CN113736567A - Preparation method of sandalwood essential oil - Google Patents
Preparation method of sandalwood essential oil Download PDFInfo
- Publication number
- CN113736567A CN113736567A CN202111057355.0A CN202111057355A CN113736567A CN 113736567 A CN113736567 A CN 113736567A CN 202111057355 A CN202111057355 A CN 202111057355A CN 113736567 A CN113736567 A CN 113736567A
- Authority
- CN
- China
- Prior art keywords
- sandalwood
- essential oil
- solvent
- extracting
- sandalwood essential
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a preparation method of sandalwood essential oil. The preparation method comprises the following steps: (1) pulverizing sandalwood into sandalwood powder, adding the sandalwood powder into the extracting solution for soaking, then stirring and extracting, filtering and collecting filtrate, stirring and extracting filter residues in the extracting solution for 2-3 times, merging the filtrate, and evaporating the extracting solution to obtain sandalwood paste; (2) adding an adsorbent into the sandalwood paste, and uniformly mixing to obtain a dry sample; (3) loading the dry sample into a glass chromatographic column, eluting with a solvent to obtain an eluent, and evaporating the solvent from the eluent to obtain sandalwood essential oil; the extracting solution is an ethanol water solution with the volume concentration of 85-95%. According to the method, the sandalwood essential oil is separated and enriched by combining a process for extracting the sandalwood essential oil at a low temperature by using an ethanol aqueous solution and a glass chromatographic column separation technology, so that the fragrance components in the sandalwood are completely extracted, the fragrance components which are poor in storage stability and sensitive to heat are enriched to the greatest extent, the quality and the yield of the sandalwood essential oil can be improved, and the production cost is reduced.
Description
Technical Field
The invention belongs to the technical field of essential oil extraction, and particularly relates to a preparation method of sandalwood essential oil.
Background
Sandalwood (Santalum album) belongs to Santalaceae and Pistacia, and is a semi-parasitic evergreen small arbor. The heartwood of the sandalwood, commonly known as sandalwood, is a rare traditional Chinese medicinal material, has the effects of warming spleen and stomach for dispelling cold, dispelling cold for relieving pain, regulating qi and harmonizing stomach, and is clinically used for treating diseases such as stomachache, eructation, hiccup, palpitation and the like. In addition, sandalwood is also a precious wood perfume, is a traditional religious article and a fine process carving material, and the essential oil extracted from sandalwood, namely sandalwood essential oil, has unique aromatic smell and lasting fragrance, is one of the most widely used essential oils in the world, is widely applied to industries such as essence/perfume, cosmetics and health products, and is an expensive essential oil, so the sandalwood essential oil is also called as 'liquid gold'.
Research paper about sandalwood essential oil extraction method reports supercritical CO2Extraction, solvent impregnation, steam distillation, and the like. Such as: supercritical CO2Research on supercritical CO was conducted by Zhongzhongfeng et al, a research on technology for extracting sandalwood essential oil2The technology for extracting sandalwood essential oil comprises the following steps under the optimal extraction process conditions: the extraction time is 150min, the extraction pressure is 30MPa, the extraction temperature is 45 ℃, and the average extraction rate of the sandalwood essential oil is 8.02 percent; the method is suitable for extracting essential oil from sandalwood with high oil content, is not suitable for extracting essential oil from sandalwood powder with extremely low content, and has large capital investment and large occupied space of equipment.
The components obtained by the solvent extraction method are complex, and the quality and the appearance of the essential oil are difficult to meet the market requirements, such as: liu Xiaojin et al recorded in the "essential oil content and component difference of Sandalwood heartwood and marginals" that essential oil of Sandalwood heartwood and marginals is extracted respectively by using an ether extraction method, and the components and content of the essential oil are contrastively analyzed by adopting a GC-MS technology, and the results show that: the sandalwood heartwood has significantly higher essential oil content than the sapwood, with average relative contents of 4.44% and 1.33%, respectively.
The steam distillation method is difficult to completely extract the aroma components, and the extraction temperature is high, the extraction time is long, and partial heat-sensitive aroma components are damaged and lost, such as: yan Ting et al, in "comparison and identification of volatile chemical components of Sandalwood heartwood in different producing areas" and Chen Shi Xia et al, in "influence of different extraction methods on the content and components of volatile oil of Sandalwood", respectively, report that the chemical components of the Sandalwood essential oil obtained by adopting the steam distillation method and the solvent extraction method are detected by the GC-MS method, and two conclusions are consistent, namely: the steam distillation method and the solvent extraction method have similar chemical components and proportion, but the steam distillation method has lower volatile oil ratio.
Mulberry sources and the like adopt thawing microwave-assisted steam distillation to extract sandalwood volatile oil in 'process research for thawing microwave-assisted steam distillation to extract sandalwood volatile oil by thawing', and the method comprises the steps of adding an ethanol extracting agent into residual powder produced in sandalwood processing in India, immediately putting the powder into a refrigerator at the temperature of-20 ℃, freezing the powder for 2 hours, then carrying out microwave heating, putting the powder into a volatile oil extractor, carrying out normal-pressure steam distillation for a certain time to obtain transparent pale yellow oily liquid with special smell, removing water by using anhydrous sodium sulfate, and measuring the yield of the volatile oil. Under the optimal process conditions, namely: the microwave irradiation time is 20s, the volume usage of the ethanol aqueous solution is 1.2 times of the raw material amount (volume ratio), the ethanol concentration is 80%, the distillation time after pretreatment is 60min, and the extraction rate of the sandalwood volatile oil is 2.03%. The article focuses on the effect of microwave irradiation time, amount of ethanol solution, ethanol concentration and steam distillation time on extraction efficiency.
