Preparation method and application of kava extract with soothing and anti-allergy capabilities

Abstract

The invention discloses a preparation method and application of a kava extract with soothing and anti-allergy capacities, and the preparation method comprises the following steps: putting kava pepper root powder into an extraction tank, and carrying out subcritical extraction on the kava pepper root powder by using an organic solvent as an extraction solvent to obtain an extraction liquid; sequentially carrying out reduced pressure evaporation and filtration on the extract to obtain a crude extract; adding the crude extract into a feeding bottle of molecular distillation equipment, and carrying out molecular distillation treatment to obtain yellow oily liquid; and finally, drying the yellow oily liquid to obtain the kavalactone extract. The method has the characteristics of high extraction efficiency, no solvent residue and low preparation cost.

Description

Technical Field

[0001] The invention relates to a method for preparing a kava extract, in particular to a method for preparing a kava extract with soothing and anti-allergy capabilities and application thereof. Background Art

[0002] Kava, commonly known as kava, is a perennial shrub of the Piperaceae family that grows wild in the South Pacific islands of Vanuatu, Fiji, Tonga, etc. It has attracted more and more attention in the cosmetics field in recent years due to its significant immediate soothing and anti-allergic abilities. The active ingredients of kava are mainly concentrated in the roots, most of which are a-pyrone derivatives, called kavalactones, which account for about 3% to 20% of the kava roots. The kavalactones mainly include the following 6 ingredients: anemone, dihydroanemone, capsaicin, dihydrocapsaicin, demethoxycapsaicin and methoxycapsaicin.

[0003] The existing preparation processes for Kava extract are mainly divided into three types: water extraction, organic solvent extraction and supercritical CO2 fluid extraction. Among them, the water extraction method has the advantages of being green and pollution-free, but because kava lactone is insoluble in water, its extraction efficiency is relatively low. The organic solvent extraction method has the problems of low extraction purity, large loss of active substances, and difficulty in removing residual solvents in the product. Compared with the first two methods, the supercritical CO2 fluid extraction method has the characteristics of high extraction efficiency and environmental friendliness, but it has the disadvantages of expensive extraction equipment, high energy consumption and high operating costs.

[0004] Therefore, a method for extracting kavalactones with high extraction efficiency, no solvent residue and low preparation cost is needed. Summary of the invention

[0005] The purpose of the present invention is to provide a preparation method and application of kava extract with soothing and anti-allergic ability. The kava extract has the characteristics of high extraction efficiency, no solvent residue and low preparation cost.

[0006] The technical solution of the present invention is a method for preparing a kava extract having soothing and anti-allergic properties, comprising the following steps:

[0007] ① Put the kava root powder into an extraction tank, and perform subcritical extraction on the kava root powder using an organic solvent as an extraction solvent to obtain an extract A;

[0008] ② The extract A is evaporated under reduced pressure and filtered in turn to obtain a crude extract B;

[0009] ③ Add the crude extract B to the feed bottle of the molecular distillation equipment, and set the feed bottle temperature to 50-70°C, the pressure to <200Pa, and the distillation temperature to 100-140°C;

[0010] When the temperature and pressure reach the set value, start feeding, and set the scraping speed to 40-70r / min and the feed flow rate to 20-50mL / min;

[0011] After the feeding is completed, the mixture is allowed to stand for 1 to 2 hours under vacuum and the fraction bottles are reassembled to obtain a yellow oily liquid C;

[0012] ④ Dry the yellow oily liquid C to obtain the kavalactone extract.

[0013] In the aforementioned method for preparing a kava extract with soothing and anti-allergic capabilities, in step ①, the kava root is first dried and crushed, and then sieved through a 50-120 mesh sieve to obtain the kava root powder.

[0014] In the aforementioned method for preparing a kava extract with soothing and anti-allergic capabilities, the drying temperature of the kava root in step ① is 45-70°C.

[0015] In the aforementioned method for preparing a kava extract with soothing and anti-allergic ability, the organic solvent in step ① is any one of butane, propane, isobutane and dimethyl ether, and the mass ratio of the kava root powder and the organic solvent during extraction is 1:3 to 4.

