Method for extracting kava lactones for cosmetic use

Abstract

The application discloses a kind of extraction methods of kava lactones for cosmetics, belong to natural plant effective component extraction technical field.The steps of the extraction method include: after drying, kava pepper root is crushed and sieved, to obtain kava pepper root powder;The kava pepper root powder is mixed with water in heating device and heated to 70~90℃, after heating, into filter device, under the pressure of 0.4~0.6MPa, filtration, filtrate is entered into filter device again by heating device, so carry out cycle filtration;Take the filtrate after cycle filtration and cool crystallization, filter, to obtain paste material, the obtained paste material is heated to 45~55℃, and centrifugal, take supernatant, after cooling, it is kava lactones for cosmetics.The extraction and purification process provided by the application does not need to use organic solvent, breaks through innovation on extraction solvent, eliminates the possibility of kava lactones product organic solvent residue from the source, and the safety of the extracted kava lactones is guaranteed.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of natural plant effective component extraction, and particularly relates to an extraction method of kavalactones for cosmetics. BACKGROUND

[0002] Kava (Piper methysticum Forst) is a perennial erect shrub medicinal plant of Piperaceae, which is produced in the South Pacific islands. The roots and rhizomes are used as medicine, and the effective part is the fat-soluble resin part. In recent years, kava is used as a food supplement by people in many countries in the world to regulate anxiety, depression and other insomnia problems and psychological problems caused by excessive stress. The main effective components of kava are kavalactones, narcotic pepper alkaline and kavacon, which can bidirectionally regulate neurotransmitters and have the effects of anti-anxiety and depression, sedation and sleep, local anesthesia, anti-convulsion and the like.

[0003] Kavalactones are insoluble in water and easily soluble in organic solvents such as methanol, ethanol and dichloromethane, and have the characteristics of low melting point. The melting point of kavalactones is 45℃. At present, the main extraction processes of kavalactones are alcohol solution extraction and supercritical extraction, but in actual technical application, there are problems of solvent residue in the finished product or excessively high extraction cost in kavalactone extraction.

[0004] Therefore, low-cost production by using conventional equipment has become the threshold for popularization of kavalactone preparation technology. SUMMARY

[0005] The application aims to provide an extraction method of kavalactones for cosmetics, which has no solvent residue and low extraction cost.

[0006] To achieve the above-mentioned purpose, the application provides the following technical scheme.

[0007] An extraction method of kavalactones for cosmetics, comprising the following steps:

[0008] The dried kava roots are crushed and sieved to obtain kava root powder; the kava root powder is mixed with water in a heating device and heated to 70-90℃, and after heating, the filtrate is introduced into a filtering device under the pressure of 0.4-0.6 MPa, and the filtering is performed by circulating the filtrate through the heating device and the filtering device; the filtrate after the circulating filtration is cooled and crystallized, filtered to obtain a paste-like substance, the paste-like substance is heated to 45-55℃ and centrifuged, and the supernatant is taken to obtain kavalactones for cosmetics after cooling.

[0009] Preferably, the drying temperature of the kava roots is 50-70℃.

[0010] Preferably, the crushed piper cubeba root is sieved to 80-100 mesh.

[0011] Preferably, the mass ratio of the piper cubeba root powder to water is 1:15-30.

[0012] Preferably, the filter screen of the filtering device has a mesh size of 500-1000 mesh.

[0013] Preferably, the time for the circulation filtering is 4-8 h.

[0014] Preferably, the cooling crystallization is performed at a temperature of 0-10℃ for 14-48 h.

[0015] Preferably, the centrifugal force for the centrifugation is not less than 3000 g.

[0016] The technical principle of the present application is as follows: according to the characteristic that kava lactone has a melting point of 45℃, the piper cubeba root or rhizome powder is heated to 70-90℃ so that the kava lactone is completely in liquid state, and then high-pressure filtration is performed to wash the kava lactone out of the piper cubeba root or rhizome powder with water as the mobile phase. In this process, the kava lactone, hot water, oil substances (such as essential oil, etc.) in the piper cubeba, and water-soluble substances form a mixed emulsion, i.e. kava lactone crude extract, and the kava lactone is extracted from the piper cubeba in this way; then the kava lactone crude extract is separated and purified, and high-purity kava lactone is obtained.

[0017] The beneficial technical effects of the present application are as follows:

[0018] (1) The present application uses pure water as the extraction solvent, and the water-insoluble kava lactone is extracted under high temperature and high pressure, which is a breakthrough innovation in the extraction solvent of kava lactone.

[0019] (2) The extraction and purification process provided by the present application does not need to use organic solvents, which completely eliminates the possibility of organic solvent residues in kava lactone products, and the safety of the extracted kava lactone is guaranteed. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 High-performance liquid chromatogram of the kava lactone extracted in Example 1. DETAILED DESCRIPTION

[0021] The various illustrative embodiments of the present application will now be described in detail in connection with the accompanying drawings. This description is made for the purpose of demonstrating certain aspects of the present application and should not be taken as a limitation on the present application. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the present application.

