CN115006314B - Kava pepper extract and preparation method and application thereof - Google Patents
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Abstract
The invention relates to a kava pepper extract and a preparation method and application thereof, belonging to the technical field of medicine extraction. The preparation method of the kava pepper extract provided by the invention comprises the following steps: (1) Pulverizing kava pepper raw material, treating at high temperature and high pressure, and drying to obtain kava pepper powder; (2) Extracting and decoloring the obtained kava pepper powder with alcohol, and separating to obtain a solid; (3) Extracting the obtained solid with ethanol twice, filtering, collecting the liquid, and concentrating. The preparation method is simple, and the prepared kava pepper extract has high activity, good purity, no impurity, good safety and excellent anti-allergy and soothing effects, and can be widely applied to the field of cosmetics.
Description
Technical Field
The invention belongs to the technical field of medicine extraction, and particularly relates to a kava extract and a preparation method and application thereof.
Background
Sensitive skin is a special skin type, and refers to skin which is easy to have objective symptoms such as erythema, pimple, telangiectasis and the like when being stimulated by the outside, and subjective symptoms such as itching, stinging, burning, tightness and the like are accompanied. Investigation according to the skin type of english-japanese 2020 shows that the proportion of sensitive muscles in consumers is self-judged to be as high as 41%. However, they often feel stinging when they use cosmetics that claim no irritation, especially facial masks, because conventional anti-inflammatory substances do not relieve the external irritation. This is also one reason for the photophobia of the hands and feet of consumers of sensitive skin when selecting cosmetics, who desire truly sensitive muscle suitable products that possess immediate comfort and restoration of the skin barrier effect.
The active substances with the anti-allergic and antipruritic restoration effects are developed from natural plants, and the natural plant anti-allergic active ingredients have small toxic and side effects, generally do not generate drug dependence, are added into daily skin care products, and are easily accepted and approved by consumers. The traditional antiallergic plants include flos Matricariae Chamomillae, herba Portulacae, and Aloe. Kava is the leaf/root/stem of kava, a perennial upright shrub medicinal plant of the family Piperaceae, native to the islands of the south Pacific ocean. The extract is rich in kavalactones, mainly kavain active substances, can bidirectionally regulate neurotransmitters, has various effects of resisting anxiety and depression, sedating and hypnotizing, local anesthesia, anticonvulsant and the like, and has no drug dependence. There are reports of its application in cosmetics or skin care products for soothing and resisting sensitization.
However, in the prior art, the preparation method of the kava pepper extract is not sound, and the problems of low efficiency, low activity and low purity of the extract, poor activity and reduced safety of the extract exist. Therefore, the kava pepper extract with high activity and good purity and the preparation method thereof are the technical problems to be solved at present.
Disclosure of Invention
The invention aims to provide a kava extract, a preparation method and application thereof, aiming at the problems existing in the existing products.
The invention is realized by the following technical scheme:
the invention provides a preparation method of a kava pepper extract, which comprises the following steps:
(1) Pulverizing kava pepper raw material, treating at high temperature and high pressure, and drying to obtain kava pepper powder;
(2) Extracting and decoloring the obtained kava pepper powder with alcohol, and separating to obtain a solid;
(3) Extracting the obtained solid with ethanol twice, filtering, collecting the liquid, and concentrating.
In the preparation method, the kava raw material is decolorized and desalted by the first alcohol extraction, the active ingredients in the kava are further effectively extracted by the second alcohol extraction, and finally the kava extract with high activity and good purity is obtained by separation and concentration. The preparation method is simple, and the prepared kava pepper extract has high activity, good purity, no impurity and good safety.
As a preferred embodiment of the method for preparing a kava extract of the present invention, in the step (1), the kava raw material comprises kava leaves, kava roots or kava stems.
As a preferred embodiment of the preparation method of kava pepper extract, in the step (1), the temperature of the high-temperature high-pressure treatment is 110-120 ℃, the pressure is 0.11-0.25 MPa, and the time is 30-50 min.
Specifically, in the step (1), the crushing is to crush naturally dried kava leaves, kava roots and kava stems by a crusher, pass through a 50-mesh screen to obtain coarse crushed kava leaf/root/stem powder, and then treat the coarse crushed kava leaf/root/stem powder at high temperature and high pressure to obtain crushed kava powder.
In the preferred embodiment of the preparation method of kava pepper extract of the present invention, in the step (1), the drying temperature is 60-75 ℃ and the drying time is 1-2 h.