The invention patent with publication number CN108203625A discloses a method for producing sandalwood essential oil, which adopts microwave and ultrasonic wave synergistic treatment to extract sandalwood essential oil, and then utilizes high-speed countercurrent chromatography and supercritical mass spectrometry to further extract and purify. The process is essentially to extract the sandalwood with high oil content, the raw materials are extremely expensive, the process is complex, the time consumption is long, the requirement on equipment is high, the production cost is high, and the price of the sandalwood essential oil product obtained by the process is also very high.
Therefore, a method for extracting sandalwood essential oil, which has the advantages of simple and easy operation process, high extraction efficiency, easy industrial production, maximally enriching and protecting aroma components with poor stability and sensitivity to heat, improving the quality of sandalwood essential oil products and reducing the production cost, is urgently needed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of sandalwood essential oil. The preparation method of the sandalwood essential oil has the advantages of simple and easy operation, high extraction efficiency and easy industrial production, and the extracted sandalwood essential oil has high yield and good quality.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of sandalwood essential oil comprises the following steps:
(1) pulverizing sandalwood into sandalwood powder, adding the sandalwood powder into the extracting solution for soaking, then stirring and extracting, filtering and collecting filtrate, stirring and extracting filter residues after filtering in the extracting solution for 2-3 times, merging the filtrate, and evaporating the extracting solution to dryness to obtain a sandalwood paste;
(2) adding an adsorbent into the sandalwood paste, and uniformly mixing to obtain a dry sample;
(3) loading the dry sample into a glass chromatographic column, eluting with a solvent to obtain an eluent, and evaporating the solvent from the eluent to obtain sandalwood essential oil;
the extracting solution is ethanol water solution with volume concentration of 85-95%.
The sandalwood is at least one of the heartwood and the edge wood of the sandalwood.
The ethanol aqueous solution with the volume concentration of 85-95% is used as the extracting solution of the sandalwood essential oil, so that the production cost is reduced, the environmental pollution is avoided, various polar fragrance components of the sandalwood are extracted from wood fibers of the sandalwood, fragrance active components of the sandalwood are completely extracted, the yield of the sandalwood essential oil is greatly improved, and the sandalwood essential oil is high in yield and strong in fragrance. Modern column chromatography technology separates and removes non-fragrant components, greatly improves the quality of essential oil. Therefore, the sandalwood essential oil is separated and enriched by combining the technology of extracting the sandalwood essential oil by the ethanol aqueous solution at low temperature and the glass chromatographic column separation technology, so that the fragrance components of sandalwood are completely extracted, the fragrance components which are poor in stability and sensitive to heat are enriched and stored to the maximum extent, the quality and the yield of the sandalwood essential oil can be improved, and the production cost is reduced.
According to the invention, the ethanol water solution with the volume concentration of 85-95% is used as the extracting solution of the sandalwood essential oil, and the obtained sandalwood essential oil has high yield, strong fragrance, good fluidity and high quality.
As a preferred embodiment of the present invention, in the step (1), the ratio of the mass of the sandalwood powder to the volume of the extracting solution is 1g: 8-12 mL; the temperature for stirring and extracting lignum Santali albi powder in the extractive solution is 40-60 deg.C, and the time is 15-60 min.
In a preferred embodiment of the invention, in the step (1), the temperature for stirring and extracting the filter residue in the extracting solution is 40-60 ℃; if the mixture is stirred and extracted for 3 times, the solid-to-liquid ratio of the 3 times of extraction is 1g: 7-11 mL, 1g: 7-10 mL, 1g: 7-10 mL, and the time is 30-45 min, 15-30 min and 15-30 min in sequence; if the mixture is stirred and extracted for 2 times, the liquid-solid ratio of the 2 times of extraction is 1g: 7-11 mL, 1g: 7-10 mL, and the time is 30-45 min and 15-30 min in sequence.
In the step (1), the solid-to-liquid ratio and the extraction time of the extracting solution and the sandalwood powder or filter residue have great influence on the yield and the quality of the sandalwood essential oil, the solid-to-liquid ratio is low, the extraction time is short, the yield of the essential oil is obviously reduced, the fragrance abundance degree of the essential oil is also reduced, mainly because the fragrance components of the sandalwood exist in the cytoplasm and the nucleus of the wood fiber cells of the sandalwood, the extracting solution firstly wets the sandalwood, then penetrates the cell wall and the cell membrane to diffuse into the cytoplasm to dissolve the fragrance active components, and finally the fragrance active components are extracted into an extracting agent from the cytoplasm, so the using amount (the solid-to-liquid ratio) of the extracting solution and the extraction time are main factors influencing the extraction efficiency. The sandalwood essential oil extracted by the extracting solution in the step (1) has high yield and high quality, wherein the yield is up to more than 4.1%.
As a preferred embodiment of the present invention, in the step (1), the stirring speed is 200-2000 rpm.
In a preferred embodiment of the present invention, in the step (1), the method of evaporating the extract solution comprises: and evaporating the combined filtrate to dryness at 40-60 ℃ and under the vacuum degree of 0.08-0.1 MPa.
In the step (2), the adsorbent is silica gel, and the particle size is 80-300 meshes; the weight ratio of the sandalwood paste to the adsorbent is 1: 1-3.
The quality of the sandalwood essential oil is affected by the proportion of the sandalwood paste and the adsorbent, the dosage of the adsorbent is too low, and the fluidity, transparency and aroma of the essential oil are poor.
More preferably, the particle size of the adsorbent is 160 to 200 meshes.
In a preferred embodiment of the present invention, in the step (3), the solvent is a mixed solvent of a solvent a and a solvent B, a volume ratio of the solvent a to the solvent B is 10:1 to 7:1, the solvent a is the petroleum ether or n-hexane, and the solvent B is acetone.
As a preferred embodiment of the present invention, in the step (3), the solvent evaporation method comprises: evaporating the solvent of the eluent at 40-60 ℃ and under the vacuum degree of 0.05-0.1 MPa.