[0016] In the aforementioned method for preparing a kava extract with soothing and anti-allergic ability, the subcritical extraction method of the kava root powder in step ① is specifically as follows: the kava root powder and the organic solvent are loaded into an extraction tank, and the organic solvent is used to extract the kava root powder at an extraction temperature of 55 to 65° C. and an extraction pressure of 1 to 3 MPa to obtain an extract A.

[0017] In the aforementioned method for preparing a kava extract with soothing and anti-allergic ability, the reduced pressure evaporation method of the A extract in step ② is specifically as follows: the A extract is sent to a separation tank for reduced pressure evaporation, the reduced pressure evaporation time is 15 to 30 minutes, and after the evaporation is completed, the liquid remaining at the bottom of the separation tank is discharged to obtain a pre-filtered concentrated liquid.

[0018] In the aforementioned method for preparing a kava extract with soothing and anti-allergic capabilities, the filtering method in step ② is centrifugal separation, and the centrifugal speed during centrifugal separation is greater than 2000g.

[0019] The present application also provides the application of the kava extract prepared by the aforementioned method for preparing the kava extract with soothing and anti-allergic ability in the soothing effect of cosmetics.

[0020] Compared with the prior art, the present invention has the following characteristics:

[0021] (1) The present invention uses kava root powder for subcritical extraction, which can effectively reduce its energy consumption and extraction cost compared with the existing extraction method, and reduce the oxidation and damage of the active ingredients in kava lactones, thereby improving the extraction efficiency and purity of kava lactones;

[0022] In view of the characteristics of the components of the liquid-liquid system of the A extract having little difference in boiling points, high viscosity and heat sensitivity after subcritical extraction, the present application can achieve the effect of removing impurities from the B crude extract at a low temperature and in a short time by combining the subcritical extraction process and the molecular distillation process, that is, reducing the damage to the active ingredients in the kavalactones on the basis of completely removing small molecule impurities;

[0023] (2) By evaporating and filtering the A extract after subcritical extraction under reduced pressure, the organic solvent in the A extract can be removed, and the A extract can be initially impurity-removed, thereby reducing the difficulty of impurity removal during subsequent molecular distillation and improving the impurity removal effect of the molecular distillation process on the B crude extract;

[0024] (3) By using butane, propane, isobutane or dimethyl ether as a subcritical fluid, the kava root can be extracted at a relatively low temperature and pressure, thereby further reducing the damage to the active ingredients in the kava lactones, and thereby reducing the difficulty and cost of the extraction process; by limiting the various parameters of the crude extract B during the subcritical extraction and molecular distillation process, the extraction and impurity removal effects of the kava lactones can be further improved; and under the above-mentioned coordination, the kava lactone extract prepared by the present invention can reach a purity of UV>99% and HPLC>80%;

[0025] Therefore, the present invention has the characteristics of high extraction efficiency, no solvent residue and low preparation cost. DETAILED DESCRIPTION

[0026] The present invention will be further described below in conjunction with the embodiments, but they are not intended to limit the present invention.

[0027] Example 1. A method for preparing a kava extract having soothing and anti-allergic properties, comprising the following steps:

[0028] ① Put the kava root powder into an extraction tank, and perform subcritical extraction on the kava root powder using an organic solvent as an extraction solvent to obtain an extract A;

[0029] ② The extract A is evaporated under reduced pressure and filtered in turn to obtain a crude extract B;

[0030] ③ Add the crude extract B to the feed bottle of the molecular distillation equipment, and set the feed bottle temperature to 50-70°C, the pressure to <200Pa, and the distillation temperature to 100-140°C;

[0031] When the temperature and pressure reach the set value, start feeding, and set the scraping speed to 40-70r / min and the feed flow rate to 20-50mL / min;

[0032] After the feeding is completed, the mixture is allowed to stand for 1 to 2 hours under vacuum and the fraction bottles are reassembled to obtain a yellow oily liquid C;

[0033] ④ Dry the yellow oily liquid C to obtain the kavalactone extract.

[0034] In the step ①, the kava root is first dried and crushed, and then passed through a 50-120 mesh sieve to obtain the kava root powder.

[0035] In the step ①, the drying temperature of the Kava root is 45-70°C.