In the step (2), the ethanol extracted solvent is ethanol with the mass fraction of 40% -60%, the temperature is 45-55 ℃ and the times are 1-3 times; the mass volume ratio of the kava powder to the solvent is 1 (5-10) (g/mL).
Preferably, in the step (2), the number of times of the alcohol extraction is 2; the ratio of the kava powder to the solvent is 1:7 (g/mL); specifically, the extracting solution obtained by each alcohol extraction is filtered by a 300-mesh filter screen to obtain solid.
As a preferred embodiment of the method for preparing kava extract of the present invention, in the step (3), the solvent for the secondary alcohol extraction is butanediol; preferably, the ratio of the solids to the butanediol is 1g:10ml.
In the step (3), the filtered liquid is centrifuged, the centrifugation is a high-speed tube type centrifugation, the rotation speed of the centrifugation is 8000 r/min-10000 r/min, and the feeding speed is 30L/h-80L/h.
Specifically, in the step (3), the obtained solid is addedExtracting with butanediol, and stirring to obtain a mixture; coarse filtering the mixture with 200 mesh filter cloth to obtain filtrate; finely filtering the obtained filtrate by a filter plate until the filtrate is clear, so as to obtain clear filtrate; subjecting the clarified filtrate to high-speed tube centrifugation (rotation speed 10000r/min, feeding speed 30L/h-40L/h), diluting the supernatant with deionized water, (supernatant: deionized water=1:2); centrifuging the diluted liquid at high speed (rotational speed 8000r/min and feeding speed 60-80L/h), collecting supernatant, concentrating at 80deg.C until the density of the material is 1.020-1.130g/cm 3 And (5) obtaining the kava pepper extract.
Still another object of the present invention is to provide kava extract prepared by the above preparation method.
The kava extract is rich in kavalactone, and 6 main active ingredients of kavalactone comprise methysticin, kavain, dihydro methysticin, dihydro kavain, demethoxy kavain and methoxy kavain in sequence, wherein kavain, dihydro kavain and dihydro kavain can bidirectionally regulate neurotransmitter, relieve pressure, and have obvious effect of relaxing muscle. The kava extract acts on nerve endings to block the transmission of information from neurons by occupying GABAA receptors and inhibiting prostaglandin PGE2, and inhibit the transmission of sensitivity, thereby achieving immediate relief and sedation. The kava pepper extract provided by the invention has the advantages of high activity, good purity and good safety, and has the effects of immediately calming, resisting inflammation, removing acnes, relieving and aiding sleep. The kava pepper extract provided by the invention is clear and transparent, has a yellow to brown yellow color, has characteristic smell, has a pH value (25 ℃) of 5.0-7.0 and a density (25 ℃) of 1.020g/cm 3 -1.130g/cm 3 。
It is still another object of the present invention to provide the above kava extract and its preparation method for use in cosmetics.
Another object of the present invention is to provide a composition containing kava extract, comprising, in parts by weight: 1-5 parts of kava extract and 30-50 parts of butanediol.
The composition containing the kava pepper extract provided by the invention is free from adding preservative, adopts butanediol as a moisturizing component, is milder, has a good antibacterial effect, can have the efficacy of relieving and resisting allergy without adding traditional preservative, and has higher safety when being applied to cosmetics.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method is simple, the butanediol is adopted for secondary alcohol extraction, the butanediol is colorless liquid, has a certain antibacterial effect, has an inhibition effect on mixed bacteria of filter residues, is high in safety, has no stimulation, can well protect the activity of the kava extract, and is high in activity and good in purity. (2) The composition containing kava pepper extract has the advantages that no preservative exists, the moisturizing component butanediol is mild, the butanediol with the weight portions has a good antibacterial effect, no additional preservative is needed to be added in cosmetics, the irritation to sensitive muscles is avoided, and the safety of the product is higher.
Drawings
FIG. 1 is a data statistical graph of PGE2 inhibition by kava extracts of examples 1-2 and comparative examples 1-4 of the present invention.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples and the accompanying drawings. It will be appreciated by persons skilled in the art that the specific embodiments described herein are for purposes of illustration only and are not intended to be limiting.
The test methods used in the examples are conventional methods unless otherwise specified; the materials, reagents and the like used, unless otherwise specified, are all commercially available.