In a preferred embodiment of the present invention, in the step (3), the aspect ratio of the glass chromatography column is 5 to 20.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the method, the sandalwood essential oil is separated and enriched by combining a process for extracting the sandalwood essential oil at a low temperature by using an ethanol aqueous solution and a glass chromatographic column separation technology, so that the fragrance components of sandalwood are completely extracted, the fragrance components which are poor in stability and sensitive to heat are enriched and stored to the greatest extent, the quality and the yield of the sandalwood essential oil can be improved, and the production cost is reduced.
(2) The preparation method of the sandalwood essential oil disclosed by the invention is simple in process, easy to operate, high in extraction efficiency, good in quality and easy for industrial production.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
In the embodiments and comparative examples of the present invention, the sandalwood powder is obtained by pulverizing sawdust generated during the production of sandalwood products into sandalwood powder.
Example 1
The embodiment of the preparation method of sandalwood essential oil of the invention is as follows:
1) 10.01g of sandalwood powder is weighed, and 120mL of ethanol aqueous solution with volume concentration of 95% (liquid: solid-12: 1, V: w), soaking in water bath at 40 ℃ for 15min, stirring at 40 ℃ for 1h, and performing vacuum filtration by using a Buchner funnel to obtain a first extracting solution A;
2) filtering residues in the step 1) according to the liquid: solid is 11: 1 (V: W), adding 110mL of 95% ethanol, stirring and extracting at 40 ℃ for 45min, and performing vacuum filtration by using a Buchner funnel to obtain a second extracting solution B;
3) filtering residues obtained in the step 2) according to the liquid: solid 10:1 (V: W), adding 100mL of 95% ethanol, stirring at 40 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a third extracting solution C;
4) filtering residues obtained in the step 3) according to the liquid: solid is 7:1 (V: W), adding 70mL of 95% ethanol, stirring at 40 ℃ for 15min, and performing vacuum filtration by using a Buchner funnel to obtain a fourth extracting solution D;
5) the A, B, C, D four extracting solutions are combined, the solvent is evaporated in a water bath at the temperature of 40 ℃ under the vacuum degree of 0.1MPa to obtain thick reddish brown paste, and a solution with the weight 1 time (W: w) silica gel (160-200 meshes), mixing the two uniformly, and fully volatilizing to obtain a dry sample;
6) loading the dry sample of 5) above into a glass chromatographic column with a length diameter of 20, and separating with petroleum ether: eluting with a mixed solvent of 8:1 acetone, and collecting the eluent; evaporating the mixed solvent to dryness in 45 deg.C water bath under vacuum degree of 0.08MPa to obtain thick light brown sandalwood essential oil 0.45 g. The yield of sandalwood essential oil is 4.5%.
Example 2
The embodiment of the preparation method of sandalwood essential oil of the invention is as follows:
1) 10.00g of sandalwood powder is weighed, 100mL of ethanol aqueous solution with volume concentration of 95% (liquid: solid 10:1, V: w), soaking in water bath at 40 ℃ for 15min, stirring at 40 ℃ for 1h, and performing vacuum filtration by using a Buchner funnel to obtain a first extracting solution A;
2) filtering residues in the step 1) according to the liquid: solid is 9: 1 (V: W), adding 90mL of 95% ethanol, stirring and extracting at 40 ℃ for 45min, and performing vacuum filtration by using a Buchner funnel to obtain a second extracting solution B;
3) filtering residues obtained in the step 2) according to the liquid: solid is 8:1 (V: W), adding 80mL of 95% ethanol, stirring at 40 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a third extracting solution C;
4) filtering residues obtained in the step 3) according to the liquid: solid is 7:1 (V: W), adding 70mL of 95% ethanol, stirring at 40 ℃ for 15min, and performing vacuum filtration by using a Buchner funnel to obtain a fourth extracting solution D;
5) the A, B, C, D four extracting solutions are combined, the solvent is evaporated in a water bath at the temperature of 40 ℃ under the vacuum degree of 0.1MPa to obtain thick reddish brown paste, and a solution with the weight 1 time (W: w) silica gel (160-200 meshes), mixing the two uniformly, and fully volatilizing to obtain a dry sample;
6) loading the dry sample of 5) above into a glass chromatographic column with a length diameter of 15, and separating with petroleum ether: eluting with a mixed solvent of 8:1 acetone, and collecting the eluent; evaporating the mixed solvent to dryness in 45 deg.C water bath under vacuum degree of 0.08MPa to obtain thick light brown sandalwood essential oil 0.41 g. The yield of the sandalwood essential oil is 4.1%.
Example 3
The embodiment of the preparation method of sandalwood essential oil of the invention is as follows:
1) 10.01g of sandalwood powder is weighed, and 120mL of ethanol aqueous solution with volume concentration of 95% (liquid: solid-12: 1, V: w), soaking in water bath at 40 ℃ for 60min, stirring at 40 ℃ for 1h, and performing vacuum filtration by using a Buchner funnel to obtain a first extracting solution A;
2) filtering residues in the step 1) according to the liquid: solid is 11: 1 (V: W), adding 110mL of 95% ethanol, stirring and extracting at 40 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a second extracting solution B;
3) filtering residues obtained in the step 2) according to the liquid: solid 10:1 (V: W), adding 100mL of 95% ethanol, stirring at 40 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a third extracting solution C;
4) filtering residues obtained in the step 3) according to the liquid: solid is 7:1 (V: W), adding 70mL of 95% ethanol, stirring at 40 ℃ for 15min, and performing vacuum filtration by using a Buchner funnel to obtain a fourth extracting solution D;
5) the A, B, C, D four extracts were combined, the solvent was evaporated in a 50 ℃ water bath under a vacuum of 0.09MPa to give a thick reddish brown paste, and 2 times the weight of the paste (W: w) silica gel (160-200 meshes), mixing the two uniformly, and fully volatilizing to obtain a dry sample;
6) loading the dry sample of 5) above into a glass chromatographic column with a length of 5, eluting with n-hexane: eluting with a mixed solvent of 8:1 acetone, and collecting the eluent; evaporating the mixed solvent to dryness in 50 deg.C water bath under vacuum degree of 0.08MPa to obtain thick light brown sandalwood essential oil 0.45 g. The yield of sandalwood essential oil is 4.5%.
