallization operation in step 5; drying the solid under negative pressure for 130-150 minutes at a temperature of 40-50° C. and a vacuum degree of -0.08-0.04 MPa; cooling the solid to room temperature after drying, restoring the air pressure in the negative pressure dryer, taking out the dried solid, crushing it through a 200-mesh sieve, and packaging it to obtain the Dahongpao Zanthoxylum bungeanum peel extract.

[0025] The advantages of the present invention are:

[0026] The present invention extracts the Dahongpao Zanthoxylum bungeanum peel by using a carbon dioxide supercritical fluid extraction method, and can extract substances in the Dahongpao Zanthoxylum bungeanum peel to the greatest extent, thereby ensuring the extraction efficiency of the Dahongpao Zanthoxylum bungeanum peel;

[0027] The present invention purifies the Dahongpao Zanthoxylum bungeanum peel essential oil obtained by carbon dioxide supercritical fluid extraction through a recrystallization method to obtain a crystalline solid, thereby purifying the Dahongpao Zanthoxylum bungeanum peel extract and converting the originally obtained Dahongpao Zanthoxylum bungeanum peel essential oil into a solid substance. Therefore, while reducing the impurity content of the Dahongpao Zanthoxylum bungeanum peel extract, it is also convenient for storage and transportation, thereby effectively reducing storage costs and transportation costs.

[0028] The invention performs a drying operation on the Dahongpao Zanthoxylum bungeanum peel extract through a low-temperature negative pressure drying operation, thereby reducing the loss of volatile substances in the Dahongpao Zanthoxylum bungeanum peel extract to the greatest extent and ensuring the yield of the Dahongpao Zanthoxylum bungeanum peel extract. DETAILED DESCRIPTION

[0029] To make the objectives, technical solutions, and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts shall fall within the scope of protection of the present invention.

[0030] A method for extracting Dahongpao Zanthoxylum bungeanum peel comprises the following steps:

[0031] Step 1: Wash and dry the freshly picked Dahongpao peppercorns;

[0032] Step 2: Dry the Dahongpao peppercorns washed and dried in step 1;

[0033] Step 3: Separate the peel and seeds of the dried Dahongpao pepper;

[0034] Step 4: crushing the Dahongpao Zanthoxylum bungeanum peel obtained in step 3 and extracting the Dahongpao Zanthoxylum bungeanum peel by supercritical fluid extraction with carbon dioxide;

[0035] Step 5: After the extraction is completed, the material obtained in step 4 is dissolved and then recrystallized;

[0036] Step 6: After recrystallization, filter, dry and crush to obtain Dahongpao Zanthoxylum bungeanum peel extract.

[0037] Specifically, the freshly picked Dahongpao peppercorns in step 1 of this embodiment are washed with clean water for 3 to 5 times and then air-dried for 18 to 24 hours.

[0038] Specifically, in step 2 of this embodiment, the cleaned and dried Dahongpao peppercorns are added to a drying oven and dried at a temperature of 40-60° C. for 3-4 hours. During the drying process, the Dahongpao peppercorns are turned over as a whole every hour to ensure drying efficiency. Then, the temperature is raised to 70-80° C. and drying is continued for 4-6 hours. During the drying process, the Dahongpao peppercorns are turned over as a whole every 2 hours to ensure drying efficiency. After drying, the peppercorns are cooled to room temperature and taken out.

[0039] More specifically, the moisture content of the Dahongpao pepper after drying in step 2 of this embodiment should be less than 6%.

[0040] More specifically, in step three of this embodiment, the peel and seeds of Zanthoxylum bungeanum are separated by a screening machine.

[0041] More specifically, in step 4 of this embodiment, the Dahongpao Zanthoxylum bungeanum peel is crushed and passed through a 200-mesh sieve. If there is any material remaining on the sieve, the residue is returned and crushed again until all of it is sieved.

[0042] Furthermore, the crushed Dahongpao Zanthoxylum bungeanum peel in step 4 of this embodiment is placed in a supercritical fluid extraction tank, the extraction temperature is raised to 56-60° C., and the extraction pressure is raised to 35-40 MPa; after stabilization for 2-3 minutes, a carbon dioxide fluid is added for extraction, the carbon dioxide fluid flow rate is 40-50 L / h, and after extraction for 8-10 minutes, the extraction pressure is reduced to 10-15 MPa, and then the extraction pressure is raised to 40-45 MPa, the extraction temperature is controlled at 58-60° C., and the extraction time is 106-118 minutes. After the extraction is completed, the peel is sent to a separation tank to reduce the pressure in the separation tank to 3-5 MPa, the temperature is controlled at 40-44° C., and the carbon dioxide fluid is gasified and separated, thereby obtaining the Dahongpao Zanthoxylum bungeanum peel extracted essential oil.