Example 1
A preparation method of kava pepper extract comprises the following steps:
(1) Pulverizing naturally air-dried Piper methysticum leaves, piper methysticum roots and Piper methysticum stems with pulverizer, sieving with 50 mesh sieve to obtain coarse pulverized Piper methysticum leaves/roots/stems powder;
treating the coarsely crushed raw materials at 0.25MPa and 120 ℃ for 50min; drying in a drying oven at 75 ℃ for 2 hours;
(2) Taking the obtained kava pepper powder, extracting with 60% ethanol with a feed-liquid ratio of 1:7 (g/mL) at 45deg.C for decolorizing for 2 times and 45 min/time; filtering the extract with 300 mesh sieve to obtain solid;
(3) Adding the solid obtained in the step (2) into butanediol for extraction, wherein the ratio of the solid to the butanediol is 1 g/10 ml, and stirring to obtain a mixture; coarse filtering the mixture with 200 mesh filter cloth to obtain filtrate; finely filtering the obtained filtrate by a filter plate until the filtrate is clear, so as to obtain clear filtrate; subjecting the clarified filtrate to high-speed tube centrifugation (rotation speed 10000r/min, feed rate 40L/h), diluting the supernatant with deionized water, (supernatant: deionized water=1:2); centrifuging the diluted liquid again at high speed (rotational speed 8000r/min and feeding speed 80L/h), collecting supernatant, concentrating, and concentrating at 80deg.C until the density of the material is 1.130g/cm 3 Obtaining the kava pepper extract.
Example 2
A preparation method of kava pepper extract comprises the following steps:
(1) Pulverizing naturally air-dried Piper methysticum leaves, piper methysticum roots and Piper methysticum stems with pulverizer, sieving with 50 mesh sieve to obtain coarse pulverized Piper methysticum leaves/roots/stems powder;
treating the coarsely crushed raw materials at a temperature of 0.11MPa and 110 ℃ for 30min; drying in a drying oven at 60 ℃ for 1h;
(2) Taking the obtained kava pepper powder, extracting with 40% ethanol with a feed-liquid ratio of 1:7 (w/v) at 45deg.C for decolorizing for 2 times and 45 min/time; filtering the extract with 300 mesh sieve to obtain solid;
(3) Adding the solid obtained in the step (2) into butanediol for extraction, and stirring to obtain a mixture; coarse filtering the mixture with 200 mesh filter cloth to obtain filtrate; finely filtering the obtained filtrate by a filter plate until the filtrate is clear, so as to obtain clear filtrate; subjecting the clarified filtrate to high-speed tube centrifugation (rotation speed 10000r/min, feed rate)30L/h), the supernatant after centrifugation was diluted with deionized water (supernatant: deionized water = 1: 2) The method comprises the steps of carrying out a first treatment on the surface of the Centrifuging the diluted liquid again at high speed (rotational speed 8000r/min and feeding speed 60L/h), collecting supernatant, concentrating, and concentrating at 80deg.C until the density of the material is 1.020g/cm 3 Obtaining the kava pepper extract.
Example 3
A composition containing kava extract comprises, by mass, 2.8% of the kava extract of example 1, 36% of butylene glycol, and 61.2% of water.
Example 4
A composition containing kava extract comprises, by mass, 5% of kava extract of example 1, 50% of butylene glycol, and 45% of water.
Example 5
A composition containing kava extract comprises, by mass, 1% of kava extract of example 1, 30% of butylene glycol, and 69% of water.
Comparative example 1
A method for preparing kava pepper extract is different from example 1 in that step (2) is not included, and the other steps are the same as in example 1.
Comparative example 2
A method for preparing kava extract is different from example 1 in that the solvent of the secondary alcohol extraction in the step (3) is replaced by an equal amount of water from butanediol, and the method is the same as in example 1.
Comparative example 3
A method for preparing kava extract is different from example 1 in that the solvent of the secondary alcohol extraction in the step (3) is replaced by the same amount of ethanol from butanediol, and the other steps are the same as in example 1.
Comparative example 4
The kava extract was prepared using the method for preparing kava extract described in example 1 of chinese patent specification publication No. CN101239104 a.
Comparative example 5
A composition containing kava extract comprises, by mass, 2.8% of the kava extract of example 1 and 97.2% of water.
Comparative example 6
A composition containing kava extract comprises, by mass, 2.8% of the kava extract of example 1, 29% of butylene glycol, and 68.2% of water.