Example 4
The embodiment of the preparation method of sandalwood essential oil of the invention is as follows:
1) 10.02g of sandalwood powder is weighed, and 120mL of ethanol aqueous solution with the volume concentration of 93% (liquid: solid-12: 1, V: w), soaking in water bath at 40 ℃ for 30min, stirring at 40 ℃ for 1h, and performing vacuum filtration by using a Buchner funnel to obtain a first extracting solution A;
2) filtering residues in the step 1) according to the liquid: solid is 11: 1 (V: W), adding 110mL of 93% ethanol, stirring and extracting at 40 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a second extracting solution B;
3) filtering residues obtained in the step 2) according to the liquid: solid 10:1 (V: W), adding 100mL of 93% ethanol, stirring at 40 ℃ for 15min, and performing suction filtration under reduced pressure by using a Buchner funnel to obtain a third extracting solution C;
4) filtering residues obtained in the step 3) according to the liquid: solid is 7:1 (V: W), adding 70mL of 93% ethanol, stirring at 40 ℃ for 15min, and performing vacuum filtration by using a Buchner funnel to obtain a fourth extracting solution D;
5) the A, B, C, D four extracts were combined, the solvent was evaporated in a water bath at 45 ℃ under a vacuum of 0.1MPa to give a thick reddish brown paste, and 1 time the weight of the paste (W: w) silica gel (160-200 meshes), mixing the two uniformly, and fully volatilizing to obtain a dry sample;
6) loading the dry sample of 5) above into a glass chromatographic column with a length diameter of 20, and separating with petroleum ether: eluting with a mixed solvent of acetone 7:1, and collecting the eluent; evaporating the mixed solvent to dryness in 45 deg.C water bath under vacuum degree of 0.08MPa to obtain thick light brown sandalwood essential oil 0.44 g. The yield of sandalwood essential oil is 4.4%.
Example 5
The embodiment of the preparation method of sandalwood essential oil of the invention is as follows:
1) 10.00g of sandalwood powder is weighed, and 120mL of ethanol aqueous solution with volume concentration of 90% (liquid: solid-12: 1, V: w), soaking in water bath at 40 ℃ for 15min, stirring at 40 ℃ for 1h, and performing vacuum filtration by using a Buchner funnel to obtain a first extracting solution A;
2) filtering residues in the step 1) according to the liquid: solid 10:1 (V: W), adding 100mL of 90% ethanol, stirring and extracting at 40 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a second extracting solution B;
3) filtering residues obtained in the step 2) according to the liquid: solid is 8:1 (V: W), adding 100mL of 90% ethanol, stirring at 40 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a third extracting solution C;
4) filtering residues obtained in the step 3) according to the liquid: solid is 7:1 (V: W), adding 70mL of 90% ethanol, stirring at 40 ℃ for 15min, and performing vacuum filtration by using a Buchner funnel to obtain a fourth extracting solution D;
5) the A, B, C, D four extracts were combined, the solvent was evaporated in a water bath at 45 ℃ under a vacuum of 0.1MPa to give a thick reddish brown paste, and 1 time the weight of the paste (W: w) silica gel (160-200 meshes), mixing the two uniformly, and fully volatilizing to obtain a dry sample;
6) loading the dry sample of 5) above into a glass chromatographic column with a length diameter of 15, and separating with petroleum ether: eluting with a mixed solvent of 8:1 acetone, and collecting the eluent; evaporating the mixed solvent to dryness in 45 deg.C water bath under vacuum degree of 0.01MPa to obtain thick light brown sandalwood essential oil 0.47 g. The yield of sandalwood essential oil is 4.7%.
Example 6
The embodiment of the preparation method of sandalwood essential oil of the invention is as follows:
1) 10.00g of sandalwood powder is weighed, and 120mL of ethanol aqueous solution with volume concentration of 95% (liquid: solid-12: 1, V: m), soaking in water bath at 60 ℃ for 15min, stirring at 60 ℃ for 1h, and performing vacuum filtration by using a Buchner funnel to obtain a first extracting solution A;
2) filtering residues in the step 1) according to the liquid: solid is 11: 1 (V: W), adding 110mL of 95% ethanol, stirring and extracting at 60 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a second extracting solution B;
3) filtering residues obtained in the step 2) according to the liquid: solid 10:1 (V: W), adding 100mL of 95% ethanol, stirring at 60 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a third extracting solution C;
4) filtering residues obtained in the step 3) according to the liquid: solid is 7:1 (V: W), adding 70mL of 95% ethanol, stirring at 60 ℃ for 15min, and performing vacuum filtration by using a Buchner funnel to obtain a fourth extraction solution D;
5) the A, B, C, D four extracting solutions are combined, the solvent is evaporated in a water bath at the temperature of 60 ℃ under the vacuum degree of 0.08MPa to obtain thick reddish brown paste, and a solution with the weight 1 time (W: w) silica gel (160-200 meshes), mixing the two uniformly, and fully volatilizing to obtain a dry sample;
6) loading the dry sample of 5) above into a glass chromatographic column with length-diameter ratio of 5, and separating with n-hexane: eluting with a mixed solvent of acetone 7:1, and collecting the eluent; evaporating the mixed solvent to dryness in 45 deg.C water bath under vacuum degree of 0.08MPa to obtain thick light brown sandalwood essential oil 0.49 g. The yield of sandalwood essential oil is 4.9%.