[0043] Furthermore, the recrystallization operation in step 5 of this embodiment includes the following steps:

[0044] Step 1: adding the Dahongpao Zanthoxylum bungeanum peel extract obtained in step 4 to a dissolving solvent, wherein the mass of the dissolving solvent added is 1.5 to 2 times the mass of the Dahongpao Zanthoxylum bungeanum peel extract, and stirring at a temperature of 40 to 50° C. until completely dissolved;

[0045] Step 2: After heating to completely dissolve, stop heating and continue stirring to cool to room temperature, then add ethyl acetate dropwise while stirring, and the mass of petroleum ether added should be 4 to 5 times the mass of the essential oil extracted from the peel of Dahongpao pepper. After the addition is complete, stir in an ice-water bath for 50 to 70 minutes;

[0046] Step 3: Place the solid-liquid mixture from which crystals have precipitated after stirring in an ice-water bath in step 2 in a dedicated refrigerator at -10 to -20°C for 10 to 14 hours.

[0047] Furthermore, the dissolving solvent in step 1 of this embodiment is a mixed solvent obtained by mixing ethanol and cyclopropane in a mass ratio of 2:1.

[0048] Furthermore, in step 6 of this embodiment, the solid-liquid mixture obtained by the recrystallization operation in step 5 is separated, and the solid is dried at a temperature of 40 to 50° C. and a vacuum degree of -0.08 to -0.04 MPa for 130 to 150 minutes under negative pressure. After drying, the mixture is cooled to room temperature and the air pressure in the negative pressure dryer is restored. The dried solid material is taken out, crushed through a 200-mesh sieve, and packaged to obtain the Dahongpao Zanthoxylum bungeanum peel extract.

[0049] Example 1

[0050] Step 1: Wash the freshly picked Dahongpao peppercorns with clean water three times and dry them for 18 hours;

[0051] Step 2: adding the washed and dried Dahongpao peppercorns in step 1 into a drying oven and drying them at 40° C. for 4 hours, turning the Dahongpao peppercorns over as a whole every hour during the drying process to ensure drying efficiency; then raising the temperature to 70° C. and continuing to dry for 6 hours, turning the Dahongpao peppercorns over as a whole every 2 hours during the drying process to ensure drying efficiency; cooling to room temperature after drying and taking out; the moisture content of the dried Dahongpao peppercorns is 5.6%;

[0052] Step 3: The dried Dahongpao peppercorns are passed through a peppercorn peel and seed screening machine to separate the two;

[0053] Step 4: 1 kg of the Dahongpao Zanthoxylum bungeanum peel obtained in step 3 was crushed through a 200-mesh sieve. If there was any residual material on the sieve, the residue was returned and crushed again until all were sieved. The crushed Dahongpao Zanthoxylum bungeanum peel was placed in a supercritical fluid extraction tank, the extraction temperature was raised to 56° C., and the extraction pressure was increased to 35 MPa; after stabilization for 2 minutes, a carbon dioxide fluid was added for extraction, the carbon dioxide fluid flow rate was 40 L / h, and after extraction for 8 minutes, the extraction pressure was reduced to 10 MPa, and then the extraction pressure was increased to 40 MPa. The extraction temperature was controlled at 58° C. and the extraction time was 118 minutes. After the extraction was completed, the separation tank was sent to reduce the pressure in the separation tank to 3 MPa, the temperature was controlled at 40° C., and the carbon dioxide fluid was gasified and separated, thereby obtaining 98.6 g of Dahongpao Zanthoxylum bungeanum peel extracted essential oil;

[0054] Step 5: After the extraction is completed, the essential oil extracted from the Dahongpao Zanthoxylum bungeanum peel obtained in step 4 is recrystallized;

[0055] The specific operations are:

[0056] Step 1: Add the Dahongpao Zanthoxylum peel extract obtained in step 4 to a dissolving solvent (a mixed solvent obtained by mixing ethanol and cyclopropane in a mass ratio of 2:1), the mass of the dissolving solvent added is 1.5 times the mass of the Dahongpao Zanthoxylum peel extract, and stir at a temperature of 50°C until completely dissolved;

[0057] Step 2: After heating to completely dissolve, stop heating and continue stirring to cool to room temperature, then add ethyl acetate dropwise while stirring, and the mass of petroleum ether added is 4 times the mass of the essential oil extracted from the peel of Dahongpao pepper. After the addition is complete, stir in an ice-water bath for 50 minutes;

[0058] Step 3: Place the solid-liquid mixture from which crystals have precipitated after stirring in an ice-water bath in step 2 into a dedicated refrigerator and allow to stand at -10°C for 14 hours.

