CN114231359A - Preparation method of agilawood extract - Google Patents
Preparation method of agilawood extract Download PDFInfo
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- CN114231359A CN114231359A CN202111585792.XA CN202111585792A CN114231359A CN 114231359 A CN114231359 A CN 114231359A CN 202111585792 A CN202111585792 A CN 202111585792A CN 114231359 A CN114231359 A CN 114231359A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/02—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in boilers or stills
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D2011/002—Counter-current extraction
Abstract
The invention relates to the technical field of agilawood extracts, in particular to a preparation method of an agilawood extract, which comprises the following steps: s1 cleaning lignum Aquilariae Resinatum, and crushing to obtain lignum Aquilariae Resinatum powder; s2, grinding agilawood powder and 35-40% ethanol solution in an inert atmosphere, and performing microwave irradiation for 60-100S to obtain an agilawood solid-liquid mixture; s3, performing supercritical fluid extraction on the solid-liquid mixture of agilawood to obtain a first-stage extract and residue 1; s4, performing multi-stage countercurrent extraction on the material slag to obtain a secondary extract and material slag 2; s5, heating and distilling the material residue 2 to obtain a distillation extract; s6 mixing the first-stage extract, the second-stage extract and the distilled extract, filtering, vacuum concentrating, recovering solvent, freezing, centrifuging, collecting supernatant, and vacuum concentrating to obtain lignum Aquilariae Resinatum essential oil; the extraction process provided by the invention not only improves the extraction rate of the agilawood essential oil, but also has the advantages of high content of effective components, good color and luster degree and high quality.
Description
Technical Field
The invention relates to the technical field of agilawood extracts, and particularly relates to a preparation method of an agilawood extract.
Background
The agilawood is wood containing resin of Aquilaria sinensis (Lour.) root (Aquilaria sinensis (Lour.) Gilg) which is a plant of Thymelaeaceae, is mainly produced in Hainan, Guangdong, Fujian and other provinces in China, has thick, lasting and long-lasting fragrance, and is widely applied to furniture, medicines, spices and other aspects.
In recent years, extraction research on agilawood components is deepened, aroma components of the agilawood components mainly comprise compounds such as sesquiterpenes, aromatics and chromones, in the existing agilawood extraction process, a water vapor distillation method, a solvent extraction method, a supercritical extraction method and the like are usually adopted to extract the active ingredients of the agilawood, but in the existing extraction process, extraction of the agilawood essential oil is long in time consumption, the extraction yield and the content of the active ingredients are low, and impurities such as residual vegetable wax and pigment are easily mixed, so that the problems of poor color degree, insufficient quality and the like of the extracted agilawood essential oil are caused. Therefore, in order to solve the above disadvantages, it is urgently needed to provide a preparation method of agilawood extract with stable extraction yield, and provide an important technical basis for promoting clinical medicine and perfume of the agilawood extract.
Disclosure of Invention
In view of this, the invention provides a preparation method of agilawood extract with stable extraction yield, which not only improves the extraction rate of agilawood essential oil, but also has high content of effective components, good color and luster degree and high quality.
The technical scheme of the invention is realized as follows:
a preparation method of agilawood extract comprises the following steps:
s1, cleaning fresh agilawood, drying in the sun, cutting into blocks, and crushing into powder to obtain agilawood powder;
s2, adding agilawood powder and 35-40% ethanol solution into a grinder in an inert atmosphere for grinding for 5-8min, and performing microwave irradiation treatment for 60-100S by using power of 280 plus power of 300W in the ball milling process to obtain an agilawood solid-liquid mixture;
s3, adding the solid-liquid mixture of agilawood into an extraction kettle, inputting supercritical carbon dioxide fluid, and performing supercritical fluid extraction to obtain a first-stage extract and material residue 1;
s4, adding the material residue into a continuous extraction kettle, and performing multistage countercurrent extraction at 40-50 ℃ by adopting an ethanol solution with the mass concentration of 95% to obtain a secondary extract and material residue 2;
s5, adding distilled water into the material residue 2, adding the material residue into a distillation kettle, heating and distilling, quickly cooling steam through a cooling pipe, and cooling to obtain a distillation extracting solution;
s6, combining the first-stage extract, the second-stage extract and the distilled extracting solution, filtering by using a multi-stage filter, concentrating under vacuum and reduced pressure by 14-18% of the volume, recovering the solvent, freezing and centrifuging, taking the supernatant, and concentrating under reduced pressure to obtain the agilawood essential oil.