Example 7
The embodiment of the preparation method of sandalwood essential oil of the invention is as follows:
1) 10.00g of sandalwood powder is weighed, and 120mL of ethanol aqueous solution with the volume concentration of 95% (liquid: solid-12: 1, V: m), soaking in water bath at 40 ℃ for 15min, stirring at 40 ℃ for 1h, and performing vacuum filtration by using a Buchner funnel to obtain a first extracting solution A;
2) filtering residues in the step 1) according to the liquid: solid is 11: 1 (V: W), adding 110mL of 95% ethanol, stirring and extracting at 40 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a second extracting solution B;
3) filtering residues obtained in the step 2) according to the liquid: solid 10:1 (V: W), adding 100mL of 95% ethanol, stirring at 40 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a third extracting solution C;
4) filtering residues obtained in the step 3) according to the liquid: solid is 7:1 (V: W), adding 70mL of 95% ethanol, stirring at 40 ℃ for 15min, and performing vacuum filtration by using a Buchner funnel to obtain a fourth extracting solution D;
5) the A, B, C, D four extracts were combined, the solvent was evaporated in a water bath at 45 ℃ under a vacuum of 0.1MPa to give a thick reddish brown paste, and 3 times the weight of the paste (W: w) silica gel (160-200 meshes), mixing the two uniformly, and fully volatilizing to obtain a dry sample;
6) loading the dry sample of the 5) into a glass chromatographic column with the length-diameter ratio of 20, and carrying out chromatographic separation on the dry sample by using petroleum ether: eluting with a mixed solvent of 8:1 acetone, and collecting the eluent; evaporating the mixed solvent to dryness in a water bath at 45 ℃ and under the vacuum degree of 0.08MPa to obtain 0.56g of thick light brown sandalwood essential oil. The yield of sandalwood essential oil is 5.6%.
Example 8
The embodiment of the preparation method of sandalwood essential oil of the invention is as follows:
1) 10.01g of sandalwood powder is weighed, and 120mL of ethanol aqueous solution with the volume concentration of 95% (liquid: solid-12: 1, V: m), soaking in water bath at 40 ℃ for 15min, stirring at 40 ℃ for 1h, and performing vacuum filtration by using a Buchner funnel to obtain a first extracting solution A;
2) filtering residues in the step 1) according to the liquid: solid is 11: 1 (V: W), adding 110mL of 95% ethanol, stirring and extracting at 40 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a second extracting solution B;
3) filtering residues obtained in the step 2) according to the liquid: solid 10:1 (V: W), adding 100mL of 95% ethanol, stirring at 40 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a third extracting solution C;
4) filtering residues obtained in the step 3) according to the liquid: solid is 7:1 (V: W), adding 70mL of 95% ethanol, stirring at 40 ℃ for 15min, and performing vacuum filtration by using a Buchner funnel to obtain a fourth extracting solution D;
5) the A, B, C, D four extracts were combined, the solvent was evaporated in a water bath at 45 ℃ under a vacuum of 0.1MPa to give a thick reddish brown paste, and 1 time the weight of the paste (W: w) silica gel (160-200 meshes), mixing the two uniformly, and fully volatilizing to obtain a dry sample;
6) loading the dry sample of the 5) into a glass chromatographic column with the length-diameter ratio of 15, and carrying out chromatographic separation on the dry sample by using petroleum ether: eluting with a mixed solvent of acetone 7:1, and collecting the eluent; evaporating the mixed solvent to dryness in 45 deg.C water bath under vacuum degree of 0.1MPa to obtain thick light brown sandalwood essential oil 0.54 g. The yield of sandalwood essential oil is 5.4%.
Example 9
The embodiment of the preparation method of sandalwood essential oil of the invention is as follows:
1) 10.01g of sandalwood powder is weighed, and 120mL of ethanol aqueous solution with the volume concentration of 95% (liquid: solid-12: 1, V: m), soaking in water bath at 40 ℃ for 15min, stirring at 40 ℃ for 1h, and performing vacuum filtration by using a Buchner funnel to obtain a first extracting solution A;
2) filtering residues in the step 1) according to the liquid: solid is 11: 1 (V: W), adding 110mL of 95% ethanol, stirring and extracting at 40 ℃ for 45min, and performing vacuum filtration by using a Buchner funnel to obtain a second extracting solution B;
3) filtering residues obtained in the step 2) according to the liquid: solid 10:1 (V: W), adding 100mL of 95% ethanol, stirring at 40 ℃ for 30min, and performing vacuum filtration by using a Buchner funnel to obtain a third extracting solution C;
4) the A, B, C three extracting solutions are combined, the solvent is evaporated in a water bath at the temperature of 45 ℃ under the vacuum degree of 0.1MPa to obtain thick reddish brown paste, and a solvent with the weight 1 time (W: w) silica gel (160-200 meshes), mixing the two uniformly, and fully volatilizing to obtain a dry sample;
5) loading the dry sample of the 4) into a glass chromatographic column with the length-diameter ratio of 15cm, and carrying out chromatographic separation on the dry sample by using petroleum ether: eluting with a mixed solvent of 8:1 acetone, and collecting the eluent; evaporating the mixed solvent to dryness in 45 deg.C water bath under vacuum degree of 0.08MPa to obtain thick light brown sandalwood essential oil 0.48 g. The yield of sandalwood essential oil is 4.8%.
Comparative example 1
The only difference between the comparative example of the preparation method of sandalwood essential oil of the invention and the example 1 is that: in the steps 1) to 4), the volume concentration of the ethanol water solution is 80 percent; the yield of sandalwood essential oil obtained was 4.3%.
Comparative example 2
This comparative example explores the effect of different sandalwood essential oil preparation methods on sandalwood essential oil yield.
