CN115466647A - Preparation method of itching-relieving essential oil - Google Patents
Preparation method of itching-relieving essential oil Download PDFInfo
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Abstract
The invention belongs to the field of plant essential oil, and particularly discloses a preparation method of itching-relieving essential oil, which comprises the following steps: (1) extracting: pulverizing herba Artemisiae Annuae, adding into extraction tank, adding solvent, and heating for extraction; (2) concentrating: heating and concentrating the extracting solution, and volatilizing the solvent until no solvent smell exists; (3) silica gel column packing: filling the silica gel into a chromatographic column, and compacting; (4) sample mixing: mixing the concentrated extract obtained in the step (2) with silica gel, stirring, drying, and adding to the silica gel column obtained in the step (3) for compaction; (5) removing impurities: eluting a silica gel column by using a solvent to remove impurities; (6) elution: eluting with mixed solvent, and collecting eluate; (7) concentrating and drying: heating and concentrating the eluent, and drying to obtain a dry extract; (8) preparing essential oil liquid: and adding a solvent into the dry extract, heating for dissolving, coarsely filtering while hot, cooling the filtrate, and centrifuging to obtain a supernatant which is the itching relieving essential oil. The essential oil is pure natural, has no toxic or side effect, can relieve swelling and itching and has obvious effect.
Description
Technical Field
The invention belongs to the field of plant essential oil, and particularly discloses a preparation method of itching relieving essential oil.
Background
Red swelling, blisters and pimples can appear after the biting of mosquitoes, and severe pruritus is accompanied. After scratching, the skin is easy to be ulcerated and infected with pus. The long-term repeated stimulation is easy to form nodules which affect the life quality of people, and the long-term pruritus is more often uncomfortable to human bodies, so that effective treatment medicines are lacked, and the life quality is seriously reduced.
In China, the sweet wormwood has long-term clinical medication history and practice, has the effects of clearing deficiency heat, cooling blood, removing heat from the blood, relieving summer heat and preventing malaria, and is an important traditional Chinese medicine for treating malaria. Researches show that the main chemical components of the composition are sesquiterpenes, diterpenes, flavonoids, phenylpropanoids, coumarins, volatile oil and the like. The sweet wormwood extract and its monomer compound have antimalarial, anti-tumor, antibacterial, insecticidal, antipyretic, anti-inflammatory, and immunoregulatory effects.
The Chinese medicine contains several natural medicinal components, especially the sweet wormwood extract, and can kill several parasitic diseases in human body and make them metabolized with human body and excreted out of human body.
The existing antipruritic medicines have the defects of poor effect, obvious side effect, inconvenient administration and the like, although the existing artemisia apiacea essential oil is on the market at present, the artemisia apiacea essential oil is all the components of the artemisia apiacea extract, and various active components are not further refined and concentrated to distinguish the artemisia apiacea essential oil, so that the economic effect and the antipruritic effect are not satisfactory.
Disclosure of Invention
Aiming at the situation, the invention discloses a preparation method of itching relieving essential oil, and provides novel itching relieving essential oil which is prepared from a common sweet wormwood herb traditional Chinese medicine extract, is combined with auxiliary materials and applied in a smearing mode, has the basic effects of detumescence and itching relieving, has an obvious effect, and can practically solve the problems of insect and mosquito bite and other pruritus.
The technical scheme of the invention is as follows:
the preparation method of the itching relieving essential oil comprises the following steps:
(1) Extraction: pulverizing herba Artemisiae Annuae, adding into extraction tank, adding solvent, and heating for extraction;
(2) Concentration: heating and concentrating the extracting solution, and volatilizing the solvent until no solvent smell exists;
(3) Loading on a silica gel column: filling the silica gel into a chromatographic column, and compacting;
(4) Mixing samples: mixing the concentrated extract obtained in the step (2) with silica gel, stirring, drying, and adding to the silica gel column obtained in the step (3) for compaction;
(5) Removing impurities: eluting the silica gel column by using a solvent to remove impurities;
(6) And (3) elution: eluting with mixed solvent, and collecting eluate;
(7) Concentration and drying: heating and concentrating the eluent, and drying to obtain a dry extract;
(8) Preparing essential oil liquid: and adding a solvent into the dry extract, heating for dissolving, roughly filtering while the dry extract is hot, cooling the filtrate, and centrifuging to obtain a supernatant which is the itching relieving essential oil.