Further, in the step S2, the ratio of the agilawood powder to the ethanol solution is (30-35):1 g/ml.
Further, in the step S3, the extraction pressure is 15-20MPa, the extraction temperature is 50-60 ℃, the extraction time is 35-45min, and CO is added2The flow rate is 10-20 Kg/h.
Further, in the S4, ethanol with the mass concentration of 90-95% is continuously and circularly sprayed at 40-50 ℃ for 3-stage countercurrent extraction, the material-liquid ratio of the material residue 1 to the ethanol solution is 1 (10-20) g/ml, and the single-stage extraction time is 10-20 min.
Further, in the step S5, the distillation temperature is 105-115 ℃, the condensation temperature of the condensation tube is 10-12 ℃, and the distillation is performed until no gas is generated.
In step S5, the ratio of the slag 2 to the distilled water is 1 (20-25) g/ml.
Further, in the step S6, the centrifugation time is 10-13 min, and the centrifugation rate is 3800-4200 r/min.
In S6, the multistage filter includes a vegetable fat filter, a pigment adsorber, and a resin filter.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, the agilawood powder is subjected to ball milling and microwave irradiation combined treatment, a low-concentration ethanol solution is used as an infiltration effect of an auxiliary agent, microwaves are used as a heat source, the surface molecular motion of the agilawood powder is promoted under the combination of physical acting force and short-time irradiation effect, the loosening effect of a plant tissue cell wall structure is fully degraded, and the obtained agilawood solid-liquid mixture not only remarkably improves the dissolution rate of the agilawood essential oil, but also is beneficial to promoting the subsequent extraction quality of the active ingredients of the agilawood.
(2) According to the invention, the solid-liquid mixture of the agilawood is subjected to combination of supercritical fluid extraction, multistage countercurrent extraction and heating distillation extraction, so that the effective components of the agilawood are fully separated and extracted, and compared with the traditional dissolution extraction separation of single powder, the extraction yield of the method is more stable, the agilawood essential oil is extracted to the maximum extent, no additional auxiliary agent is required to be added, the quality of the extracted agilawood essential oil is improved, and the color degree is good and stable.
(3) The primary extract and the secondary extract obtained by combining multiple extraction methods are combined with distillation extraction, combined and filtered, so that the vegetable wax, resin and pigment in the agilawood essential oil are reduced, the purity and color of the agilawood essential oil are ensured, the quality of the agilawood is improved, the defect of high loss rate caused by the traditional refining treatment is effectively avoided, the yield of the agilawood essential oil is ensured, and the quality of the agilawood essential oil is improved.
Detailed Description
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the examples of the present invention can be obtained commercially without specific description.
Example 1-method for preparing agilawood extract comprising the steps of:
s1, cleaning fresh agilawood, drying in the sun, cutting into blocks, and crushing into powder to obtain agilawood powder;
s2, adding agilawood powder and 35% ethanol solution into a grinder to be ground for 8min in an argon inert atmosphere according to the material-liquid ratio of 30:1g/ml, and performing microwave irradiation treatment for 100S by adopting power of 280W in the ball milling process to obtain an agilawood solid-liquid mixture;
s3, adding the solid-liquid mixture of lignum Aquilariae Resinatum into an extraction kettle, and inputting supercritical carbon dioxide fluid for supercritical fluid extraction at an extraction temperature of 50 deg.C and an extraction pressure of 15MPa for 45min with CO2The flow rate is 10Kg/h, and a first-grade extract and material slag 1 are obtained;
s4, adding the material residue 1 into a continuous extraction kettle, and performing 3-stage countercurrent extraction at 40 ℃ by adopting an ethanol solution with the mass concentration of 90%, wherein the material-liquid ratio of the material residue 1 to the ethanol solution is 1:10g/ml, and the single-stage extraction time is 10min, so as to obtain a second-stage extract and material residue 2;
s5, adding distilled water into the material residue 2, wherein the material-liquid ratio of the material residue 2 to the distilled water is 1:20g/ml, adding the material residue 2 to the distilled water into a distillation kettle, heating and distilling, wherein the distillation temperature is 105 ℃, the condensation temperature of a condensation pipe is 10 ℃, the distillation is carried out until no gas is generated, steam is rapidly cooled by a cooling pipe, and a distilled extracting solution is obtained after cooling;
s6, combining the first-stage extract, the second-stage extract and the distilled extract, sequentially filtering by a multi-stage filter provided with a vegetable fat filter, a pigment adsorber and a resin filter, concentrating the mixture in vacuum at 14% of the volume, recovering the solvent, carrying out refrigerated centrifugation at-18 ℃ for 10min at a centrifugation speed of 3800r/min, taking the supernatant, and concentrating the supernatant in vacuum to obtain the agilawood essential oil.