(1) Method for extracting sandalwood essential oil by microwave
Weighing 150.0g of sandalwood powder, soaking for 1h by 1200mL of 95% ethanol, then extracting by microwave for 3 times at the microwave power of 300W and the extraction temperature of 50 ℃ for 10min, wherein the solid-to-liquid ratio (W: V) is as follows in sequence: 1g:8mL, 1g:7mL, 1g:6mL, combining the extracting solutions for 3 times, and carrying out rotary evaporation and evaporation on the solvent in a water bath at the temperature of 60 ℃ under reduced pressure to obtain 18.21g of crude extract of red sandalwood essential oil, wherein the extraction rate is 12.14%.
Adding 23.2g of silica gel (260-200 meshes) into the crude extract of the sandalwood essential oil, mixing, and continuously stirring until the solvent is volatilized to obtain a dry sample; the dry sample was loaded into a glass chromatography column, purified with petroleum ether: eluting with a mixed solution of 15:1 acetone until the eluate has no fragrance of lignum Santali albi, collecting eluate, evaporating to remove solvent in 55 deg.C water bath under reduced pressure, and obtaining orange lignum Santali albi essential oil 5.08g with strong fragrance and good fluidity, with a yield of 3.3%.
(2) Method for extracting sandalwood essential oil by ultrasonic wave
Weighing 10.0g of sandalwood powder, soaking in 80mL of 95% ethanol for 1h, and then extracting by ultrasonic waves at 50 ℃ for 10min for 3 times, wherein the solid-to-liquid ratio is respectively as follows: 1g:8mL, 1g:7mL, 1g:7mL, combining the extracting solutions for 3 times, and performing rotary evaporation to remove the solvent by reduced pressure in a water bath at 60 ℃ to obtain 0.91g of crude extract of red sandalwood essential oil, wherein the extraction rate is 9.1%.
Adding 1.0g of silica gel (160-200 meshes) into the crude extract of the sandalwood essential oil, mixing, and continuously stirring until the solvent is volatilized to obtain a dry sample. The dry sample was loaded into a glass chromatography column, purified with petroleum ether: eluting with mixed solution of acetone 8:1 until the eluate has no fragrance of lignum Santali albi, collecting eluate, steaming in water bath at 60 deg.C under reduced pressure, and evaporating to remove solvent to obtain light brown lignum Santali albi essential oil 5.08g with strong fragrance and good fluidity, with a yield of lignum Santali albi essential oil of 2.5%.
(3) Method for extracting sandalwood essential oil by steam distillation method
Weighing 50.0g of sandalwood powder, adding sufficient water (submerging the surface of sandalwood chips), soaking for 2h, extracting for 8h by using a steam distillation method, extracting the extracting solution for 3 times by using anhydrous ether after the extraction is finished, combining the ether extracting solutions for 3 times, drying by using a proper amount of anhydrous magnesium sulfate, and carrying out reduced pressure rotary evaporation on the dried solution in a water bath at the temperature of 30 ℃ to evaporate the solvent to dryness, thereby obtaining 0.18g of light yellow sandalwood essential oil with light fragrance and good fluidity, wherein the yield of the sandalwood essential oil is 0.35%.
(4) Method for extracting sandalwood essential oil by 95% ethanol water
Weighing 20.0g of sandalwood powder, taking 95% ethanol as an extractant, heating and stirring for extraction for four times under 40 ℃ water bath, wherein the solid-to-liquid ratio (W: V) of each time is 1g:8mL, 1g:6mL, 1g:5mL and 1g:5mL, the extraction for 1h is carried out for each time, combining the extraction solutions of the four times, and carrying out decompression rotary evaporation and evaporation on the extraction solution in 50 ℃ water bath to remove the solvent to obtain 2.72g of red sandalwood paste, wherein the extraction rate is 13.6%.
Adding silica gel (160-200 meshes) with equal mass into the sandalwood paste, mixing, continuously stirring until the solvent is volatilized to obtain a dry sample, loading the dry sample into a glass chromatographic column, eluting with redistilled n-hexane until the effluent has light sandalwood fragrance, collecting the eluent, and evaporating the eluent in a 45 ℃ water bath under reduced pressure to dryness to obtain 0.29g of dark yellow sandalwood essential oil with strong fragrance and good fluidity, wherein the yield of the sandalwood essential oil is 1.45%.
Comparative example 3
This comparative example explores the effect of different extraction solvents on the yield of sandalwood essential oil.
(1) Heating, stirring and extracting petroleum ether
Weighing 20.0g of sandalwood powder, adding 160mL of petroleum ether, heating and stirring for extraction for 40min at 50 ℃ in a water bath, and extracting for four times, wherein the solid-to-liquid ratio is respectively as follows: 8mL of 1g, 7mL of 1g, 6mL of 1g and 5mL of 1g are combined, and the four extracting solutions are subjected to decompression rotary evaporation in a water bath at 50 ℃ to evaporate the solvent to dryness to obtain 0.34g of thick dark yellow sandalwood essential oil crude extract with the extraction rate of 1.7%.
(2) Petroleum ether room temperature extraction
Weighing 5.0g of sandalwood powder, extracting with petroleum ether at room temperature for three times: soaking the raw materials in a solid-liquid ratio of 1g:8mL for one day, 1g:7mL for two days, 1g:6mL for three days, combining the three extracting solutions, and performing rotary evaporation to remove the solvent by reduced pressure in a water bath at 60 ℃ to obtain 0.09g of viscous yellow sandalwood essential oil crude extract with the extraction rate of 1.8%.
(3) Extracting with 95% ethanol at room temperature
Weighing 5.0g of sandalwood powder, extracting with 95% ethanol at room temperature for three times: soaking the raw materials in a solid-liquid ratio of 1g:8mL for one day, 1g:7mL for two days, 1g:6mL for three days, combining the three extracting solutions, and performing rotary evaporation to remove the solvent by reduced pressure in a water bath at 60 ℃ to obtain 0.60g of thick red sandalwood essential oil crude extract with the extraction rate of 12.0%.