[0036] The organic solvent in step ① is any one of butane, propane, isobutane and dimethyl ether, and the mass ratio of the kava root powder to the organic solvent during extraction is 1:3-4.

[0037] The subcritical extraction method of the kava root powder in step ① is specifically as follows: the kava root powder is loaded into an extraction tank, and then an organic solvent is injected into the extraction tank by using a pressure difference, so that the organic solvent extracts the kava root powder under an extraction temperature of 55 to 65° C. and an extraction pressure of 1 to 3 MPa, the extraction times are 3 to 5 times, and the extraction time is 30 to 90 minutes, to obtain an extract A.

[0038] The reduced pressure evaporation method of the A extract in step ② is specifically as follows: the A extract is sent to a separation tank for reduced pressure evaporation, the reduced pressure evaporation time is 15 to 30 minutes, the vaporized solvent in the reduced pressure evaporation process is refluxed to the solvent tank through a compressor for recycling, and after the evaporation is completed, the liquid remaining at the bottom of the separation tank is discharged to obtain a pre-filtered concentrated liquid.

[0039] The filtering method in step ② is centrifugal separation, and the centrifugal speed during centrifugal separation is greater than 2000g.

[0040] The kava extract prepared by the preparation method can be used in cosmetics for soothing effect.

[0041] Working principle of the present invention: The present invention combines the subcritical extraction process with the molecular distillation process, and can utilize the characteristics of the subcritical extraction process, which is non-toxic, energy-saving and low in preparation cost, to effectively overcome the defects of the existing extraction process and reduce the oxidation and damage to the active ingredients in the kavalactones. In view of the characteristics of the extract after subcritical extraction, which has similar boiling points, high viscosity and heat sensitivity, the present invention utilizes the molecular distillation process to achieve a high degree of separation of the B crude extract in a short time at a relatively low temperature, thereby achieving stable extraction of the kavalactones and subsequently improving the purity of the kavalactones after extraction.

[0042] The kava extract prepared by this embodiment has kavalactone content>80% HPLC, wherein the content of anthemis nobilis is 8-10%, the content of dihydroanthemis nobilis is 8-9%, the content of capsaicin is 26-35%, the content of dihydrocapsaicin is 19-25%, the content of methoxycapsaicin is 8-10%, and the content of demethoxycapsaicin is 8-11%.

[0043] Example 2. A method for preparing a kava extract having soothing and anti-allergic properties, comprising the following steps:

[0044] ① First, the kava root is dried and crushed, the drying temperature is set to 60°C, and then passed through a 100-mesh sieve to obtain the kava root powder;

[0045] The kava root powder is then loaded into an extraction tank, and an organic solvent is injected into the extraction tank using a pressure difference, so that the organic solvent extracts the kava root powder under an extraction temperature of 60° C. and an extraction pressure of 3 MPa, the number of extractions is 4, the extraction time is 70 min, the organic solvent is butane, and the mass ratio of the kava root powder to the organic solvent during extraction is 1:3, to obtain an extract A;

[0046] ② The A extract is sent to a separation tank for reduced pressure evaporation. The reduced pressure evaporation time is 30 minutes. The vaporized solvent in the reduced pressure evaporation process is refluxed to the solvent tank through the compressor for recycling. After the evaporation is completed, the liquid remaining at the bottom of the separation tank is collected to obtain a pre-filtered concentrated liquid;

[0047] Then, the residue in the concentrate is removed by centrifugation at a speed of 2200 g to obtain a crude extract B in an extract state;

[0048] ③ Add crude extract B into the feed bottle of the molecular distillation equipment, and set the feed bottle temperature to 60°C, the pressure to 180Pa, and the distillation temperature to 130°C;

[0049] When the temperature and pressure reach the set value, start feeding, and set the scraping speed to 50r / min and the feed flow rate to 40mL / min;

[0050] After the feeding is completed, the mixture is allowed to stand for 1.5 h under vacuum and the fraction bottles are reassembled to obtain yellow oily liquid C;

[0051] ④ Dry the yellow oily liquid C to obtain the kava lactone extract in a viscous yellow paste state.

