High-purity xanthoxylin cylinder extraction and column chromatography extraction method

Abstract

The invention discloses a high-purity xanthoxylin cylinder extraction and column chromatography extraction method. The method comprises the following steps: step 1, cleaning new Chinese prickly ash; step 2, airing and crushing; step 3, extracting; 4, after extraction is completed, filtering is conducted, ethyl alcohol is removed, an initial eluent is added, and then silica gel resin powder is added for mixed adsorption; 5, filling a chromatographic column; 6, adding the silica gel resin adsorbing xanthoxylin to the top of the chromatographic column; step 7, starting gradient elution, collecting an eluent by using a test tube, and monitoring whether a substance in the monitored eluent in the elution process is xanthoxylin or not by using TLC (Thin Layer Chromatography); and 8, mixing the obtained eluent containing pure xanthoxylin, then removing the eluent, drying, and crushing to obtain xanthoxylin. According to the method, high-purity xanthoxylin can be obtained through extraction and column chromatography and is used as a calibration object for calibration, the purity detection error in the actual production process of xanthoxylin can be reduced, and the accuracy of the purity detection result of xanthoxylin is ensured.

Description

Technical Field

[0001] The present invention belongs to the field of extraction of sanshools, and particularly relates to a method for extracting high-purity sanshools by cylinder extraction + column chromatography. Background Art

[0002] Sanshools (molecular formula: C 15 H 16 03) belong to alkaloid compounds and have various biological activities. They also have effects such as antioxidation, anti-aging, antibacterial and anti-inflammatory, so current sanshools are widely used in fields such as beauty and medicine.

[0003] Currently, the acquisition of sanshools mainly relies on extraction from Chinese prickly ash. Since current sanshools are mostly used externally on the human skin, a relatively high purity is required. In the actual production of sanshools, in order to ensure the accuracy of product purity detection, it is necessary to regularly use high-purity sanshool calibrators to determine whether there are problems with existing solvents, chromatographic columns, and instruments, so as to avoid inaccurate product purity detection results caused by such problems. Therefore, the purity of the sanshool calibrator needs to reach 99.8%. However, the current production processes of sanshools are uneven, resulting in relatively low purity of many sanshool calibrators, thus affecting the purity detection of sanshools. Summary of the Invention

[0004] The present invention provides a method for extracting high-purity sanshools by cylinder extraction + column chromatography to solve the defects in the prior art.

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

[0006] A method for extracting high-purity sanshools by cylinder extraction + column chromatography includes the following steps:

[0007] Step 1: Wash the freshly picked Chinese prickly ash with clean water, dry it after washing, and soak it in deionized water.

[0008] Step 2: Take out the soaked Chinese prickly ash in Step 1, dry it, and then crush the Chinese prickly ash.

[0009] Step 3: Add the crushed Chinese prickly ash particles in Step 2 into an extraction cylinder and then add an ethanol solution for extraction.

[0010] Step 4: After extraction, filter. After the filtrate is rotary evaporated to remove ethanol, add an initial eluent to dissolve the obtained Chinese prickly ash extract, and then add silica resin powder for thorough mixing and adsorption.

[0011] Step 5: Fill a chromatography column with silica resin powder in the same particle size range as in Step 4. After filling, compact it with the initial eluent.

[0012] Step 6: After the chromatographic column is compacted, add the silica gel resin adsorbed with zanthoxylum bungeanum maxim to the top of the chromatographic column and compact it with the initial eluent.

[0013] Step 7: Start gradient elution, collect the eluate with test tubes, and monitor whether the substances in the monitored eluate during the elution process are zanthoxylum bungeanum maxim by TLC.

[0014] Step 8: Mix the obtained eluate containing pure zanthoxylum bungeanum maxim, then remove the eluate, dry it, and pulverize it to obtain zanthoxylum bungeanum maxim.

[0015] For a method for extracting high-purity zanthoxylum bungeanum maxim by cylinder extraction + column chromatography as described above, the freshly picked zanthoxylum bungeanum maxim in Step 1 is washed 3 - 5 times with clear water, dried, and then added to deionized water and soaked at a temperature of 25 - 35 °C for 20 - 30 min.

[0016] For a method for extracting high-purity zanthoxylum bungeanum maxim by cylinder extraction + column chromatography as described above, the zanthoxylum bungeanum maxim in Step 2 is dried and then pulverized, and after pulverization, it is sieved through a 200-mesh sieve. If there are residues on the sieve, continue to pulverize them until all pass through the sieve finally.