(4) Leaching acetone at room temperature
Weighing 5.0g of sandalwood powder, extracting with acetone at room temperature for three times: soaking the raw materials in a solid-liquid ratio of 1g:8mL for one day, 1g:7mL for two days, 1g:6mL for three days, combining the three extracting solutions, and performing rotary evaporation to remove the solvent by reduced pressure in a water bath at 60 ℃ to obtain 0.49g of thick orange red sandalwood essential oil crude extract, wherein the extraction rate is 9.8%.
Comparative example 4
This comparative example explores the effect of different extraction temperatures on the yield of sandalwood essential oil.
Weighing 10.0g of sandalwood powder, extracting with 95% ethanol at 40-60 ℃ for four times: the solid-liquid ratio is respectively 1g:12mL, 1g:11mL, 1g:10mL and 1g:7mL, and the extraction time is respectively as follows: 1h, 45min, 30min and 15 min. Mixing the extractive solutions, performing rotary evaporation at 60 deg.C under reduced pressure in water bath to remove solvent to obtain thick crude extract of red lignum Santali albi essential oil, adding silica gel (160-200 mesh) into the above lignum Santali albi paste, mixing, stirring to remove solvent to obtain dry sample, loading the dry sample into glass chromatographic column, and separating with petroleum ether: acetone ═ 8:1, collecting eluent, evaporating the eluent in a water bath at 45 ℃ under reduced pressure to dryness to obtain sandalwood essential oil, wherein the yield of the sandalwood essential oil is shown in the following table:
TABLE 1 yield values of sandalwood essential oil at different extraction temperatures
| Extraction temperature (. degree.C.) | Sandalwood essential oil yield (%) |
| 40 | 4.5 |
| 50 | 4.6 |
| 60 | 4.9 |
As can be seen from table 1, the sandalwood essential oil yield increased with increasing extraction temperature. But the yield of the sandalwood essential oil cannot be increased all the time, and when the extraction temperature is higher than 60 ℃, the yield of the sandalwood essential oil is reduced, so that the extraction temperature is within the range limited by the invention, and the essential oil prepared by the preparation method of the sandalwood essential oil has high yield and high quality.
Comparative example 5
In order to further explore the influence of each process condition of the sandalwood essential oil preparation method on the fragrance and appearance of the sandalwood essential oil, the following test groups were provided, the sandalwood essential oil preparation method of the test group was different from example 1 only in the parameters of the process condition of each test group in table 1, other parameters were the same as example 1, and the variable process conditions, the appearance, fragrance and comprehensive evaluation results of the sandalwood essential oil of the test groups are shown in table 2.
Evaluation of aroma: fixing three testers to smell the sandalwood essential oil products respectively, recording, if the smelling feels that the aroma concentrations are similar, then resting for 5min, then smelling again, taking the first smelling feeling as the standard, and finally integrating the evaluation results of 3 persons.
Criteria for comprehensive evaluation: the fragrance is strong, and the clarity and the fluidity of the product are better (++); the fragrance is strong or distinctive, and the product is turbid and is not (+); the fragrance is lighter, and the product is turbid and is lower (-).
TABLE 2 influence of different process conditions on appearance and fragrance of sandalwood essential oil
According to the data results in table 2, the addition amount (solid-to-liquid ratio) of the extracting solution, the extraction time, the extraction temperature, the concentration of the extracting solution, the weight ratio of the paste to the silica gel, and the ratio of the mixed solvent all affect the quality of the essential oil. Moreover, the above process parameters are within the limits of the present invention, and the quality of the prepared essential oil is the best.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. The preparation method of the sandalwood essential oil is characterized by comprising the following steps:
(1) pulverizing sandalwood into sandalwood powder, adding the sandalwood powder into the extracting solution for soaking, then stirring and extracting, filtering and collecting filtrate, stirring and extracting filter residues after filtering in the extracting solution for 2-3 times, merging the filtrate, and evaporating the extracting solution to dryness to obtain a sandalwood paste;
(2) adding an adsorbent into the sandalwood paste, and uniformly mixing to obtain a dry sample;
(3) loading the dry sample into a glass chromatographic column, eluting with a solvent to obtain an eluent, and evaporating the solvent from the eluent to obtain sandalwood essential oil;
the extracting solution is ethanol water solution with the volume concentration of 85-95%.
2. The method for preparing sandalwood essential oil as claimed in claim 1, wherein in step (1), the ratio of mass of sandalwood powder to volume of extracting solution is 1g: 8-12 mL; the temperature for stirring and extracting lignum Santali albi powder in the extractive solution is 40-60 deg.C, and the time is 15-60 min.
3. The method for preparing sandalwood essential oil as claimed in claim 1, wherein in step (1), the temperature of the residue in the extract solution is 40-60 ℃ for extraction by stirring; if the mixture is stirred and extracted for 3 times, the solid-to-liquid ratio of the 3 times of extraction is 1g: 7-11 mL, 1g: 7-10 mL, 1g: 7-10 mL, and the time is 30-45 min, 15-30 min and 15-30 min in sequence; if the mixture is stirred and extracted for 2 times, the liquid-solid ratio of the 2 times of extraction is 1g: 7-11 mL, 1g: 7-10 mL, and the time is 30-45 min and 15-30 min in sequence.
4. The method for preparing sandalwood essential oil as claimed in claim 1 wherein in step (1) the stirring speed is 200-2000 rpm.
5. The method for preparing sandalwood essential oil as claimed in claim 1 wherein in step (1) the method of evaporating the extract comprises: and evaporating the combined filtrate to dryness at 40-60 ℃ and under the vacuum degree of 0.08-0.1 MPa.