Comparative example 7
A composition containing kava extract comprises, by mass, 0.5% of kava extract of example 1, 36% of butylene glycol, and 63.5% of water.
Test example 1
The kava extracts prepared in examples 1-2 and comparative examples 1-4 were used for anti-inflammatory test, i.e., PGE2 inhibition. The action mechanism of the kava extract is as follows: acting on nerve endings, blocking neuronal transmission information by kavain occupying GABAA receptors and inhibiting PGE2 (prostaglandin PGE2 is a known mediator of inflammation, which can cause pain), potentially inhibiting transmission of sensitivity, thus achieving immediate relief of sedation.
The test method comprises the following steps: 70 experimental rats were randomly divided into 7 groups of 10 rats, and each rat was intradermally injected with 0.1mL of Freund's complete adjuvant to the right foot plantar, thereby inducing adjuvant arthritis in the rats. The kava pepper extract with the equivalent mass concentration of 1% prepared in examples 1-2 and comparative examples 1-4 and 1% normal saline (used as a blank control group) were taken, the fasted injection was performed on 7 groups of rats, after 24 consecutive days, the paw tissues of the rats were sheared, the rats were immersed in 5mL of normal saline for 2 hours, 3000g of the immersed solution was centrifuged for 15 minutes to suck the supernatant, and the PGE2 content was measured by EIA method, and the PGE2 content of each group was shown in table 1.
TABLE 1 PGE2 content of the extracts of examples 1-2, comparative examples 1-4 and blank
| Numbering device | PGE2 content (ng/g) |
| Example 1 | 1.82 |
| Example 2 | 1.69 |
| Comparative example 1 | 4.67 |
| Comparative example 2 | 4.12 |
| Comparative example 3 | 3.83 |
| Comparative example 4 | 3.45 |
| Blank control group | 5.01 |
As can be seen from fig. 1 and table 1, the kava extract prepared by the preparation method of examples 1-2 of the present invention has high activity, obvious inhibition effect on PGE2, and remarkable anti-inflammatory effect. In the preparation method of the comparative example 1, the ethanol extraction and decoloration step is not included, and the prepared kava extract has more impurities and poor activity, and the anti-inflammatory effect is only slightly better than that of a blank control group. In the preparation method of comparative example 2, water is adopted for secondary alcohol extraction, active ingredients in kava cannot be effectively extracted, and the prepared kava extract has low purity, poor activity and poor anti-inflammatory effect. In the preparation method of the comparative example 3, the activity of the prepared kava extract is superior to that of the comparative example 2 which adopts water as a secondary alcohol extraction solvent by adopting ethanol, but the anti-inflammatory effect is obviously lower than that of the kava extract of the example 1 which adopts butanediol as a solvent, which shows that the invention adopts butanediol as a solvent, so that the prepared kava extract has high purity, good activity and excellent anti-inflammatory effect. The prior art of comparative example 4 produced kava extract with lower anti-inflammatory activity than that of example 1 of the present invention. Compared with the prior art, the preparation method of the kava pepper extract is simple, and the prepared kava pepper extract has obvious anti-inflammatory effect.
Test example 2
The kava pepper extract prepared in comparative examples 1-4 was taken and combined with butylene glycol and water, respectively, to form a composition comprising, in mass percent: 2.8% of kava extract, 36% of butanediol and 61.2% of water. The compositions containing kava extracts obtained in comparative examples 1 to 4 were designated as test comparative examples 1 to 4, and the obtained compositions containing kava extracts of comparative examples 1 to 4, examples 3 to 5 and comparative examples 5 to 7 were used for anti-acne and anti-inflammatory tests.
100 female volunteers with inflamed and red swelling on the face, aged 30-50 years, were selected and randomly divided into 10 groups of 10. Volunteers daily wipe the compositions containing kava extract of comparative examples 1-4, examples 3-5, and comparative examples 5-7 1 time, once a week, for 4 weeks continuously without changing or using other similar products during the test. The volunteers were tested with MPA580 skin elasticity tester and VISIA full face analyzer, respectively, and the volume and area of the vaccinia on the faces of the volunteers and the detumescence of the faces of the volunteers were observed. After the corresponding samples were applied, a skin lactic acid stimulation test was performed, and the samples were scored according to a score 4 method (0 for no stinging, 1 for mild stinging, 2 for moderate stinging, and 3 for heavy stinging), and whether the samples had a soothing anti-allergic effect was confirmed by detecting the lactic acid stimulation level of the volunteers.
TABLE 2 anti-inflammatory and soothing Effect of compositions of comparative examples 1-4, examples 3-5, comparative examples 5-7
| Composition numbering | Skin anti-inflammatory effect | Change in vaccinia volume reduction | Skin lactic acid stinging degree |
| Example 3 | 89％ | 82％ | 0.7 |
| Example 4 | 85％ | 80％ | 0.8 |
| Example 5 | 81％ | 78％ | 0.85 |
| Test comparative example 1 | 23％ | 22％ | 3.4 |
| Test comparative example 2 | 30％ | 32％ | 2.0 |
| Test comparative example 3 | 42％ | 39％ | 2.4 |
| Test comparative example 4 | 56％ | 53％ | 1.9 |
| Comparative example 5 | 70％ | 60％ | 1.1 |
| Comparative example 6 | 71％ | 65％ | 0.9 |
| Comparative example 7 | 60％ | 55％ | 1.3 |
As can be seen from Table 2, the compositions containing kava extract provided in examples 3-5 of the present invention have remarkable anti-acne and anti-inflammatory effects, can effectively modify the acne inflammation and inflammation problems of volunteers within 4 weeks, and have a certain anti-allergy relieving effect. The compositions of test comparative examples 1 to 4 use kava pepper extract prepared in comparative examples 1 to 4 as an active ingredient, and the prepared extract has many impurities and poor activity, so that the composition has reduced anti-inflammatory effect and poor acne removing effect and can not effectively relieve skin. The composition of comparative example 5, to which the moisturizing ingredient butylene glycol was not added, was not effective in relieving weak skin irritation of kava extract during anti-inflammatory process, and thus the anti-inflammatory effect of the composition was inferior to that of example 3. In the composition of comparative example 6, the addition amount of butanediol was small, the antibacterial effect was weakened, and the skin anti-inflammatory effect was inferior to the compositions of examples 3 to 5. In comparative example 7, the addition amount of kava extract was too small and the anti-inflammatory effect was poor. The composition containing the kava extract has the advantages of low cost and good anti-inflammatory repairing effect. Therefore, the composition containing kava extract has excellent anti-inflammatory repairing and soothing effects under specific component proportions.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (7)
1. A preparation method of kava pepper extract is characterized by comprising the following steps:
(1) Pulverizing kava pepper raw material, treating at high temperature and high pressure, and drying to obtain kava pepper powder; the temperature of the high-temperature high-pressure treatment is 110-120 ℃, the pressure is 0.11-0.25 MPa, and the time is 30-50 min;
(2) Extracting and decoloring the obtained kava pepper powder with alcohol, and separating to obtain a solid; the ethanol extraction solvent is ethanol with the mass fraction of 40% -60%, the temperature is 45-55 ℃, and the times are 1-3 times; the mass volume ratio of the kava powder to the solvent is 1 (5-10);
(3) Extracting the obtained solid with ethanol twice, filtering, and concentrating the liquid to obtain the final product; the solvent for the secondary alcohol extraction is butanediol.
2. The method of preparing a kava extract according to claim 1, wherein in the step (1), the kava raw material comprises kava leaves, kava roots or kava stems.
3. The method for preparing kava extract according to claim 1, wherein in the step (1), the drying temperature is 60 ℃ to 75 ℃ and the drying time is 1h to 2h.
4. The method for preparing kava extract according to claim 1, wherein in the step (3), the filtered liquid is centrifuged, the centrifugation is a high-speed tube type centrifugation, the rotational speed of the centrifugation is 8000r/min to 10000r/min, and the feeding speed is 30L/h to 80L/h.
5. A kava extract, characterized in that it is produced by the production method according to any one of claims 1 to 4.
6. Use of kava extract according to claim 5 for the preparation of cosmetics.
7. A composition comprising kava extract, which comprises 1-5 parts of kava extract according to claim 5 and 30-50 parts of butylene glycol in parts by weight.
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| CN116350566A (en) * | 2023-02-17 | 2023-06-30 | 广州市妆泽生物科技有限公司 | Preparation method of skin nourishing and allergy relieving combined by multiple plant extracts |
| CN117598950B (en) * | 2023-12-01 | 2024-05-14 | 广州星汇生物科技有限公司 | Extract containing kava root, preparation method and application thereof in cosmetic with soothing and repairing effects |
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