[0017] For a method for extracting high-purity zanthoxylum bungeanum maxim by cylinder extraction + column chromatography as described above, the volume-mass ratio of ethanol used in the extraction in Step 3 to the volume of zanthoxylum bungeanum maxim powder is 6 - 8:1, the extraction temperature is 50 - 60 °C, the extraction time is 1.5 - 2 h, and the cylinder is equipped with a condensation reflux device to condense and liquefy the volatilized ethanol and then re-enter the cylinder.

[0018] For a method for extracting high-purity zanthoxylum bungeanum maxim by cylinder extraction + column chromatography as described above, the addition amount of the initial eluent to the volume-mass ratio of the zanthoxylum bungeanum maxim extract from which ethanol has been removed in Step 4 is: 2 - 3:1, and the addition amount of the silica gel resin powder to the mass ratio of the zanthoxylum bungeanum maxim extract from which ethanol has been removed in Step 4 is: 3 - 4:1.

[0019] For a method for extracting high-purity zanthoxylum bungeanum maxim by cylinder extraction + column chromatography as described above, the particle size of the silica gel resin powder in Step 5 is 200 - 300 mesh, and the initial eluent is petroleum ether.

[0020] For a method for extracting high-purity zanthoxylum bungeanum maxim by cylinder extraction + column chromatography as described above, the mass of the silica gel resin powder used to fill the chromatographic column in Step 5 is 8 - 12 times the mass of the silica gel resin powder that adsorbed the zanthoxylum bungeanum maxim extract in Step 4.

[0021] A method for extracting high-purity zanthoxylum bungeanum maxim extract by cylinder extraction + column chromatography as described above. The gradient elution operation in step seven is as follows: In the first stage, the ratio of the eluent is petroleum ether: ethyl acetate = 60:40, and the elution time is 5 minutes; in the second stage, the ratio of the eluent is petroleum ether: ethyl acetate = 30:70, and the elution time is 10 minutes; in the third stage, the ratio of the eluent is petroleum ether: ethyl acetate: ethanol = 30:65:5, and the elution time is 10 minutes; in the fourth stage, the ratio of the eluent is petroleum ether: ethyl acetate: ethanol = 30:65:5, and the elution time is 10 minutes; in the fifth stage, the ratio of the eluent is ethyl acetate: ethanol = 95:5, and the elution time is 5 minutes; in the sixth stage, the ratio of the eluent is ethyl acetate: ethanol = 90:10, and the elution time is 5 minutes; in the seventh stage, the ratio of the eluent is ethyl acetate: ethanol = 80:20, and the elution time is 5 minutes; in the eighth stage, the ratio of the eluent is ethyl acetate: ethanol = 70:30, and the elution time is 5 minutes; in the ninth stage, the ratio of the eluent is ethyl acetate: ethanol = 60:40, and the elution time is 5 minutes; in the tenth stage, the ratio of the eluent is ethyl acetate: ethanol = 50:50, and the elution time is 10 minutes; the gradient elution process is all under normal pressure elution.

[0022] A method for extracting high-purity zanthoxylum bungeanum maxim extract by cylinder extraction + column chromatography as described above. The pure zanthoxylum bungeanum maxim substance starts to appear from the sixth stage and a mixture appears in the eighth stage.

[0023] A method for extracting high-purity zanthoxylum bungeanum maxim extract by cylinder extraction + column chromatography as described above. After mixing all the eluents containing pure zanthoxylum bungeanum maxim in step eight, the eluent is removed by rotary evaporation, then dried at 60 - 80 °C for 30 - 40 minutes, and pulverized through a 100-mesh sieve to obtain zanthoxylum bungeanum maxim.

[0024] The advantages of the present invention are as follows: The present invention can obtain high-purity zanthoxylum bungeanum maxim through extraction plus column chromatography. Using it as a calibration substance for calibration can reduce the error in purity detection during the actual production process of zanthoxylum bungeanum maxim and ensure the accuracy of its purity detection results. Specific embodiments

[0025] 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. Apparently, the described embodiments are some, but not all, of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0026] Example 1

[0027] Step 1: Wash the freshly picked Chinese prickly ash three times with clean water. After drying, add it to deionized water and soak it at 25°C for 30 minutes.

[0028] Step 2: Take out the soaked Chinese prickly ash from Step 1 and let it dry. After drying, crush the Chinese prickly ash, and pass it through a 200-mesh sieve. If there are residues on the sieve, continue to crush them until all pass through the sieve.