6. The method for preparing sandalwood essential oil as claimed in claim 1 wherein in step (2) the adsorbent is silica gel with a particle size of 80-300 mesh; the weight ratio of the sandalwood paste to the adsorbent is 1: 1-3.
7. The method for preparing sandalwood essential oil as claimed in claim 1, wherein in step (3), the solvent is a mixed solvent of solvent A and solvent B, the volume ratio of solvent A to solvent B is 10: 1-7: 1, solvent A is the petroleum ether or n-hexane, and solvent B is acetone.
8. The method for preparing sandalwood essential oil as claimed in claim 1 wherein in step (3) the solvent is evaporated by a method comprising: evaporating the solvent of the eluent at 40-60 ℃ and under the vacuum degree of 0.05-0.1 MPa.
9. The method for preparing sandalwood essential oil as claimed in claim 1 wherein in step (3) the glass chromatographic column has an aspect ratio of 5 to 20.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111057355.0A CN113736567A (en) | 2021-09-09 | 2021-09-09 | Preparation method of sandalwood essential oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111057355.0A CN113736567A (en) | 2021-09-09 | 2021-09-09 | Preparation method of sandalwood essential oil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113736567A true CN113736567A (en) | 2021-12-03 |
Family
ID=78737734
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111057355.0A Pending CN113736567A (en) | 2021-09-09 | 2021-09-09 | Preparation method of sandalwood essential oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113736567A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101322738A (en) * | 2007-06-11 | 2008-12-17 | 陈丽华 | Preparation of red sandalwood extract for treating diabetic and uses thereof |
| CN101624554A (en) * | 2009-08-04 | 2010-01-13 | 田仁德 | Method for extracting pterocarpus santalinus and method for using extracting liquid solution for surface decoration of wooden products |
| CN102321501A (en) * | 2011-08-24 | 2012-01-18 | 华宝食用香精香料（上海）有限公司 | A kind of process for extracting of santal characteristic perfume material |
| CN103789094A (en) * | 2014-01-21 | 2014-05-14 | 广州大学 | Method for extracting agilawood essential oil from agilawood chips |
| CN108203625A (en) * | 2018-03-16 | 2018-06-26 | 惠州学院 | A kind of production method of sandalwood essential oil |
| CN111084795A (en) * | 2019-09-12 | 2020-05-01 | 天津芸熙生物技术有限公司 | Preparation process of compound preparation extracted from sandalwood leaves at low temperature |
-
2021
- 2021-09-09 CN CN202111057355.0A patent/CN113736567A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101322738A (en) * | 2007-06-11 | 2008-12-17 | 陈丽华 | Preparation of red sandalwood extract for treating diabetic and uses thereof |
| CN101624554A (en) * | 2009-08-04 | 2010-01-13 | 田仁德 | Method for extracting pterocarpus santalinus and method for using extracting liquid solution for surface decoration of wooden products |
| CN102321501A (en) * | 2011-08-24 | 2012-01-18 | 华宝食用香精香料（上海）有限公司 | A kind of process for extracting of santal characteristic perfume material |
| CN103789094A (en) * | 2014-01-21 | 2014-05-14 | 广州大学 | Method for extracting agilawood essential oil from agilawood chips |
| CN108203625A (en) * | 2018-03-16 | 2018-06-26 | 惠州学院 | A kind of production method of sandalwood essential oil |
| CN111084795A (en) * | 2019-09-12 | 2020-05-01 | 天津芸熙生物技术有限公司 | Preparation process of compound preparation extracted from sandalwood leaves at low temperature |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1066055C (en) | Production method for extracting flavonoid compound extract or powder from bamboo leaf | |
| Li et al. | Focused microwave-assisted solvent extraction and HPLC determination of effective constituents in Eucommia ulmodies Oliv.(E. ulmodies) | |
| CN104398542B (en) | A kind of method of the extraction and purification flavones from the plant containing flavones | |
| CN102432582A (en) | Preparation method of proanthocyanidin | |
| CN104095174B (en) | The extracting method of propolis | |
| CN112545926A (en) | Comprehensive extraction method of folium artemisiae argyi volatile oil and folium artemisiae argyi total flavonoids and oxidation resistance evaluation of folium artemisiae argyi volatile oil | |
| CN102031116B (en) | New method for preparing rosemary natural antioxidant | |
| CN110496179B (en) | Method for extracting antioxidant substances from betel nut fruits and application | |
| CN104356105B (en) | A kind of preparation method of EGCG | |
| CN111840342B (en) | Synchronous extraction method of total flavonoids, triterpenes and high-antioxidant-activity yellow pigments | |
| CN110563584B (en) | Method for extracting and purifying chlorogenic acid in chrysanthemum morifolium ramat | |
| CN113736567A (en) | Preparation method of sandalwood essential oil | |
| CN104306758A (en) | Method for extracting polyphenol from sugar cane bark | |
| CN1248992C (en) | Preparation of oligomer and monomer from tannin by catalytic hydrogen degradation | |
| CN101177422A (en) | Process for preparing methylation catechin by tea | |
| EP3243828A1 (en) | Method for extracting stilbene compounds | |
| CN109771475A (en) | A method of extracting polyphenol from purple perilla seed shell | |
| CN101773528B (en) | Preparation method of total terpene lactones with low phenolic acid | |
| Li et al. | Extraction of aucubin from seeds of Eucommia ulmoides Oliv. using supercritical carbon dioxide | |
| CN114907191A (en) | Hemp impurity removal method | |
| CN105267440A (en) | Preparation technology of high EGCG low caffeine tea extract | |
| CN112552994A (en) | Zanthoxylum oil and preparation method thereof | |
| RU2279284C1 (en) | Method for integrated utilization of larch wood | |
| CN111096456A (en) | Preparation method of active component for inhibiting formation of late glycosylation product in lotus leaf | |
| CN117229850A (en) | Method for continuously extracting cinnamon essential oil by using steam and water |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |