CN115895782A - A black tiger essential oil, its preparation method and application in preparing product with repercussive and analgesic effects - Google Patents
A black tiger essential oil, its preparation method and application in preparing product with repercussive and analgesic effects Download PDFInfo
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 112
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 230000000202 analgesic effect Effects 0.000 title claims description 7
- 239000000284 extract Substances 0.000 claims abstract description 71
- 238000000034 method Methods 0.000 claims abstract description 20
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- Medicines Containing Plant Substances (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to the technical field of natural products, and particularly discloses black tiger essential oil, a preparation method thereof and application thereof in preparation of products with swelling and pain relieving effects. The preparation method of the black tiger essential oil comprises the following steps of mixing the black tiger root and the black tiger leaf, putting the mixture into a steam distillation device, adding water into the steam distillation device for steam distillation, and separating oil phase components in a distillation product after the distillation is finished to obtain the black tiger essential oil. Furthermore, the black tiger essential oil also comprises a black tiger extract. Researches show that the black tiger essential oil prepared by the method has better effects of diminishing swelling and relieving pain; particularly, the black cutworm extract prepared by the method disclosed by the invention is added into the black cutworm essential oil, so that the swelling and pain relieving effects of the black cutworm essential oil can be greatly improved.
Description
Technical Field
The invention relates to the technical field of natural products, in particular to black tiger essential oil, a preparation method thereof and application thereof in preparing products with swelling and pain relieving effects.
Background
Black tiger, known under the scientific name Kadsura coccinea (lem.) a.c. smith, is a plant of the genus Kadsura of the family magnoliaceae. The whole plant of the root to the leaf can be used as a medicine, and has the functions of clearing heat and detoxicating, dispelling wind and activating collaterals, regulating qi and relieving pain, clearing liver and improving vision, tonifying kidney and securing essence, enriching blood and beautifying, and the like. It also has therapeutic effects on chronic gastritis, ulcer, gastroenteritis, arthritis, traumatic injury, dysmenorrhea, and puerperal blood stasis.
The invention discloses a black tiger root extract, a preparation method thereof and application thereof in preparing a medicament with the effects of relaxing muscles and tendons and relieving pain in the prior invention patent CN 202210379417.8. The preparation method of the tiger root extract comprises the following steps: (1) Taking the root of Saxifraga stolonifera, adding an organic solvent for extraction, and concentrating and drying an extracting solution after extraction is finished to obtain an organic solvent extract; (2) Suspending the organic solvent extract in water, extracting with petroleum ether, and extracting with ethyl acetate; concentrating and drying the ethyl acetate extraction part to obtain an ethyl acetate extract; (3) Separating the ethyl acetate extract by preparative HPLC to obtain the extract of the root of Saxifraga nigra. The study of the extract of the black tiger root shows that the extract of the black tiger root has the effects of relaxing muscles and tendons and relieving pain.
However, the current prior art has few research reports on the black tiger essential oil; therefore, the development of the essential oil with the functions of relieving swelling and pain has important application value.
Disclosure of Invention
In order to overcome at least one technical problem in the prior art, the invention firstly provides a preparation method of the black tiger essential oil.
The technical problem to be solved by the invention is realized by the following technical scheme:
the invention firstly provides a preparation method of the black tiger essential oil, which comprises the following steps,
mixing the black tiger root and the black tiger leaf, putting the mixture into a steam distillation device, adding water for steam distillation, and separating oil phase components in a distillation product after the distillation is finished to obtain the black tiger essential oil.
The inventor surprisingly discovers in research that the black tiger essential oil prepared by taking black tiger roots and black tiger leaves as raw materials has better swelling and pain relieving effects; the swelling and pain relieving effect of the black tiger essential oil is better than that of the black tiger essential oil prepared by singly adopting black tiger roots or black tiger leaves as raw materials.
Preferably, the weight ratio of the black tiger root to the black tiger leaf is 2-4.
Most preferably, the weight ratio of the black tiger root to the black tiger leaf is 3.
Preferably, the weight of the water is 10 to 20 times of the total weight of the tiger root and the tiger leaf.
Most preferably, the amount of water is 15 times the total weight of the root and leaf of black tiger.
The invention also provides the black tiger essential oil prepared by the preparation method.
Preferably, the black tiger essential oil also comprises black tiger extract.