[0029] Step 3: Add the crushed Chinese prickly ash particles from Step 2 into an extraction cylinder and then add an ethanol solution for extraction. The volume-mass ratio of the ethanol used for extraction to the volume of the Chinese prickly ash powder is 6:1. The extraction temperature is 60°C, and the extraction time is 2 hours. The extraction cylinder is equipped with a condensation reflux device to condense and liquefy the volatilized ethanol and then let it re-enter the extraction cylinder.

[0030] Step 4: After the extraction is completed, filter. After the filtrate is rotary evaporated to remove ethanol, add petroleum ether to dissolve the obtained Chinese prickly ash extract, and then add silica gel resin powder for thorough mixing and adsorption. The addition amount of petroleum ether to the volume-mass ratio of the Chinese prickly ash extract after removing ethanol is 2:1. The addition amount of the silica gel resin powder in Step 4 to the mass ratio of the Chinese prickly ash extract after removing ethanol is 3:1. The particle size of the silica gel resin powder is 200 - 300 mesh.

[0031] Step 5: Pack the chromatography column with silica gel resin powder in the same particle size range as in Step 4. After packing, compact it with petroleum ether. The particle size of the silica gel resin powder is 200 - 300 mesh, and the mass of the silica gel resin powder used for packing the chromatography column is 8 times the mass of the silica gel resin powder that adsorbed the Chinese prickly ash extract in Step 4.

[0032] Step 6: After the chromatography column is compacted, add the silica gel resin that adsorbed the xanthoxylin obtained in Step 4 to the top of the chromatography column and compact it with petroleum ether.

[0033] Step 7: Start gradient elution, collect the eluate with test tubes, and monitor whether the substance in the monitored eluate during the elution process is sanshool by TLC. The gradient elution operation is as follows: In the first stage, the ratio of the eluent is petroleum ether: ethyl acetate = 60:40, and the elution time is 5 min; in the second stage, the ratio of the eluent is petroleum ether: ethyl acetate = 30:70, and the elution time is 10 min; in the third stage, the ratio of the eluent is petroleum ether: ethyl acetate: ethanol = 30:65:5, and the elution time is 10 min; in the fourth stage, the ratio of the eluent is petroleum ether: ethyl acetate: ethanol = 30:65:5, and the elution time is 10 min; in the fifth stage, the ratio of the eluent is ethyl acetate: ethanol = 95:5, and the elution time is 5 min; in the sixth stage, the ratio of the eluent is ethyl acetate: ethanol = 90:10, and the elution time is 5 min; in the seventh stage, the ratio of the eluent is ethyl acetate: ethanol = 80:20, and the elution time is 5 min; in the eighth stage, the ratio of the eluent is ethyl acetate: ethanol = 70:30, and the elution time is 5 min; in the ninth stage, the ratio of the eluent is ethyl acetate: ethanol = 60:40, and the elution time is 5 min; in the tenth stage, the ratio of the eluent is ethyl acetate: ethanol = 50:50, and the elution time is 10 min. The gradient elution process is all under normal pressure. The pure sanshool substance starts to appear from the sixth stage and a mixture appears in the eighth stage. Select the eluent of all pure substances by TLC monitoring. At the same time, discard the eluate of the test tube where the earliest pure substance appears and the next three test tubes, as well as the eluate of the test tube where the last pure substance appears and the previous three test tubes to ensure the purity of the substance;

[0034] Step 8: After mixing all the eluates containing pure sanshool, remove the eluate by rotary evaporation, then dry it at 60 °C for 40 min, crush it through a 100-mesh sieve to obtain sanshool, and conduct purity detection. Its purity is 99.9%.

[0035] Example 2

[0036] Step 1: Wash the freshly picked Chinese prickly ash 5 times with clean water, dry it, and add it to deionized water and soak it at 35 °C for 20 min;

[0037] Step 2: Take out the soaked Chinese prickly ash in Step 1 and let it dry. After drying the Chinese prickly ash, crush it, and sieve it through a 200-mesh sieve. If there are residues on the sieve, continue to crush it until all pass through the sieve;

[0038] Step 3: Add the crushed Chinese prickly ash particles in Step 2 to the extraction cylinder and then add an ethanol solution for extraction. The volume-mass ratio of ethanol used for extraction to the volume of Chinese prickly ash powder is 8:1. The extraction temperature is 50 °C, and the extraction time is 1.5 h. The extraction cylinder is equipped with a condensing reflux device to condense and liquefy the volatilized ethanol and then enter the extraction cylinder;

[0039] Step 4: After extraction is completed, filter. After the filtrate is rotary evaporated to remove ethanol, add petroleum ether to the obtained Zanthoxylum extract to dissolve it, and then add silica resin powder for thorough mixing and adsorption. The volume-mass ratio of the added petroleum ether to the Zanthoxylum extract after ethanol removal is 3:1. The mass ratio of the added silica resin powder to the Zanthoxylum extract after ethanol removal in Step 4 is 4:1. The particle size of the silica resin powder is 200 - 300 mesh;

[0040] Step 5: Pack the chromatography column with silica resin powder in the same particle size range as in Step 4. After packing is completed, compact it with petroleum ether. The particle size of the silica resin powder is 200 - 300 mesh. The mass of the silica resin powder used for packing the chromatography column is 12 times the mass of the silica resin powder that adsorbed the Zanthoxylum extract in Step 4;

[0041] Step 6: After the chromatography column is compacted, add the silica resin that adsorbed zanthoxylum in Step 4 to the top of the chromatography column and compact it with petroleum ether;

[0042] Step 7: Start gradient elution, collect the eluate with test tubes, and monitor whether the substance in the monitored eluate during the elution process is zanthoxylum by TLC. The gradient elution operation is as follows: In the first stage, the ratio of the eluent is petroleum ether:ethyl acetate = 60:40, and the elution time is 5 min; in the second stage, the ratio of the eluent is petroleum ether:ethyl acetate = 30:70, and the elution time is 10 min; in the third stage, the ratio of the eluent is petroleum ether:ethyl acetate:ethanol = 30:65:5, and the elution time is 10 min; in the fourth stage, the ratio of the eluent is petroleum ether:ethyl acetate:ethanol = 30:65:5, and the elution time is 10 min; in the fifth stage, the ratio of the eluent is ethyl acetate:ethanol = 95:5, and the elution time is 5 min; in the sixth stage, the ratio of the eluent is ethyl acetate:ethanol = 90:10, and the elution time is 5 min; in the seventh stage, the ratio of the eluent is ethyl acetate:ethanol = 80:20, and the elution time is 5 min; in the eighth stage, the ratio of the eluent is ethyl acetate:ethanol = 70:30, and the elution time is 5 min; in the ninth stage, the ratio of the eluent is ethyl acetate:ethanol = 60:40, and the elution time is 5 min; in the eighth stage, the ratio of the eluent is ethyl acetate:ethanol = 50:50, and the elution time is 10 min. The gradient elution process is all under atmospheric pressure. The pure zanthoxylum substance starts to appear from the sixth stage and a mixture appears in the eighth stage. Select the eluent of all pure substances by TLC monitoring. At the same time, discard the eluate of the test tube with the earliest pure substance and the next three test tubes, as well as the eluate of the test tube with the last pure substance and the previous three test tubes to ensure the purity of the substance;

[0043] Step 8: Mix all the eluents containing pure zanthoxylum bungeanum maxim extract, then remove the eluent by rotary evaporation, and then dry it at 80 °C for 30 min. After pulverizing and passing through a 100-mesh sieve, zanthoxylum bungeanum maxim extract is obtained and its purity is detected to be 99.8%.

[0044] Example 3

[0045] Step 1: Wash the freshly picked zanthoxylum bungeanum maxim with water 3 - 5 times, dry it, and then soak it in deionized water at 30 °C for 25 min.

[0046] Step 2: Take out the soaked zanthoxylum bungeanum maxim in Step 1 and let it dry. After drying, pulverize it and pass it through a 200-mesh sieve. If there are residues on the sieve, continue to pulverize them until all pass through the sieve.

[0047] Step 3: Add the pulverized zanthoxylum bungeanum maxim particles in Step 2 into the extraction cylinder and then add ethanol solution for extraction. The volume-mass ratio of ethanol used for extraction to the volume of zanthoxylum bungeanum maxim powder is 7:1. The extraction temperature is 55 °C and the extraction time is 1.8 h. The extraction cylinder is equipped with a condensation reflux device to condense and liquefy the volatilized ethanol and then let it enter the extraction cylinder again.