Example 2-method for preparing agilawood extract, comprising the steps of:
s1, cleaning fresh agilawood, drying in the sun, cutting into blocks, and crushing into powder to obtain agilawood powder;
s2, adding agilawood powder and 40% ethanol solution into a grinding machine to be ground for 5min in an argon inert atmosphere according to the material-liquid ratio of 30:1g/ml, and performing microwave irradiation treatment for 60S by adopting power of 300W in the ball milling process to obtain an agilawood solid-liquid mixture;
s3, adding the solid-liquid mixture of lignum Aquilariae Resinatum into an extraction kettle, and inputting supercritical carbon dioxide fluid for supercritical fluid extraction at an extraction temperature of 60 deg.C and an extraction pressure of 20MPa for 35min with CO2The flow rate is 20Kg/h, and a first-grade extract and material slag 1 are obtained;
s4, adding the material residue 1 into a continuous extraction kettle, and performing 3-stage countercurrent extraction at 50 ℃ by adopting an ethanol solution with the mass concentration of 95%, wherein the material-liquid ratio of the material residue 1 to the ethanol solution is 1:20g/ml, and the single-stage extraction time is 10-20min, so as to obtain a second-stage extract and material residue 2;
s5, adding distilled water into the material residue 2, wherein the material-liquid ratio of the material residue 2 to the distilled water is 1:25g/ml, adding the material residue 2 to the distilled water into a distillation kettle, heating and distilling, wherein the distillation temperature is 115 ℃, the condensation temperature of a condensation pipe is 12 ℃, the distillation is carried out until no gas is generated, steam is rapidly cooled by a cooling pipe, and a distilled extracting solution is obtained after cooling;
s6, combining the first-stage extract, the second-stage extract and the distilled extract, sequentially filtering by a multi-stage filter provided with a vegetable fat filter, a pigment adsorber and a resin filter, concentrating the mixture in vacuum at a volume of 18% and recovering the solvent, freezing and centrifuging the mixture at-18 ℃ for 13min at a centrifugation speed of 4200r/min, taking the supernatant, and concentrating the supernatant in vacuum to obtain the agilawood essential oil.
Example 3-method for preparing agilawood extract, comprising the steps of:
s1, cleaning fresh agilawood, drying in the sun, cutting into blocks, and crushing into powder to obtain agilawood powder;
s2, adding agilawood powder and 38% ethanol solution into a grinding machine for grinding for 6min in an argon inert atmosphere according to the material-liquid ratio of 32:1g/ml, and performing microwave irradiation treatment for 90S by adopting power of 280W in the ball milling process to obtain an agilawood solid-liquid mixture;
s3, adding the solid-liquid mixture of lignum Aquilariae Resinatum into an extraction kettle, and inputting supercritical carbon dioxide fluid for supercritical fluid extraction at an extraction temperature of 55 deg.C and an extraction pressure of 18MPa for 40min with CO2The flow rate is 15Kg/h, and a first-grade extract and material slag 1 are obtained;
s4, adding the material residue 1 into a continuous extraction kettle, and performing 3-stage countercurrent extraction at 45 ℃ by adopting an ethanol solution with the mass concentration of 95%, wherein the material-liquid ratio of the material residue 1 to the ethanol solution is 1:15g/ml, and the single-stage extraction time is 15min to obtain a second-stage extract and material residue 2;
s5, adding distilled water into the material residue 2, wherein the material-liquid ratio of the material residue 2 to the distilled water is 1:22g/ml, adding the material residue 2 to the distilled water into a distillation kettle, heating and distilling, wherein the distillation temperature is 110 ℃, the condensation temperature of a condensation pipe is 11 ℃, the distillation is carried out until no gas is generated, steam is rapidly cooled by a cooling pipe, and a distilled extracting solution is obtained after cooling;
s6, combining the first-stage extract, the second-stage extract and the distilled extract, sequentially filtering by a multi-stage filter provided with a vegetable fat filter, a pigment adsorber and a resin filter, concentrating the mixture in vacuum at 16% of the volume, recovering the solvent, carrying out refrigerated centrifugation at-18 ℃ for 12min at the centrifugation speed of 4000r/min, taking the supernatant, and concentrating the supernatant in vacuum to obtain the agilawood essential oil.
Comparative example 1
According to the preparation method of the agilawood extract in the embodiment 3, the preparation method of the agilawood solid-liquid mixture is changed, and specifically, in the step S2, agilawood solid-liquid mixture is obtained by adding agilawood powder and 38% ethanol solution into a grinder to grind for 6min in an inert atmosphere according to the material-liquid ratio of 32:1g/ml, and performing microwave irradiation treatment for 5min with the power of 600W in the ball milling process.
Comparative example 2
According to the preparation method of the agilawood extract in the embodiment 3, the preparation method of the agilawood solid-liquid mixture is changed, and specifically, in the step S2, agilawood solid-liquid mixture is obtained by adding agilawood powder and distilled water into a grinding machine for grinding for 6min in an inert atmosphere according to the material-liquid ratio of 32:1g/ml, and performing microwave irradiation treatment for 90S with power of 280W in the ball milling process.
Comparative example 3
Preparing an agilawood extract by using conventional agilawood powder, specifically, according to the agilawood powder prepared in the step S1 of the example 3, directly performing extraction treatment in the steps S3-S5, combining the first-stage extract, the second-stage extract and the distilled extract, filtering by using a multi-stage filter, performing vacuum concentration on the mixture by 16% of volume, recovering the solvent, performing refrigerated centrifugation, taking supernate, and performing vacuum concentration to obtain agilawood essential oil.
According to the preparation methods of the agilawood extracts of the above examples and comparative examples, under the same batch of agilawood raw materials, the extraction yield of each agilawood essential oil is counted, wherein the yield of the agilawood essential oil is ═ g of the mass of the agilawood essential oil/g of the mass of the raw material multiplied by 100%; and (3) analyzing active substances of the prepared different agilawood essential oil samples by adopting a gas chromatography-mass spectrometer GC-MS (gas chromatography-mass spectrometer), wherein the chromatographic conditions are as follows: the chromatographic column is as follows: RTX-5MS (30m × 0.25mm × 0.25 μm), sample introduction temperature of 280 deg.C, sample introduction amount of 1 μ l, and flow rate of 1.0 ml/min; the split ratio is 28:1, the sample carrier gas is He, and the temperature rising procedure is as follows: keeping the temperature at 80 ℃ for 2min, heating to 160 ℃ at 10 ℃/min, heating to 280 ℃ at 3 ℃/min, and keeping the temperature for 10 min; the mass spectrum conditions are as follows: measuring the contents of terpenoids, chromones, aromatic compounds and fatty acid compounds at an electron energy of 70eV and an ion source temperature of 250 ℃, observing the physicochemical properties of the agilawood essential oil, and obtaining the results shown in the following table,
as can be seen from the above table, the solid-liquid mixture of agilawood obtained by performing ball milling and microwave irradiation combined treatment on agilawood powder and using a low-concentration ethanol solution as an infiltration effect of an auxiliary agent and using microwave irradiation with a certain power as a heat source is extracted by the combination of supercritical fluid extraction, multistage countercurrent extraction and heating distillation extraction, thereby maximally extracting agilawood essential oil, wherein the extraction yield can reach more than 1.5%, meanwhile, the total content of effective active substances of the extracted agilawood essential oil can reach more than 80%, the content of fatty acid compounds is low, and the color and luster are stable.