Preferably, the method comprises the following steps:
(1) Extraction: pulverizing herba Artemisiae Annuae, adding into extraction tank, adding organic solvent, heating and reflux-extracting for 2 times and 2 times, and mixing extractive solutions;
(2) Concentration: concentrating the extracting solution in the step (1) until no alcohol smell exists;
(3) Loading on a silica gel column: according to the step (2), the concentrated solution without alcoholic smell: silica gel (1;
(4) Mixing samples: and (3) the mass ratio of the alcohol smell-free step (2) to the silica gel (1:1) is less, and the steps of mixing, stirring and drying are carried out. Adding the mixture to the silica gel column obtained in the step (3) for compaction;
(5) Removing impurities: leaching the silica gel column in the step (3) by using 2BV petroleum ether;
(6) And (3) elution: using 6BV petroleum ether: eluting with ethyl acetate (1:5) at a volume ratio, and collecting the eluate; the first 3 column volumes and the last 3 column volumes are separated;
(7) Concentration and drying: concentrating the eluent in the step (6), slightly drying the collected liquid, preparing a dry extract A artemisinin crude product from the first 3 column volumes, and preparing a dry extract B from the last 3 column volumes;
(8) Essential oil liquid: and (3) heating and dissolving the dry extract B in the step (7) with 75% ethanol (1).
Further, in the preparation method of the itching relieving essential oil, in the step (1), the artemisia annua raw material is artemisia annua stems and leaves.
Further, in the above preparation method of the itching relieving essential oil, the solvent in the step (1) is a lipophilic organic solvent.
Further, in the above preparation method of the itching relieving essential oil, the solvent in the step (1) is at least one of methanol, ethanol and chloroform; preferably, it is at least one of methanol and ethanol.
Further, in the preparation method of the itching-relieving essential oil, in the step (1), the heating temperature is 40-80 ℃, and the heating time is 0.5-4h. Preferably, the heating temperature is 70 ℃, and the extraction time is 2h.
Further, in the preparation method of the itching relieving essential oil, the concentration temperature in the step (2) is 50-80 ℃; preferably, the concentration temperature is 70 deg.C
Further, in the preparation method of the itching relieving essential oil, the mesh number of the silica gel in the step (3) and the step (4) is 100-300 meshes.
Further, in the above preparation method of the itching relieving essential oil, the solvent in the step (5) is at least one of petroleum ether, n-hexane and cyclohexane; preferably, the solvent is petroleum ether.
Further, in the above preparation method of the itching relieving essential oil, the mixed solvent in the step (6) is at least 2 of petroleum ether, n-hexane, cyclohexane, ethyl acetate, dichloromethane and chloroform; preferably, the eluent is petroleum ether: ethyl acetate (1:5) volume ratio.
Further, in the preparation method of the itching relieving essential oil, the concentration temperature in the step (7) is 50-80 ℃; preferably, the temperature is 50 ℃.
Further, in the preparation method of the itching relieving essential oil, the solvent in the step (8) is at least one of ethanol and methanol, and the heating temperature is 50-80 ℃. Preferably, the temperature is 70 ℃ and the solvent is 75% ethanol.
The invention has the following beneficial effects:
the novel itching relieving essential oil is developed by combining related itching relieving or traditional Chinese medicine products on the market through a drug administration way and a drug administration method by utilizing the characteristic that the essential oil is easy to absorb and protects the skin and adopting a quick drug administration way and a quick drug administration mode, is novel and convenient to carry, has an obvious effect and meets the requirements of various crowds by taking Chinese herbal medicines as the purpose.