Preferably, the weight ratio of the black tiger essential oil to the black tiger extract is 3-5.
Most preferably, the weight ratio of the black tiger essential oil to the black tiger extract is 4.
Preferably, the black tiger extract is prepared by the following method:
taking the residue of the black tiger roots and the black tiger leaves which are subjected to the steam distillation of the claim 1, then adding glycerol, extracting for 1-2 h at the temperature of 130-150 ℃, and performing solid-liquid separation after the extraction is finished to obtain a glycerol extracting solution;
adding an extracting agent into the glycerol extracting solution for extraction to obtain an extracting solution, and concentrating and drying the extracting solution under reduced pressure to obtain the black tiger extract.
The inventor surprisingly discovers in further research that the swelling and pain relieving effects of the black tiger essential oil can be greatly improved by adding the black tiger extract prepared by the method into the black tiger essential oil.
The inventor needs to explain here that the extraction solvent and the extraction temperature are critical in the above preparation method; the inventor shows through a large number of experiments that the swelling and pain relieving effects of the essential oil of the black cutworm can be greatly improved only through the black cutworm extract prepared by extracting glycerol at 130-150 ℃. The swelling and pain relieving effects of the black tiger essential oil cannot be improved or greatly improved by adopting other organic solvents to extract the black tiger extract at other temperatures.
Preferably, the weight of the glycerol is 3-5 times of the total weight of the residue of the tiger's root and the tiger's leaf.
Most preferably, the amount of glycerol is 4 times the total weight of the residue of black tiger root and black tiger leaf.
Preferably, the extractant is petroleum ether.
Preferably, the volume ratio of the extracting agent to the glycerol extracting solution is 1-3.
Most preferably, the volume ratio of the extractant to the glycerol extract is 1.
Preferably, trimethyldodecylammonium chloride is added to the glycerol during the extraction.
More preferably, the weight ratio of the trimethyldodecylammonium chloride to the glycerol is 1;
most preferably, the weight ratio of trimethyldodecylammonium chloride to glycerol is 1.
The inventor further surprisingly discovers in research that the swelling and pain relieving effects of the black tiger essential oil can be further improved by adding the black tiger extract prepared by extracting with trimethyl dodecyl ammonium chloride in the glycerol extraction process and adding the black tiger extract into the black tiger essential oil.
The invention also provides application of the black tiger essential oil in preparing a product with an analgesic effect or a swelling and pain relieving effect.
Preferably, the product is an application in skin care products, health care products or medicines.
Has the advantages that: the invention provides a black tiger essential oil prepared by a brand new method; researches show that the black tiger essential oil prepared by the method has better effects of relieving swelling and pain; particularly, the black cutworm extract prepared by the method disclosed by the invention is added into the black cutworm essential oil, so that the swelling and pain relieving effects of the black cutworm essential oil can be greatly improved. The black tiger essential oil has better effects of relieving swelling and pain; therefore, the application prospect of the compound as a skin care product, a health care product or a medicine with the functions of relieving swelling and pain is wide.
Detailed Description
The present invention is further explained below with reference to specific examples, which are not intended to limit the present invention in any way.
Example 1 preparation of black tiger essential oil
Mixing the dried black tiger root and the black tiger leaf according to the weight ratio of 3.
Example 2 preparation of black tiger essential oil
Adding the black tiger extract into the black tiger essential oil, and uniformly mixing to obtain the black tiger essential oil; wherein the weight ratio of the black tiger essential oil to the black tiger extract is 4.
The black tiger essential oil is prepared by the following method: mixing dried black tiger roots and black tiger leaves according to a weight ratio of 3;
the black tiger extract is prepared by the following method:
(1) Taking the residue of the tiger's root and the black tiger's leaf after steam distillation, then adding glycerol which is 4 times of the total weight of the residue of the tiger's root and the black tiger's leaf, extracting for 1.5h at 140 ℃, and carrying out solid-liquid separation after the extraction is finished to obtain glycerol extract;
(2) Adding petroleum ether with the same volume as the glycerol extracting solution into the glycerol extracting solution for extraction to obtain an extracting solution, and concentrating and drying the extracting solution under reduced pressure to obtain the black tiger extract.
Example 3 preparation of black tiger essential oil
Adding the black tiger extract into the black tiger essential oil, and uniformly mixing to obtain the black tiger essential oil; wherein the weight ratio of the black tiger essential oil to the black tiger extract is 4.