Compared with the comparative examples 1-3, the preparation method of the agilawood solid-liquid mixture is changed in the comparative example 1, and the excessively high-power microwave irradiation treatment and the ball milling treatment are combined, so that the content of the fatty acid compound is obviously increased, and the condition for regulating and controlling the treatment condition of the agilawood solid-liquid mixture is favorable for ensuring the quality of the agilawood essential oil; the extraction in the comparative example 2 is obviously reduced, and the total content of the effective active substances of the agilawood essential oil is lower, which shows that the low-concentration ethanol solution is adopted as the auxiliary agent to infiltrate the agilawood powder, thereby being beneficial to promoting the dissolution rate of the agilawood essential oil, reducing the loss rate of the effective active substances and improving the quality of the essential oil; the results of the embodiment 3 and the comparative example 3 show that the yield of the agilawood essential oil is improved by 51.4 percent by adopting the solid-liquid agilawood mixture to directly extract the agilawood powder, the content of the active ingredients of the agilawood essential oil is improved, the color degree is good, and the quality is high.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. The preparation method of the agilawood extract is characterized by comprising the following steps of:
s1, cleaning fresh agilawood, drying in the sun, cutting into blocks, and crushing into powder to obtain agilawood powder;
s2, adding agilawood powder and 35-40% ethanol solution into a grinder in an inert atmosphere for grinding for 5-8min, and performing microwave irradiation treatment for 60-100S by using power of 280 plus power of 300W in the ball milling process to obtain an agilawood solid-liquid mixture;
s3, adding the solid-liquid mixture of agilawood into an extraction kettle, inputting supercritical carbon dioxide fluid, and performing supercritical fluid extraction to obtain a first-stage extract and material residue 1;
s4, adding the material slag into a continuous extraction kettle, and performing multistage countercurrent extraction at 40-50 ℃ by adopting an ethanol solution with the mass concentration of 90-95% to obtain a secondary extract and material slag 2;
s5, adding distilled water into the material residue 2, adding the material residue into a distillation kettle, heating and distilling, quickly cooling steam through a cooling pipe, and cooling to obtain a distillation extracting solution;
s6, combining the first-stage extract, the second-stage extract and the distilled extracting solution, filtering by using a multi-stage filter, concentrating under vacuum and reduced pressure by 14-18% of the volume, recovering the solvent, freezing and centrifuging, taking the supernatant, and concentrating under reduced pressure to obtain the agilawood essential oil.
2. The method for preparing agilawood extract according to claim 1, wherein in step S2, the material-to-liquid ratio of agilawood powder to ethanol solution is (30-35):1 g/ml.
3. The method for preparing agilawood extract according to claim 1, wherein in step S3, the extraction pressure is 15-20MPa, the extraction temperature is 50-60 ℃, the extraction time is 35-45min, and CO is added2The flow rate is 10-20 Kg/h.
4. The preparation method of the agilawood extract according to claim 1, wherein in S4, ethanol with a mass concentration of 95% is continuously and circularly sprayed at 40-50 ℃ to perform 3-stage countercurrent extraction, the feed-liquid ratio of the residue 1 to the ethanol solution is 1 (10-20) g/ml, and the single-stage extraction time is 10-20 min.
5. The method as claimed in claim 1, wherein in step S5, the distillation temperature is 105-115 ℃, the condensation temperature of the condensation tube is 10-12 ℃, and no gas is generated.
6. The method for preparing an agilawood extract according to claim 5, wherein in step S5, the feed-liquid ratio of residue 2 to distilled water is 1 (20-25) g/ml.
7. The method for preparing an agilawood extract according to claim 1, wherein in the step S6, the centrifugation time is 10-13 min, and the centrifugation rate is 3800-4200 r/min.
8. The method of claim 1, wherein in step S6, the multistage filter comprises a vegetable fat filter, a pigment adsorber and a resin filter.
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| CN115772446A (en) * | 2022-11-17 | 2023-03-10 | 钟伟杰 | Agilawood essential oil and preparation method and application thereof |
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