Detailed Description
The preparation method of the itching relieving essential oil comprises the following steps:
(1) Extraction: pulverizing herba Artemisiae Annuae, adding into extraction tank, adding organic solvent, heating and reflux-extracting for 2 times and 2 times, and mixing extractive solutions;
(2) Concentration: concentrating the extracting solution in the step (1) until no alcohol smell exists;
(3) Loading on a silica gel column: according to the step (2), the concentrated solution without alcoholic smell: silica gel (1;
(4) Mixing samples: and (3) the mass ratio of the alcohol smell-free step (2) to the silica gel (1:1) is less, and the steps of mixing, stirring and drying are carried out. Adding the mixture to the silica gel column obtained in the step (3) for compaction;
(5) Removing impurities: leaching the silica gel column in the step (3) by using 2BV petroleum ether;
(6) And (3) elution: using 6BV petroleum ether: eluting with ethyl acetate (1:5) in volume ratio, and collecting the eluate; the first 3 column volumes and the last 3 column volumes are separated;
(7) Concentration and drying: concentrating the eluent in the step (6), slightly drying the collected liquid, and preparing a dry extract A from the eluent with the previous 3 column volumes: preparing a crude artemisinin product from the eluent with the last 3 column volumes to obtain a dry extract B;
(8) Preparing essential oil liquid: and (3) heating and dissolving the dry extract B in the step (7) with 75% ethanol (1).
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The reagents or instruments used in the examples of the present invention are not indicated by manufacturers, and are all conventional reagent products commercially available.
Example 1
(1) Extraction: pulverizing stem and leaf of Artemisia annua 100kg, extracting with 6 times of 600L methanol at 70 deg.C for 2 times (each for 2 hr), and mixing extractive solutions;
(2) Concentration: concentrating the extractive solution at 70 deg.C until there is no alcohol smell, and slightly drying to get 30kg of paste;
(3) Column assembling: 450kg200 to 300 mesh silica gel is weighed, added into a chromatographic column (800 × 60cm), compacted,
(4) Mixing samples: weighing 30kg200 to 300-mesh silica gel and 30kg of the micro-dry paste in the step (2), dissolving in methanol, heating, mixing the sample, and concentrating to dryness; adding the upper layer of the chromatographic column in the operation (3), and compacting by using a little silica gel.
(5) Removing impurities: eluting silica gel column with 2BV800L petroleum ether;
(6) And (3) elution: eluting with 6BV2400L petroleum ether and ethyl acetate (1:5), and collecting effluent 2400L, front 1200L and rear 1200L;
(7) Concentration and drying: concentrating the collected liquid in the step (6) at 50 ℃, slightly drying, and drying at 70 ℃ to obtain 8kg (front 1200L) of crude artemisinin of the dry extract and 12kg (rear 1200L) of dry extract of the mixture;
(8) Preparing essential oil liquid: and (4) heating and dissolving 12kg of the mixture dry extract obtained in the step (7) with 180L of 75% ethanol at 70 ℃, coarsely filtering while hot, cooling the filtrate, and centrifuging to obtain supernatant, namely 170L of essential oil solution.
Example 2
(1) Extraction: pulverizing stem and leaf of Artemisia annua 150kg, extracting with 6 times of 900L methanol at 70 deg.C for 2 times (each for 2 hr), mixing extractive solutions,
(2) And (3) concentrating: concentrating the extractive solution at 70 deg.C until no alcohol smell is produced, slightly drying to obtain extract 45kg,
(3) Column assembling: weighing 675kg200 to 300 mesh silica gel, adding into a chromatographic column (800 × 60cm), compacting,
(4) Mixing samples: weighing 45kg200 to 300-mesh silica gel and 45kg of the micro-dry paste in the step (2), dissolving in methanol, heating, mixing, concentrating, adding the upper layer of the chromatographic column in the operation (3), and compacting by using little silica gel.
(5) Removing impurities: eluting silica gel column with 2BV1200L petroleum ether;
(6) And (3) elution: eluting with 6BV3600L petroleum ether and ethyl acetate (1:5), collecting eluate 3600L 1800L before and 1850L after,
(7) Concentration and drying: concentrating and slightly drying the collected liquid in the step (6) at 50 ℃, and drying at 70 ℃ to obtain 12kg (front 1200L) of crude artemisinin of the dry extract and 18kg (rear 1250L) of dry extract of the mixture;
(8) Preparing essential oil liquid: and (3) heating and dissolving the mixture dry extract obtained in the step (7) with 270L of 75% ethanol at 70 ℃, coarsely filtering while hot, cooling the filtrate, and centrifuging to obtain supernatant, namely the essential oil liquid 285L.
Example 3
(1) Extraction: pulverizing stem and leaf of Artemisia annua 200kg, extracting with 6 times of 1200L methanol at 70 deg.C for 2 times (each for 2 hr), mixing extractive solutions,
(2) Concentration: concentrating the extractive solution at 70 deg.C until no alcohol smell is produced, slightly drying 59.8kg,
(3) Column assembling: weighing 900kg200 to 300 mesh silica gel, adding into a chromatographic column (800 × 60cm), compacting,
(4) Sample mixing: weighing 60kg200-300 mesh silica gel and 60kg of the micro-dry paste in the step (2), dissolving in methanol, heating, mixing, concentrating, adding the upper layer of the chromatographic column in the operation (3), and compacting by using little silica gel.
(5) Removing impurities: eluting silica gel column with 2BV1800L petroleum ether;
(6) And (3) elution: eluting with 6BV5400L petroleum ether and ethyl acetate (1:5), collecting effluent 5400L front 2700L and back 2700L;
(7) Concentration and drying: concentrating and slightly drying the collected liquid in the step (6) at 50 ℃, and drying at 70 ℃ to obtain 16kg (front 2700L) of dry extract artemisinin crude product and 24kg (rear 2700L) of mixture dry extract;
(8) Preparing essential oil liquid: and (3) heating and dissolving the dry extract of the mixture obtained in the step (7) with 360L of 75% ethanol at 70 ℃, coarsely filtering while hot, cooling the filtrate, and centrifuging to obtain supernatant, namely 340L of essential oil solution.
Example 4
(1) Extraction: pulverizing stem and leaf of Artemisia annua 200kg, extracting with 6 times of 1200L methanol at 70 deg.C for 2 times (each for 2 hr), mixing extractive solutions,
(2) Concentration: concentrating the extractive solution at 70 deg.C until there is no alcohol smell, and slightly drying to get a paste 59.5kg,
(3) Column assembling: weighing 900kg200 to 300 mesh silica gel, adding into a chromatographic column (800 × 60cm), compacting,
(4) Sample mixing: weighing 60kg200-300 mesh silica gel and 60.5kg of the micro-dry paste in the step (2), dissolving in methanol, heating, stirring, concentrating, adding the upper layer of the chromatographic column in the step (3), and compacting by using a small amount of silica gel.
(5) Removing impurities: eluting silica gel column with 2BV1800L petroleum ether;
(6) And (3) elution: eluting with 6BV5400L petroleum ether and ethyl acetate (1:5), collecting effluent 5400L front 2700L and back 2700L;
(7) And (3) concentrating and drying: concentrating and slightly drying the collected liquid in the step (6) at 50 ℃, and drying at 70 ℃ to obtain 15.8kg (front 2700L) of dry extract artemisinin crude product and 24.5kg (rear 2700L) of mixture dry extract;
(8) Preparing essential oil liquid: and (4) heating and dissolving the dry extract of the mixture obtained in the step (7) with 360L of 75% ethanol at 70 ℃, coarsely filtering while hot, cooling the filtrate, and centrifuging to obtain supernatant, namely the essential oil solution 341L.
Example 5
(1) Extraction: pulverizing stem and leaf of Artemisia annua 200kg, extracting with 6 times of 1200L methanol at 70 deg.C for 2 times (each for 2 hr), mixing extractive solutions,
(2) Concentration: concentrating the extractive solution at 70 deg.C until no alcohol smell is produced, slightly drying 59.7kg,
(3) Column assembling: weighing 900kg200 to 300 mesh silica gel, adding into a chromatographic column (800 × 60cm), compacting,
(4) Mixing samples: and (3) weighing 60kg200-300 mesh silica gel and 60.3kg of the micro-dry paste in the step (2), dissolving in methanol, heating, stirring, concentrating, drying, adding the upper layer of the chromatographic column in the step (3), and compacting by using small-point silica gel.
(5) Removing impurities: eluting silica gel column with 2BV1800L petroleum ether;
(6) And (3) elution: eluting with 6BV5400L petroleum ether and ethyl acetate (1:5), collecting effluent 5400L front 2700L and back 2700L;
(7) Concentration and drying: concentrating the collected liquid in the step (6) at 50 ℃, slightly drying, and drying at 70 ℃ to obtain 15.7kg (front 2700L) of a dry extract artemisinin crude product and 23.9kg (rear 2700L) of a mixture dry extract;
(8) Preparing essential oil liquid: and (4) heating and dissolving the dry extract of the mixture obtained in the step (7) with 360L of 75% ethanol at 70 ℃, coarsely filtering while hot, cooling the filtrate, and centrifuging to obtain supernatant, namely 340L of essential oil solution.
Test example 1
Crude artemisinin and dry extract of the mixture, as well as essential oil solutions were prepared according to the above examples and the yield results are shown in the table below.
Table 1 table of preparation parameters for examples 1-5.
The results in Table 1 show that the preparation method has mild preparation conditions and high yield of artemisinin and target essential oil.
Test example 2
The test of the antipruritic effect comprises selecting 35 rabbits weighing about 2kg, randomly dividing into a blank control group 1, an example group 5 and a market comparison group 1, wherein each group comprises 5 rabbits, 1cm x 2cm is bought on the left paw back of each group, each group is coated with 2ml of samples, and the blank control group is coated with 2ml of distilled water. The above parts were smeared with histamine phosphate after 10min, and after 5min, an equal amount was smeared 1 time until licking occurred, and the total amount of histamine phosphate was recorded, and the results are shown in table 2.
TABLE 2 test of antipruritic effect
The result shows that the 5 groups of the invention have higher itching relieving threshold which is obviously higher than that of the blank control group and the market control group, and the invention has better itching relieving effect.
The above-mentioned embodiments only represent a limited number of preferred embodiments of the present invention, and the description is specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (10)
1. The preparation method of the itching relieving essential oil is characterized by comprising the following steps:
(1) Extraction: pulverizing herba Artemisiae Annuae, adding into extraction tank, adding solvent, and heating for extraction;
(2) Concentration: heating and concentrating the extracting solution, and volatilizing the solvent until no solvent smell exists;
(3) Loading on a silica gel column: filling the silica gel into a chromatographic column, and compacting;
(4) Mixing samples: mixing the concentrated extract obtained in the step (2) with silica gel, stirring, drying, and adding to the silica gel column obtained in the step (3) for compaction;
(5) Removing impurities: eluting a silica gel column by using a solvent to remove impurities;
(6) And (3) elution: eluting with mixed solvent, and collecting eluate;
(7) Concentration and drying: heating and concentrating the eluent, and drying to obtain a dry extract;
(8) Preparing essential oil liquid: and adding a solvent into the dry extract, heating for dissolving, roughly filtering while the dry extract is hot, cooling the filtrate, and centrifuging to obtain a supernatant which is the itching relieving essential oil.
2. The method for preparing itching relieving essential oil according to claim 1, wherein the solvent in the step (1) is a lipophilic organic solvent.
3. The method for preparing itching-relieving essential oil according to claim 1, wherein the solvent in step (1) is at least one of methanol, ethanol and chloroform.
4. The method for preparing itching-relieving essential oil according to claim 1, wherein in the step (1), the heating temperature is 40-80 ℃ and the heating time is 0.5-4h.
5. The method for preparing itching relieving essential oil according to claim 1, wherein the temperature of the concentration in the step (2) is 50-80 ℃.
6. The method for preparing itching-relieving essential oil according to claim 1, wherein the mesh number of the silica gel in the step (3) and the step (4) is 100-300 meshes.
7. The method for preparing itching-relieving essential oil according to claim 1, wherein the solvent in the step (5) is at least one of petroleum ether, n-hexane and cyclohexane.
8. The method for preparing itching-relieving essential oil according to claim 1, wherein the mixed solvent in step (6) is at least 2 of petroleum ether, n-hexane, cyclohexane, ethyl acetate, dichloromethane and chloroform.
9. The method for preparing essential oil for relieving itching according to claim 1, wherein the temperature of the concentration in the step (7) is 50-80 ℃.
10. The method for preparing itching-relieving essential oil according to claim 1, wherein the solvent of step (8) is at least one of ethanol and methanol, and the heating temperature is 50-80 ℃.
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