[0059] Step 6: After the recrystallization is completed, the solid is filtered and dried at a temperature of 40°C and a vacuum degree of -0.08 MPa for 150 minutes. After the drying is completed, the temperature is cooled to room temperature and the air pressure in the negative pressure dryer is restored. The dried solid material is taken out and crushed through a 200 mesh sieve to obtain 91.5 g of Dahongpao Zanthoxylum bungeanum peel extract. The recrystallization yield is 92.8%.

[0060] Example 2

[0061] Step 1: Wash the freshly picked Dahongpao peppercorns with clean water 5 times and dry them for 24 hours;

[0062] Step 2: adding the washed and dried Dahongpao peppercorns in step 1 into a drying oven and drying them at a temperature of 60° C. for 4 hours, turning the Dahongpao peppercorns over as a whole every hour during the drying process to ensure drying efficiency; then raising the temperature to 80° C. and continuing to dry for 6 hours, turning the Dahongpao peppercorns over as a whole every 2 hours during the drying process to ensure drying efficiency; cooling to room temperature after drying and taking out; the moisture content of the dried Dahongpao peppercorns is 4.9%;

[0063] Step 3: The dried Dahongpao peppercorns are passed through a peppercorn peel and seed screening machine to separate the two;

[0064] Step 4: 1 kg of the Dahongpao Zanthoxylum bungeanum peel obtained in step 3 was crushed through a 200-mesh sieve. If there was any residual material on the sieve, the residue was returned and crushed again until all were sieved. The crushed Dahongpao Zanthoxylum bungeanum peel was placed in a supercritical fluid extraction tank, the extraction temperature was raised to 60° C., and the extraction pressure was increased to 40 MPa; after stabilization for 3 min, a carbon dioxide fluid was added for extraction, the carbon dioxide fluid flow rate was 50 L / h, and after extraction for 10 min, the extraction pressure was reduced to 15 MPa, and then the extraction pressure was increased to 45 MPa. The extraction temperature was controlled at 60° C. and the extraction time was 106 min. After the extraction was completed, the separation tank was sent to reduce the pressure in the separation tank to 5 MPa, the temperature was controlled at 44° C., and the carbon dioxide fluid was gasified and separated, thereby obtaining 99.1 g of Dahongpao Zanthoxylum bungeanum peel extracted essential oil;

[0065] Step 5: After the extraction is completed, the essential oil extracted from the Dahongpao Zanthoxylum bungeanum peel obtained in step 4 is recrystallized;

[0066] The specific operations are:

[0067] Step 1: Add the Dahongpao Zanthoxylum peel extract obtained in step 4 to a dissolving solvent (a mixed solvent obtained by mixing ethanol and cyclopropane in a mass ratio of 2:1), the mass of the dissolving solvent added is twice the mass of the Dahongpao Zanthoxylum peel extract, and stir at a temperature of 50°C until completely dissolved;

[0068] Step 2: After heating to completely dissolve, stop heating and continue stirring to cool to room temperature, then add ethyl acetate dropwise while stirring, and the mass of petroleum ether added is 5 times the mass of the essential oil extracted from the peel of Dahongpao pepper. After the addition is complete, stir in an ice-water bath for 50 minutes;

[0069] Step 3: Place the solid-liquid mixture from which crystals have precipitated after stirring in an ice-water bath in step 2 into a dedicated refrigerator and allow to stand at -20°C for 10 hours.

[0070] Step 6: After the recrystallization is completed, the solid is filtered and dried at a temperature of 50°C and a vacuum degree of -0.04 MPa for 130 minutes. After the drying is completed, the temperature is cooled to room temperature and the air pressure in the negative pressure dryer is restored. The dried solid material is taken out and crushed through a 200 mesh sieve to obtain 92.1g of Dahongpao Zanthoxylum bungeanum peel extract, and the recrystallization yield is 92.9%.

[0071] Example 3

[0072] Step 1: Wash the freshly picked Dahongpao peppercorns with clean water 4 times and dry them for 21 hours;

[0073] Step 2: adding the washed and dried Dahongpao peppercorns in step 1 to a drying oven and drying them at a temperature of 50° C. for 3.5 hours, turning the Dahongpao peppercorns over as a whole every hour during the drying process to ensure drying efficiency; then raising the temperature to 75° C. and continuing to dry for 5 hours, turning the Dahongpao peppercorns over as a whole every 2 hours during the drying process to ensure drying efficiency, cooling to room temperature after drying and taking out, the moisture content of the dried Dahongpao peppercorns being 5.1%;

[0074] Step 3: The dried Dahongpao peppercorns are passed through a peppercorn peel and seed screening machine to separate the two;

[0075] Step 4: 1 kg of the Dahongpao Zanthoxylum bungeanum peel obtained in step 3 was crushed through a 200-mesh sieve. If there was any residual material on the sieve, the residue was returned and crushed again until all were sieved. The crushed Dahongpao Zanthoxylum bungeanum peel was placed in a supercritical fluid extraction tank, the extraction temperature was raised to 58° C., and the extraction pressure was increased to 38 MPa. After stabilization for 2.5 min, a carbon dioxide fluid was added for extraction, the carbon dioxide fluid flow rate was 45 L / h, and after extraction for 9 min, the extraction pressure was reduced to 13 MPa, and then the extraction pressure was increased to 42 MPa. The extraction temperature was controlled at 59° C. and the extraction time was 112 in. After the extraction was completed, the separation tank was sent to reduce the pressure in the separation tank to 4 MPa, the temperature was controlled at 42° C., and the carbon dioxide fluid was gasified and separated, thereby obtaining 99.3 g of Dahongpao Zanthoxylum bungeanum peel extracted essential oil;

[0076] Step 5: After the extraction is completed, the essential oil extracted from the Dahongpao Zanthoxylum bungeanum peel obtained in step 4 is recrystallized;

[0077] The specific operations are:

[0078] Step 1: Add the Dahongpao Zanthoxylum peel extract obtained in step 4 to a dissolving solvent (a mixed solvent obtained by mixing ethanol and cyclopropane in a mass ratio of 2:1), the mass of the dissolving solvent added is 1.8 times the mass of the Dahongpao Zanthoxylum peel extract, and stir at a temperature of 450° C. until completely dissolved;

[0079] Step 2: After heating to completely dissolve, stop heating and continue stirring to cool to room temperature, then add ethyl acetate dropwise while stirring, and the mass of petroleum ether added is 4.5 times the mass of the essential oil extracted from the peel of Dahongpao pepper. After the addition is complete, stir in an ice-water bath for 60 minutes;

[0080] Step 3: Place the solid-liquid mixture from which crystals have precipitated after stirring in an ice-water bath in step 2 into a dedicated refrigerator and allow to stand at -15°C for 12 hours.

[0081] Step 6: After the recrystallization is completed, the solid is filtered and dried at a temperature of 45°C and a vacuum degree of -0.06 MPa for 140 minutes under negative pressure. After the drying is completed, the temperature is cooled to room temperature and the air pressure in the negative pressure dryer is restored. The dried solid material is taken out and crushed through a 200-mesh sieve and packaged to obtain 91.9 g of Dahongpao Zanthoxylum peel extract, and the recrystallization yield is 92.5%.

[0082] By performing component detection on the Dahongpao Zanthoxylum bungeanum peel essential oil obtained in step 4 of Examples 1-3 and the Dahongpao Zanthoxylum bungeanum peel extract obtained in step 6, the test results show that the impurity content of Example 1 before and after recrystallization is reduced by 94.8%, the impurity content of Example 2 before and after recrystallization is reduced by 95.1%, and the impurity content of Example 3 before and after recrystallization is reduced by 95.8%. In addition, the Dahongpao Zanthoxylum bungeanum peel extracts obtained in Examples 1-3 of the present invention are solid, so the present invention can prepare a high-purity solid Dahongpao Zanthoxylum bungeanum peel extract.

[0083] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the various embodiments of the present invention.

Claims

1. A method for extracting Dahongpao Zanthoxylum bungeanum peel, characterized in that: The steps include: Step 1: Wash and dry the freshly picked Dahongpao peppercorns; Step 2: Dry the Dahongpao peppercorns washed and dried in step 1; Step 3: Separate the peel and seeds of the dried Dahongpao pepper; Step 4: crushing the Dahongpao Zanthoxylum bungeanum peel obtained in step 3 and extracting the Dahongpao Zanthoxylum bungeanum peel by supercritical fluid extraction with carbon dioxide; Step 5: After the extraction is completed, the material obtained in step 4 is dissolved and then recrystallized; Step 6: After recrystallization, filter, dry and crush to obtain Dahongpao Zanthoxylum bungeanum peel extract.

2. A method for extracting Dahongpao Zanthoxylum bungeanum peel according to claim 1, characterized in that: The freshly picked Dahongpao peppercorns in step 1 are washed with clean water for 3 to 5 times and then air-dried for 18 to 24 hours.

3. A method for extracting Dahongpao Zanthoxylum bungeanum peel according to claim 1, characterized in that: In the step 2, the cleaned and dried Dahongpao peppercorns are placed in a drying oven and dried at a temperature of 40 to 60° C. for 3 to 4 hours. During the drying process, the Dahongpao peppercorns are turned over as a whole every hour to ensure drying efficiency. Then heat up to 70-80℃ and continue drying for 4-6 hours. Turn the Dahongpao peppercorns over every 2 hours during the drying process to ensure drying efficiency. After drying, cool to room temperature and take out.

4. A method for extracting Dahongpao Zanthoxylum bungeanum peel according to claim 1, characterized in that: The moisture content of the Dahongpao pepper after drying in the step 2 is lower than 6%.

5. A method for extracting Dahongpao Zanthoxylum bungeanum peel according to claim 1, characterized in that: In the step three, the peel and seeds of the pepper are separated by a screening machine.

6. A method for extracting Dahongpao Zanthoxylum bungeanum peel according to claim 1, characterized in that: In the step 4, the Dahongpao pepper peel is crushed and passed through a 200-mesh sieve. If there is any material remaining on the sieve, the residue is returned and crushed again until all the material is sieved.

7. A method for extracting Dahongpao Zanthoxylum bungeanum peel according to claim 1, characterized in that: The crushed Dahongpao Zanthoxylum bungeanum peel in the step 4 is placed in a supercritical fluid extraction tank, the extraction temperature is raised to 56-60° C., and the extraction pressure is raised to 35-40 MPa; after stabilization for 2-3 minutes, carbon dioxide fluid is added for extraction, the flow rate of the carbon dioxide fluid is 40-50 L / h, the extraction pressure is reduced to 10-15 MPa after extraction for 8-10 minutes, and then the extraction pressure is increased to 40-45 MPa, the extraction temperature is controlled at 58-60° C., and the extraction time is 106-118 minutes. After the extraction is completed, the peel is placed in a separation tank, the pressure in the separation tank is reduced to 3-5 MPa, the temperature is controlled at 40-44° C., and the carbon dioxide fluid is gasified and separated, thereby obtaining the Dahongpao Zanthoxylum bungeanum peel extracted essential oil.

8. The method for extracting Dahongpao Zanthoxylum bungeanum peel according to claim 1, wherein: The recrystallization operation in the described step 5 comprises the following steps: Step 1: adding the Dahongpao Zanthoxylum bungeanum peel extract obtained in step 4 to a dissolving solvent, wherein the mass of the dissolving solvent added is 1.5 to 2 times the mass of the Dahongpao Zanthoxylum bungeanum peel extract, and stirring at a temperature of 40 to 50° C. until completely dissolved; Step 2: After heating to completely dissolve, stop heating and continue stirring to cool to room temperature, then add ethyl acetate dropwise while stirring, and the mass of petroleum ether added should be 4 to 5 times the mass of the essential oil extracted from the peel of Dahongpao pepper. After the addition is complete, stir in an ice-water bath for 50 to 70 minutes; Step 3: Place the solid-liquid mixture from which crystals have precipitated after stirring in an ice-water bath in step 2 in a dedicated refrigerator at -10 to -20°C for 10 to 14 hours.

9. The method for extracting Dahongpao Zanthoxylum bungeanum peel according to claim 8, wherein: The dissolving solvent in step 1 is a mixed solvent obtained by mixing ethanol and cyclopropane in a mass ratio of 2:

1.

10. The method for extracting Dahongpao Zanthoxylum bungeanum peel according to claim 1, wherein: In the step 6, the solid-liquid mixture obtained by the recrystallization operation in the step 5 is separated, and the solid is dried under negative pressure for 130-150 minutes at a temperature of 40-50° C. and a vacuum degree of -0.08-0.04 MPa. After the drying is completed, the temperature is cooled to room temperature and the air pressure in the negative pressure dryer is restored. The dried solid material is taken out, crushed through a 200-mesh sieve, and packaged to obtain the Dahongpao Zanthoxylum bungeanum peel extract.