[0022] Also, for ranges of values, the disclosure herein is understood to include every possible intermediate value, as well as every sub-range between any two of the stated values or intermediate values. The upper and lower limits of these smaller ranges can independently be included or excluded in the ranges.

[0023] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. Although methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present application, the preferred methods and materials are described herein.

[0024] As used herein, the terms "comprise", "comprising", "include", "including", "have", "having" and the like are open-ended and do not exclude additional elements or steps.

[0025] Example 1

[0026] Extraction process of kava lactones:

[0027] (1) Take 20 kg of kava pepper root powder dried at 60°C to a moisture content of about 5%, pass through an 80-mesh sieve to obtain kava pepper root powder, ready for use;

[0028] (2) Take 10 kg of kava pepper root powder and add it to a reaction kettle containing 150 kg of water. The reaction kettle is connected to a plate and frame filter (500 mesh). The inlet of the reaction kettle is connected to the outlet of the plate and frame filter, and the outlet of the reaction kettle is connected to the inlet of the plate and frame filter. The mixture in the reaction kettle is stirred uniformly and heated to 80°C. The clear liquid is filtered out under a filtration pressure of 0.4 MPa, and the clear liquid is transferred from the outlet of the plate and frame filter to the reaction kettle for heat preservation. The cycle is repeated for 6 hours, and the clear liquid is separated;

[0029] (3) The obtained clear liquid is crystallized at 4°C for 24 hours, filtered, and the paste-like substance obtained is the crude extract of kava lactones;

[0030] (4) The crude extract of kava lactones is re-heated to 50°C and centrifuged at a centrifugal force of 3000 g for 10 min. The supernatant is cooled to room temperature to obtain 802 g of kava lactones.

[0031] The purity of the obtained kava lactones is analyzed by ultraviolet spectrophotometry. The analysis results show that the purity of kava lactones is 80.31%.

[0032] When determining the purity of kava lactones by ultraviolet spectrophotometry, the standard substance is selected as methysticin standard substance (CAS No. 500-64-1, Shanghai Shidand, purity ≥98.0%); the detection wavelength is 506 nm.

[0033] The preparation method of the blank group is as follows: in a centrifuge tube, add 2 mL of 0.5 mol / L hydroxylamine hydrochloride ethanol solution, 0.6 mL of 6 mol / L sodium hydroxide solution, and 0.2 mL of methanol solution, mix thoroughly, shake for 140 s, then add 4 mL of 1 mol / L hydrochloric acid solution, continue to shake for 60 s, then add 0.3 mL of 5% FeCl3 solution, shake well and stand still.

[0034] The blank group is used for wavelength of 506 nm under the condition of absorbance zero calibration.

[0035] The control group and the sample group refer to the preparation method of the blank group, and the standard and sample are added respectively.

[0036] Further, the specific composition of the kava lactones obtained is identified by high performance liquid chromatography.

[0037] When identifying the kava lactone components by high performance liquid chromatography, the standard used is piperlongumine standard (CAS No. 500-64-1, Shanghai Shidand, purity ≥98.0%), dihydropiperlongumine standard (CAS No. 587-63-3, Shanghai Yuanye, purity ≥98.0%), piperlongumine (CAS No. 495-85-2, Shanghai Yuanye, purity ≥98.0%), dihydropiperlongumine (CAS No. 19902-91-1, Shanghai Yuanye, purity ≥95.0%), desmethoxy piperlongumine (CAS No. 15345-89-8, Shanghai Yuanye, purity ≥97.0%) and methoxy piperlongumine (CAS No. 500-62-9, Shanghai Yuanye, purity ≥98.0%).

[0038] The chromatographic conditions are as follows:

[0039] Chromatographic column: Agilent TC-C18 25 cm x 4.6 mm 5 μm;

[0040] Mobile phase: methanol: acetonitrile: water (21:26:38, V / V / V);

[0041] Column temperature: 25°C;

[0042] Flow rate: 1.0 mL / min;

[0043] Detection wavelength: 246 nm.

[0044] The high performance liquid chromatogram of the sample is shown in Figure 1 , which is identified, Figure 1The components were as follows: narcotic pepper bitter (retention time 11.16 min), dihydro-narcotic pepper bitter (retention time 11.55 min), kava-kava bitter (retention time 12.22 min), dihydro-kava-kava bitter (retention time 13.16 min), desmethoxy-kava-kava bitter (retention time 16.82 min) and methoxy-kava-kava bitter (retention time 17.87 min).

[0045] Example 2

[0046] Extraction process of kava-kava bitter:

[0047] (1) 20 kg of kava-kava root powder dried at 60°C to a moisture content of about 5% was pulverized through an 80-mesh sieve to obtain kava-kava root powder, which was used as needed;

[0048] (2) 10 kg of kava-kava root powder was added to a reaction kettle containing 150 kg of water, the reaction kettle was connected to a plate-and-frame filter (500 mesh), the inlet of the reaction kettle was connected to the outlet of the plate-and-frame filter, the outlet of the reaction kettle was connected to the inlet of the plate-and-frame filter, the mixture in the reaction kettle was stirred uniformly and heated to 90°C, the clear liquid was filtered out under a filtration pressure of 0.5 MPa, and the clear liquid was circulated and filtered for 4 h, and the clear liquid was separated;

[0049] (3) The obtained clear liquid was crystallized at 0°C for 14 h, and then filtered to obtain a paste-like substance, which was kava-kava bitter crude extract;

[0050] (4) The kava-kava bitter crude extract was heated to 45°C again, and centrifuged at a centrifugal force of 3000 g for 10 min, and the supernatant was cooled to room temperature to obtain 809 g of kava-kava bitter.

[0051] The purity of the obtained kava-kava bitter was analyzed by ultraviolet spectrophotometry, and the analysis results showed that the purity of the kava-kava bitter was 80.27%.

[0052] The component identification results were the same as those of Example 1.

[0053] Example 3

[0054] Extraction process of kava-kava bitter:

[0055] (1) 20 kg of kava-kava root powder dried at 60°C to a moisture content of about 5% was pulverized through an 80-mesh sieve to obtain kava-kava root powder, which was used as needed;

[0056] (2) take 10 kg of Piper cubeba root powder into a reactor containing 150 kg of water, the reactor is connected with a plate and frame filter (500 mesh), the inlet of the reactor is connected with the outlet of the plate and frame filter, the outlet of the reactor is connected with the inlet of the plate and frame filter, the mixture in the reactor is stirred uniformly and heated to 70℃, the mixture is discharged from the outlet into the plate and frame filter, the filtrate is filtered out under a filtration pressure of 0.6 MPa, the filtrate is discharged from the outlet of the plate and frame filter into the reactor for heat preservation, and the cycle filtration is performed for 8 h, and the filtrate is separated;

[0057] (3) the obtained filtrate is crystallized at 10℃ for 48 h, filtered, and a paste-like substance is obtained, which is the crude extract of cubebin;

[0058] (4) the crude extract of cubebin is heated to 55℃ again, centrifuged at a centrifugal force of 3000 g for 10 min, and the supernatant is cooled to room temperature, and 814 g of cubebin is obtained.

[0059] The purity of the obtained cubebin is analyzed by a UV spectrophotometer, and the analysis result shows that the purity of the cubebin is 80.11%.

[0060] The component identification result is the same as that of Example 1.

[0061] The above-described examples only describe the preferred modes of the present application, and do not limit the scope of the present application, and various modifications and improvements to the technical solutions of the present application made by those skilled in the art without departing from the design spirit of the present application shall fall within the protection scope of the present application defined by the claims.

Claims

1. A method for extracting a kava lactone for cosmetic use, characterized by, The method comprises the following steps: The dried piper cubeba root is crushed and sieved to obtain piper cubeba root powder; the piper cubeba root powder is mixed with water in a heating device and heated to 70-90 DEG C, and after heating, the mixture is filtered in a filtering device under a pressure of 0.4-0.6 MPa, the filtrate is again introduced into the filtering device through the heating device, and the cycle is repeated; the filtrate after the cycle is cooled and crystallized, filtered, to obtain a paste-like substance, which is heated to 45-55 DEG C and centrifuged, and the supernatant is obtained and cooled to obtain the piper cubeba lactone for cosmetics; The temperature for the cooling and crystallization is 0-10 DEG C, and the time is 14-48 h.

2. The extraction method of a carbophenol for cosmetics according to claim 1, characterized by, The drying temperature of the piper cubeba root is 50-70 DEG C.

3. The extraction method of a carbavexanoid for a cosmetic according to claim 1, characterized by, The crushed and sieved piper cubeba root is sieved through a 80-100 mesh sieve.

4. The extraction method of a carbavexine for a cosmetic according to claim 1, characterized by, The mass ratio of the piper cubeba root powder to water is 1:15-30.

5. The extraction method of a carbavexanoid for a cosmetic according to claim 1, characterized by, The mesh size of the filter screen of the filtering device is 500-1000.

6. The extraction method of a carbavexanoid for a cosmetic according to claim 1, characterized by, The time for the cycle filtration is 4-8 h.

7. The extraction method of a carbavexanoid for a cosmetic according to claim 1, characterized by, The centrifugal force for the centrifugation is not less than 3000 g.

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