[0052] Compared with Example 1, this example further defines various parameters for the extraction of kavalactones, so that it is possible to further improve the extraction effect of kavalactones and the purity of the kavalactone extract after extraction.

[0053] Experimental Example: In this experimental example, the kava lactone extract prepared in Example 2 is used as sample 1, and sample 2 and sample 3 are set. Compared with Example 2, the preparation process of sample 2 only extracts the kava pepper root powder through the subcritical extraction process of step ① to obtain the kava lactone extract, that is, there is no purification and impurity removal process of steps ②-④; compared with Example 2, the preparation process of sample 3 replaces the molecular distillation process of step ③ with a conventional rotary evaporation impurity removal process, and the remaining processes are the same as Example 2. Then the three groups of samples were tested by high performance liquid chromatography, and the test results are shown in Table 1:

[0054] Table 1 Detection results of kava content in different samples

[0055]

[0056] It can be seen from Table 1 that the purity of sample 1 is significantly improved compared with sample 2 and sample 3, indicating that the combination of subcritical extraction and molecular distillation can effectively improve the extraction effect of kavalactones compared with the other two groups of methods. The purity of sample 3 is better than sample 2, but it is significantly lower than that of sample 1, indicating that the crude extract obtained by subcritical extraction is removed by rotary evaporation instead of molecular distillation. Although it can improve the purity of the kavalactone extract, it still cannot achieve the purification effect of the present application.

Claims

1. A method for preparing a kava extract having soothing and anti-allergic properties, characterized in that: The following steps are involved: ① Put the kava root powder into an extraction tank, and perform subcritical extraction on the kava root powder using an organic solvent as an extraction solvent to obtain an extract A; ② The extract A is evaporated under reduced pressure and filtered in turn to obtain a crude extract B; ③ Add the crude extract B into the feed bottle of the molecular distillation equipment, and set the feed bottle temperature to 50-70°C, the pressure to <200Pa, and the distillation temperature to 100-140°C; When the temperature and pressure reach the set value, start feeding, and set the scraping speed to 40-70r / min and the feed flow rate to 20-50mL / min; After the feeding is completed, the mixture is allowed to stand for 1 to 2 hours under vacuum and the fraction bottles are reassembled to obtain a yellow oily liquid C; ④ Dry the yellow oily liquid C to obtain the kavalactone extract.

2. The method for preparing a kava extract having soothing and anti-allergic properties according to claim 1, characterized in that: In the step ①, the kava root is first dried and crushed, and then passed through a 50-120 mesh sieve to obtain the kava root powder.

3. The method for preparing a kava extract having soothing and anti-allergic properties according to claim 2, characterized in that: In the step ①, the drying temperature of the Kava root is 45-70°C.

4. The method for preparing a kava extract having soothing and anti-allergic properties according to claim 1, characterized in that: The organic solvent in step ① is any one of butane, propane, isobutane and dimethyl ether, and the mass ratio of the kava root powder to the organic solvent during extraction is 1:3-4.

5. The method for preparing a kava extract having soothing and anti-allergic properties according to claim 1, characterized in that: The subcritical extraction method of the kava root powder in step ① is specifically as follows: the kava root powder and the organic solvent are loaded into an extraction tank, and the organic solvent is used to extract the kava root powder under an extraction temperature of 55 to 65° C. and an extraction pressure of 1 to 3 MPa to obtain an extract A.

6. The method for preparing a kava extract having soothing and anti-allergic properties according to claim 1, characterized in that: The reduced pressure evaporation method of the A extract in step ② is specifically as follows: the A extract is sent to a separation tank for reduced pressure evaporation, the reduced pressure evaporation time is 15 to 30 minutes, and after the evaporation is completed, the liquid remaining at the bottom of the separation tank is discharged to obtain a pre-filtered concentrated liquid.

7. The method for preparing a kava extract having soothing and anti-allergic properties according to claim 1, characterized in that: The filtering method in step ② is centrifugal separation, and the centrifugal speed during centrifugal separation is greater than 2000g.

8. Use of the kava extract prepared by the method for preparing the kava extract with soothing and anti-allergic ability according to any one of claims 1 to 7 in the soothing effect of cosmetics.

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