[0048] Step 4: After extraction, filter. After the filtrate is rotary evaporated to remove ethanol, add petroleum ether to dissolve the obtained zanthoxylum bungeanum maxim extract and then add silica gel resin powder for thorough mixing and adsorption. The addition amount of petroleum ether to the volume-mass ratio of the zanthoxylum bungeanum maxim extract after removing ethanol is: 2.5:1. The addition amount of silica gel resin powder in Step 4 to the mass ratio of the zanthoxylum bungeanum maxim extract after removing ethanol is: 3.5:1. The particle size of the silica gel resin powder is 200 - 300 mesh.

[0049] Step 5: Fill the chromatography column with silica gel resin powder in the same particle size range as in Step 4. After filling, compact it with petroleum ether. The particle size of the silica gel resin powder is 200 - 300 mesh. The mass of silica gel resin powder used for filling the chromatography column is 10 times the mass of silica gel resin powder that adsorbed zanthoxylum bungeanum maxim extract in Step 4.

[0050] Step 6: After the chromatography column is compacted, add the silica gel resin that adsorbed zanthoxylum bungeanum maxim extract in Step 4 to the top of the chromatography column and compact it with petroleum ether.

[0051] Step 7: Start gradient elution, collect the eluate with test tubes, and monitor whether the substance in the monitored eluate during the elution process is sanshools by TLC. The gradient elution operation is as follows: In the first stage, the ratio of the eluent is petroleum ether: ethyl acetate = 60:40, and the elution time is 5 min; in the second stage, the ratio of the eluent is petroleum ether: ethyl acetate = 30:70, and the elution time is 10 min; in the third stage, the ratio of the eluent is petroleum ether: ethyl acetate: ethanol = 30:65:5, and the elution time is 10 min; in the fourth stage, the ratio of the eluent is petroleum ether: ethyl acetate: ethanol = 30:65:5, and the elution time is 10 min; in the fifth stage, the ratio of the eluent is ethyl acetate: ethanol = 95:5, and the elution time is 5 min; in the sixth stage, the ratio of the eluent is ethyl acetate: ethanol = 90:10, and the elution time is 5 min; in the seventh stage, the ratio of the eluent is ethyl acetate: ethanol = 80:20, and the elution time is 5 min; in the eighth stage, the ratio of the eluent is ethyl acetate: ethanol = 70:30, and the elution time is 5 min; in the ninth stage, the ratio of the eluent is ethyl acetate: ethanol = 60:40, and the elution time is 5 min; in the tenth stage, the ratio of the eluent is ethyl acetate: ethanol = 50:50, and the elution time is 10 min. The above gradient elution process is all under normal pressure. The pure sanshools substance starts to appear from the sixth stage and a mixture appears in the eighth stage. Select the eluent of all pure substances by TLC monitoring. At the same time, discard the eluate of the test tube with the earliest pure substance and the next three test tubes, as well as the eluate of the test tube with the last pure substance and its first three test tubes to ensure the purity of the substance;

[0052] Step 8: After mixing all the eluates containing pure sanshools, remove the eluate by rotary evaporation, then dry it at 70 °C for 35 min, pulverize it through a 100-mesh sieve to obtain sanshools, and conduct purity detection. Its purity is 99.9%.

[0053] The purity of the sanshools prepared in Examples 1-3 of the present invention is all above 99.8%. As a calibrator, it reduces the error in purity detection during the actual production process of sanshools and ensures the accuracy of its purity detection results.

[0054] Finally, it should be noted that the above examples are only used to illustrate the technical solutions of the present invention, not to limit them. Although the present invention has been described in detail with reference to the foregoing examples, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing examples, or perform equivalent replacements for some of the technical features. And these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for extracting high-purity zanthoxylum extract by cylinder extraction + column chromatography, characterized in that: It includes the following steps: Step 1: Wash the freshly picked Chinese prickly ash with clean water, dry it after washing, and soak it in deionized water; Step 2: Take out the soaked Chinese prickly ash in Step 1, dry it in the air, and then crush the Chinese prickly ash; Step 3: Add the crushed Chinese prickly ash particles in Step 2 into the extraction cylinder and then add an ethanol solution for extraction; Step 4: After the extraction is completed, filter it. After the filtrate is rotary evaporated to remove ethanol, add the initial eluent to dissolve the obtained Chinese prickly ash extract, and then add silica gel resin powder for thorough mixing and adsorption; Step 5: Fill the chromatography column with silica gel resin powder in the same particle size range as in Step 4. After the filling is completed, compact it with the initial eluent; Step 6: After the chromatography column is compacted, add the silica gel resin adsorbed with sanshool in Step 4 to the top of the chromatography column and compact it with the initial eluent; Step 7: Start gradient elution, collect the eluate with a test tube, and monitor whether the substance in the monitored eluate during the elution process is sanshool by TLC; Step 8: Mix the obtained eluate containing pure sanshool, then remove the eluate, dry it, crush it to obtain sanshool.

2. A method for extracting high-purity zanthoxylum extract by cylinder extraction + column chromatography according to claim 1, characterized in that: The freshly picked Chinese prickly ash in Step 1 is washed with clean water 3 - 5 times. After drying, it is added to deionized water and soaked at a temperature of 25 - 35°C for 20 - 30 min.

3. A method for extracting high-purity zanthoxylum extract by cylinder extraction + column chromatography according to claim 1, characterized in that: The Chinese prickly ash in Step 2 is dried in the air and then crushed. After crushing, it is sieved through a 200 - mesh sieve. If there are residues on the sieve, continue to crush them until all pass through the sieve.

4. A method for extracting high-purity zanthoxylum extract by cylinder extraction + column chromatography according to claim 1, characterized in that: In Step 3, the volume - to - volume - mass ratio of ethanol used for extraction to the volume of Chinese prickly ash powder is 6 - 8:1, the extraction temperature is 50 - 60°C, the extraction time is 1.5 - 2 h, and the extraction cylinder is equipped with a condensing reflux device to condense and liquefy the volatilized ethanol and then re - enter the extraction cylinder.

5. A method for extracting high-purity xanthoxylin by cylinder extraction + column chromatography according to claim 1, characterized in that: In Step 4, the addition amount of the initial eluent to the volume - to - volume - mass ratio of the Chinese prickly ash extract after removing ethanol is 2 - 3:

1. In Step 4, the addition amount of silica gel resin powder to the mass ratio of the Chinese prickly ash extract after removing ethanol is 3 - 4:

1.

6. A method for extracting high-purity zanthoxylumol by cylinder extraction + column chromatography according to claim 1, characterized in that: In Step 5, the particle size of the silica gel resin powder is 200 - 300 mesh, and the initial eluent is petroleum ether.

7. A method for extracting high-purity zanthoxylum extract by cylinder extraction + column chromatography according to claim 1, characterized in that: In Step 5, the mass of the silica gel resin powder used to fill the chromatography column is 8 - 12 times the mass of the silica gel resin powder adsorbed with the Chinese prickly ash extract in Step 4.

8. A method for extracting high-purity zanthoxylum extract by cylinder extraction + column chromatography according to claim 1, characterized in that: The gradient elution operation in Step 7 is as follows: In the first stage, the ratio of the eluent is petroleum ether:ethyl acetate = 60:40, and the elution time is 5 min; in the second stage, the ratio of the eluent is petroleum ether:ethyl acetate = 30:70, and the elution time is 10 min; in the third stage, the ratio of the eluent is petroleum ether:ethyl acetate:ethanol = 30:65:5, and the elution time is 10 min; in the fourth stage, the ratio of the eluent is petroleum ether:ethyl acetate:ethanol = 30:65:5, and the elution time is 10 min; in the fifth stage, the ratio of the eluent is ethyl acetate:ethanol = 95:5, and the elution time is 5 min; in the sixth stage, the ratio of the eluent is ethyl acetate:ethanol = 90:10, and the elution time is 5 min; in the seventh stage, the ratio of the eluent is ethyl acetate:ethanol = 80:20, and the elution time is 5 min; in the eighth stage, the ratio of the eluent is ethyl acetate:ethanol = 70:30, and the elution time is 5 min; in the ninth stage, the ratio of the eluent is ethyl acetate:ethanol = 60:40, and the elution time is 5 min; in the tenth stage, the ratio of the eluent is ethyl acetate:ethanol = 50:50, and the elution time is 10 min; the gradient elution process is carried out under normal pressure.

9. A method for extracting high-purity xanthoxylin by cylinder extraction + column chromatography according to claim 8, characterized in that: The pure substance of xanthoxylin starts to appear from the sixth stage and a mixture appears in the eighth stage.

10. A method for extracting high-purity xanthoxylin by cylinder extraction + column chromatography according to claim 8, characterized in that: In Step 8, after mixing all the eluents containing pure xanthoxylin, the eluent is removed by rotary evaporation, then dried at 60 - 80 °C for 30 - 40 min, pulverized and passed through a 100-mesh sieve to obtain xanthoxylin.