The black tiger essential oil is prepared by the following method: mixing dried black tiger roots and black tiger leaves according to a weight ratio of 3;
the black tiger extract is prepared by the following method:
(1) Taking the residue of the tiger's root and the black tiger's leaf after steam distillation, then adding glycerol which is 4 times of the total weight of the residue of the tiger's root and the black tiger's leaf, then adding trimethyl dodecyl ammonium chloride, extracting for 1.5h at 140 ℃, and carrying out solid-liquid separation after the extraction is finished to obtain glycerol extract; wherein the weight ratio of the trimethyldodecylammonium chloride to the glycerol is 1;
(2) Adding petroleum ether with the same volume as the glycerol extracting solution into the glycerol extracting solution for extraction to obtain an extracting solution, and concentrating and drying the extracting solution under reduced pressure to obtain the black tiger extract.
Example 3 differs from example 2 in that example 3 also added trimethyldodecylammonium chloride during the extraction with glycerol.
Comparative example 1 preparation of black tiger essential oil
Adding the black tiger extract into the black tiger essential oil, and uniformly mixing to obtain the black tiger essential oil; wherein the weight ratio of the black cutworm essential oil to the black cutworm extract is 4.
The preparation method of the black tiger essential oil is the same as that of the embodiment 2;
the black tiger extract is prepared by the following method:
(1) Collecting the residue of radix Kadsurae Coccineae and folium Kadsurae Coccineae after steam distillation, adding 4 times of water of the total weight of the residue, extracting at 100 deg.C for 1.5 hr, and performing solid-liquid separation to obtain water extractive solution;
(2) Adding petroleum ether with the same volume as the water extract into the water extract for extraction to obtain an extract, and concentrating and drying the extract under reduced pressure to obtain the black cutworm extract.
Comparative example 1 is different from example 2 in that the extraction solvent and extraction temperature are different in the preparation of the kadsura coccinea extract, and comparative example 1 is carried out using water at 100 ℃; while example 2 was an extraction with glycerol at 140 ℃.
Comparative example 2 preparation of black tiger essential oil
Adding the black tiger extract into the black tiger essential oil, and uniformly mixing to obtain the black tiger essential oil; wherein the weight ratio of the black tiger essential oil to the black tiger extract is 4.
The preparation method of the black tiger essential oil is the same as that of the embodiment 2;
the black tiger extract is prepared by the following method:
(1) Taking the residue of the black tiger root and the black tiger leaf after the steam distillation, then adding 70 percent ethanol with the volume fraction of 4 times of the total weight of the residue of the black tiger root and the black tiger leaf, extracting for 1.5h at 78 ℃, and carrying out solid-liquid separation after the extraction is finished to obtain ethanol extract;
(2) Adding petroleum ether with the same volume as the ethanol extracting solution into the ethanol extracting solution for extraction to obtain an extracting solution, and concentrating and drying the extracting solution under reduced pressure to obtain the black tiger extract.
Comparative example 2 is different from example 2 in that the extraction solvent and the extraction temperature are different in the preparation process of the black tiger extract, and comparative example 2 is extracted at 78 ℃ using ethanol with a volume fraction of 70%; while example 2 was an extraction with glycerol at 140 ℃.
Comparative example 3 preparation of black tiger essential oil
Adding the black tiger extract into the black tiger essential oil, and uniformly mixing to obtain the black tiger essential oil; wherein the weight ratio of the black tiger essential oil to the black tiger extract is 4.
The preparation method of the black tiger essential oil is the same as that of the embodiment 2;
the black tiger extract is prepared by the following method:
(1) Collecting the residue of radix Kadsurae Coccineae and folium Kadsurae Coccineae after steam distillation, adding 4 times of methanol at 64 deg.C, extracting for 1.5 hr, and performing solid-liquid separation to obtain methanol extractive solution;
(2) Adding petroleum ether with the same volume as the methanol extracting solution into the methanol extracting solution for extraction to obtain an extracting solution, and concentrating and drying the extracting solution under reduced pressure to obtain the black cutworm extract.
Comparative example 3 is different from example 2 in that the extraction solvent and the extraction temperature are different in the preparation of the black tiger extract, and comparative example 3 is performed at 64 ℃ using methanol; while example 2 was an extraction with glycerol at 140 ℃.
Comparative example 4 preparation of black tiger essential oil
Adding the black tiger extract into the black tiger essential oil, and uniformly mixing to obtain the black tiger essential oil; wherein the weight ratio of the black tiger essential oil to the black tiger extract is 4.
The black tiger essential oil is prepared by the following method: mixing dry black tiger root and black tiger leaf according to a weight ratio of 3;
the black tiger extract is prepared by the following method:
(1) Taking the residue of the tiger's root and the black tiger's leaf after steam distillation, then adding glycerol which is 4 times of the total weight of the residue of the tiger's root and the black tiger's leaf, extracting for 1.5h at 100 ℃, and carrying out solid-liquid separation after the extraction is finished to obtain glycerol extract;
(2) Adding petroleum ether with the same volume as the glycerol extracting solution into the glycerol extracting solution for extraction to obtain an extracting solution, and concentrating and drying the extracting solution under reduced pressure to obtain the black tiger extract.
Comparative example 4 is different from example 2 in that the extraction temperature during the preparation of the black tiger extract is different, and comparative example 4 is performed at 100 ℃ using glycerol; while example 2 was an extraction with glycerol at 140 ℃.
Examples of the experiments
A sample to be tested: the black cutworm essential oil prepared in the examples 1 to 3 and the comparative examples 1 to 4 is diluted by adding the black cutworm essential oil into olive oil according to the addition amount of 2% by mass, and is used for testing the swelling and pain relieving effects of the black cutworm essential oil.
Pain relief experiments:
taking a KM mouse, putting the KM mouse on a hot plate at 55 ℃, and observing the time (namely pain threshold) required by the mouse to lick feet; mice with 15s + -1 s time for licking were selected as subjects. The experiment is divided into a control group and an experimental group, and each group comprises 20 experiments; smearing the to-be-detected samples on the soles and the rear legs of the mice of the experimental group every morning, noon and evening; the control group was not treated at all; after three consecutive days of application, the mice were again placed on a hot plate at 55 ℃ to test the time required for the mice to lick their feet (i.e., the pain threshold). The experimental results are shown in table 1; wherein a longer time for the mouse to lick the foot (i.e., the pain threshold) indicates a better analgesic effect.
TABLE 1 test of analgesic effect of the essential oil of black tiger of the present invention
As can be seen from the experimental data in Table 1, the pain threshold of the black tiger essential oil prepared in example 1 is obviously higher than that of the control group; this indicates that: the black tiger essential oil prepared from the raw materials of black tiger root and black tiger leaf has the effect of relieving pain.
As can be seen from the experimental data in Table 1, the pain threshold of the black tiger essential oil prepared in example 2 is greatly higher than that of the black tiger essential oil prepared in example 1; this indicates that: the black tiger extract prepared by the method disclosed by the invention is added into the black tiger essential oil, so that the pain relieving effect of the black tiger essential oil can be greatly improved.
As can be seen from the experimental data in Table 1, the pain threshold of the essential oil of black tiger prepared in comparative examples 1-4 is not higher or is greatly higher than that of the essential oil of black tiger prepared in example 1; this indicates that: in the preparation process of the black tiger extract, the extraction solvent and the extraction temperature are very critical; the pain relieving effect of the black tiger essential oil can be greatly improved only by the black tiger extract prepared by extracting glycerol at 130-150 ℃. The extract of black tiger extracted by other organic solvents at other temperatures cannot improve or greatly improve the pain relieving effect of the black tiger essential oil.
As can be seen from the experimental data in Table 1, the pain threshold of the black cutworm essential oil prepared in example 3 is further greatly higher than that of the black cutworm essential oil prepared in example 2, and is far higher than that of the black cutworm essential oil prepared in a control group and example 1; this indicates that: the black tiger extract prepared by extracting trimethyl dodecyl ammonium chloride is added in the glycerol extraction process, and is added into the black tiger essential oil, so that the pain relieving effect of the black tiger essential oil can be further improved.
Detumescence experiment
Taking KM mice, and dividing into 7 experimental groups and 1 control group, wherein each group comprises 10 mice; measuring hind limb toe volumes of each group of mice by using a toe volume measuring instrument; then 0.1mL of fresh egg white is injected subcutaneously on the right hind paw of each group of mice to cause swelling; then smearing the sample to be tested on the toes of the mouse; testing the volume of the hind limb and toe of each group of mice 1h after smearing the sample; the degree of toe swelling was calculated. Swelling degree = swollen hind toe volume-swollen forefoot volume; the experimental results are shown in table 2, and the smaller the swelling degree is, the better the swelling reducing effect of the sample to be tested is.
Table 2. Swelling reducing effect test of the black tiger essential oil
As can be seen from the experimental data in Table 2, the swelling degree of the black tiger essential oil prepared in example 1 is obviously lower than that of the control group; this indicates that: the kadsura coccinea essential oil prepared from kadsura coccinea root and kadsura coccinea leaf has good detumescence effect.
As can be seen from the experimental data in table 2, the swelling degree of the black tiger essential oil prepared in example 2 is much lower than that of the black tiger essential oil prepared in example 1; this indicates that: the black tiger extract prepared by the method disclosed by the invention is added into the black tiger essential oil, so that the pain relieving effect of the black tiger essential oil can be greatly improved.
As can be seen from the experimental data in Table 2, the swelling degree of the black tiger essential oil prepared in comparative examples 1-4 is not lower or greatly lower than that of the black tiger essential oil prepared in example 1; this indicates that: in the preparation process of the black tiger extract, the extraction solvent and the extraction temperature are very critical; the swelling reducing effect of the black tiger essential oil can be greatly improved only by the black tiger extract prepared by extracting glycerol at 130-150 ℃. The swelling reducing effect of the black tiger essential oil cannot be improved or greatly improved by adopting other organic solvents to extract the black tiger extract at other temperatures.
As can be seen from the experimental data in table 2, the swelling degree of the black tiger essential oil prepared in example 3 is further greatly lower than that of the black tiger essential oil prepared in example 2, and is far lower than that of the control group and the black tiger essential oil prepared in example 1; this indicates that: the black tiger extract prepared by extracting trimethyl dodecyl ammonium chloride is added in the glycerol extraction process, and is added into the black tiger essential oil, so that the swelling reducing effect of the black tiger essential oil can be further improved.
Claims (10)
1. A preparation method of black tiger essential oil is characterized by comprising the following steps of,
mixing the black tiger root and the black tiger leaf, putting the mixture into a steam distillation device, adding water for steam distillation, and separating oil phase components in a distillation product after the distillation is finished to obtain the black tiger essential oil.
2. The method for preparing black tiger essential oil according to claim 1, wherein the weight ratio of black tiger root to black tiger leaf is 2-4;
most preferably, the weight ratio of the black tiger root to the black tiger leaf is 3.
3. The method for preparing black tiger essential oil of claim 1, wherein the weight amount of water is 10 to 20 times of the total weight of black tiger roots and black tiger leaves;
most preferably, the amount of water is 15 times the total weight of the root and leaf of Kadsura coccinea.
4. A black tiger essential oil prepared by the preparation method of any one of claims 1 to 3.
5. The black tiger essential oil of claim 4, further comprising black tiger extract.
6. The essential oil of black tiger according to claim 5, wherein the weight ratio of the essential oil of black tiger to the extract of black tiger is 3 to 5;
most preferably, the weight ratio of the black tiger essential oil to the black tiger extract is 4.
7. The essential oil of black tiger according to claim 5, wherein the extract of black tiger is prepared by the following steps:
taking the residue of the black tiger roots and the black tiger leaves which are subjected to the steam distillation of the claim 1, then adding glycerol, extracting for 1-2 h at the temperature of 130-150 ℃, and performing solid-liquid separation after the extraction is finished to obtain a glycerol extracting solution;
adding an extracting agent into the glycerol extracting solution for extraction to obtain an extracting solution, and concentrating and drying the extracting solution under reduced pressure to obtain the black tiger extract.
8. The essential oil of black tiger according to claim 7, wherein the amount of glycerol is 3 to 5 times of the total weight of the residue of black tiger root and black tiger leaf.
9. Use of the essential oil of black tiger according to any one of claims 4 to 8 for the preparation of a product having analgesic or repercussive and analgesic effects.
10. Use according to claim 9, wherein the product is a skin care product, a health product or a pharmaceutical product.
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| CN114601875A (en) * | 2022-04-12 | 2022-06-10 | 湖南环境生物职业技术学院 | A radix Saxifragae extract, its preparation method and application in preparing medicine with effects of relaxing muscles and tendons and relieving pain |
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