CN113004975A - Method for extracting mixed volatile oil of angelica and fingered citron - Google Patents
Method for extracting mixed volatile oil of angelica and fingered citron Download PDFInfo
- Publication number
- CN113004975A CN113004975A CN202110295643.3A CN202110295643A CN113004975A CN 113004975 A CN113004975 A CN 113004975A CN 202110295643 A CN202110295643 A CN 202110295643A CN 113004975 A CN113004975 A CN 113004975A
- Authority
- CN
- China
- Prior art keywords
- volatile oil
- angelica
- fingered citron
- decoction pieces
- extracting
- 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.)
- Granted
Links
Images
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
-
- 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
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)
- Fats And Perfumes (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting mixed volatile oil of angelica and fingered citron, which comprises the following steps: (1) preparing raw materials of angelica and fingered citron; (2) extracting; (3) introducing steam, directly steaming radix Angelicae sinensis and fructus Citri Sarcodactylis decoction pieces, controlling temperature in the extraction container, controlling pressure of introduced steam, reflux-extracting volatile oil, collecting volatile oil, and extracting oil. The angelica is dried in the shade, so that the loss of the angelica volatile oil caused by traditional sun drying, baking and the like is avoided, and the extraction rate of the angelica volatile oil is low; the angelica and the fingered citron are cut into pieces with proper thickness, so that the volatile oil components are not damaged, the damage and the loss of the volatile oil components are avoided, and the extraction rate of the volatile oil is improved; the invention adopts steam to directly dry-steam the soaked decoction pieces, controls the pressure of the steam and the temperature and the pressure of condensed water, and improves the extraction rate of volatile oil. The volatile oil extracted by the invention is light yellow or light yellow brown transparent and uniform oily matter, and is suitable for industrial large-scale production.
Description
Technical Field
The invention relates to the technical field of volatile oil extraction, and particularly relates to a method for extracting mixed volatile oil of Chinese angelica and fingered citron.
Background
The extraction of volatile oil from angelica and fingered citron is difficult and is mainly limited by factors such as the origin of medicinal materials, processing mode, storage conditions, purity of the extracted volatile oil, extraction method, extraction conditions and the like. When the effective components in the angelica are sensitive to light and temperature and are easy to decompose and deteriorate, the angelica is easy to deteriorate and go oily due to overhigh temperature and overlong time or long-term contact with air during storage, and the quality of the angelica is seriously influenced. The angelica and fingered citron volatile oil contains light oil and heavy oil, if the volatile oil is dried in the sun, the light oil is mainly used, and if the volatile oil is dried, most of the volatile oil is heavy oil. The content of the dried angelica medicinal material is about 20 to 30 percent higher than that of the dried medicinal material volatile oil. However, the content of volatile oil is not high in both the sun-dried angelica and the oven-dried angelica. The processing temperature of the angelica medicinal material and the volatile oil content are in a straight negative relation.
At present, the methods for extracting the angelica or the fingered citron volatile oil generally comprise a steam distillation method, an organic solvent extraction method and a supercritical solvent extraction method. Although the steam distillation method has low cost, the extraction temperature is high, so that the components with lower boiling points are easy to volatilize, and the yield of the angelica oil is lower; the organic solvent extraction method commonly uses normal hexane, diethyl ether, petroleum ether, ethyl acetate, ethanol and the like as solvents, and the organic solvents are inflammable and explosive, have poor production safety, have solvent residues in products, influence the quality and quality of the products and influence the application of the products; the supercritical extraction method has high requirements on the process and equipment and is complex to operate. There are significant disadvantages to all three of the above methods.
The temperature control in the extraction process is also difficult in extracting the angelica and fingered citron mixed volatile oil, particularly in extracting the volatile oil by a steam distillation method, and the heating extraction temperature is effectively controlled. The temperature in the oil-water separator is better controlled, because the angelica volatile oil is extracted to obtain light oil at high temperature and heavy oil at low temperature, the extraction temperature and the temperature in the separator need to be reasonably controlled, thereby improving the extraction rate of the volatile oil as much as possible.
CN1014025B discloses a method for preparing 50% angelica volatile oil, which comprises washing angelica with clear water, soaking in distilled water, wherein the loss of angelica volatile oil is large, then extracting with water vapor without controlling the conditions of water vapor extraction, the obtained angelica volatile oil is milky oil-water mixture with low volatile oil content, in the embodiment, 500 g of angelica raw material is extracted to obtain 1000 g of milky product containing 50% angelica volatile oil, which is equivalent to 500 g of angelica volatile oil, and 500 g of angelica volatile oil is obtained by extracting 500 g of raw material, which is obviously unreasonable. According to the method recorded by researchers, the volatile oil cannot be obtained in the recorded amount, the obtained volatile oil product is milky oil-water mixture, belongs to aromatic water, does not belong to the volatile oil in the strict sense, and the proportion of the volatile oil in the mixture cannot be determined.
Disclosure of Invention
The invention provides a method for extracting mixed volatile oil of angelica and fingered citron, which aims to solve the technical problem of low extraction rate of the volatile oil of the angelica and the fingered citron in the prior art.
According to one aspect of the invention, the invention provides a method for extracting the mixed volatile oil of angelica and fingered citron, which aims to solve the technical problem of low purity of the volatile oil of angelica and fingered citron in the prior art.
The invention adopts the technical scheme that the method for extracting the mixed volatile oil of angelica and fingered citron comprises the following steps:
(1) preparing raw materials of angelica and fingered citron:
removing impurities from fresh radix Angelicae sinensis, drying in the shade, and slicing to obtain radix Angelicae sinensis decoction pieces; taking dried fingered citron raw medicinal materials, removing impurities, and slicing to obtain fingered citron decoction pieces for later use;
the angelica raw material is dried in the shade, washing and solarization are not needed, and volatile oil can be lost through washing, solarization and drying.
Further, the angelica and the fingered citron are sliced by a medicine slicing machine, and the thickness of the slices is 0.3 cm-0.8 cm. Too thick oil yield is low and almost oil-free; too thin, on the one hand, has great processing difficulty, and on the other hand, can damage the volatile oil components and has great loss of the volatile oil.
(2) Extraction: weighing radix Angelicae sinensis decoction pieces and fructus Citri Sarcodactylis decoction pieces, mixing, adding wetting amount of water, wetting, draining off excessive water after soaking for a period of time, and placing the soaked radix Angelicae sinensis decoction pieces and fructus Citri Sarcodactylis decoction pieces in an extraction container;
further, in the step (2), the mass ratio of the angelica sinensis decoction pieces to the fingered citron decoction pieces is 1:0.5-1.5 (preferably 1:0.8-1.2, more preferably 1: 1). Too high or too low a ratio can affect the yield of the final volatile oil.
Further, in the step (2), the extraction container is a multifunctional extraction tank.
Further, in the step (2), the water with the wetting amount is the water surface covered by the medicinal materials. Preferably 0.5-1.5 times (preferably 0.8-1.2 times, more preferably 1 time) of the total weight of radix Angelicae sinensis decoction pieces and fructus Citri Sarcodactylis decoction pieces. Too much water will dissolve the volatile oil and too little water will not completely soak the decoction pieces.
Further, in the step (2), the soaking time is 5-30min (preferably 15 min). The soaking time is too long, volatile oil in the decoction pieces can be dissolved and taken away, and the yield of the obtained volatile oil can be influenced. The soaking time is too short, the decoction pieces cannot be fully soaked, so that volatile oil in the decoction pieces cannot be extracted, and the yield is also influenced.
The invention mixes and puts angelica decoction pieces and fingered citron decoction pieces into an extraction container to extract volatile oil, the obtained volatile oil is light yellow or light yellow brown transparent and uniform oily matter, and the extraction rate and the purity are higher.
(3) Introducing steam from the bottom of the extraction container, directly dry-steaming the soaked radix Angelicae sinensis decoction pieces and fructus Citri Sarcodactylis decoction pieces, controlling the temperature in the extraction container, introducing steam and volatile oil into the volatile oil extractor, condensing to generate stable condensate, controlling the pressure of the introduced steam, reflux-extracting volatile oil, collecting volatile oil, and finishing oil extraction.
Further, in the step (3), the temperature in the extraction container is controlled to be 95-100 ℃, and the amount of steam introduced into the extraction container is controlled.
Further, in the step (3), the pressure of the introduced steam is controlled to be 0.05mpa or less, preferably 0.02 to 0.04mpa, more preferably 0.03 mpa. The pressure is too large to generate pressure in the tank, the volatile oil can not be volatilized, the medicinal materials can be damaged, the water outlet speed is high, the collected water is mainly water, and the target oil components can not be separated.
Further, in step (3), collecting the volatile oil with a clean jar.
Further, in the step (3), the volatile oil is extracted under reflux for 6 to 12 hours, and the optimal time is 8 hours (the time is long and no volatile oil is increased).
Further, in the step (3), the pressure of condensed water used for condensation is more than or equal to 0.2MPa, and the temperature of the condensed water is 15-20 ℃. Research shows that the pressure and the temperature of condensed water are reasonably controlled, so that the purity of the volatile oil obtained by condensation is higher, and the yield of the volatile oil is considered at the same time. The temperature of the condensed water is too low, the volatile oil contains more impurities, and the yield of the volatile oil is influenced due to the too high temperature of the condensed water.
And (3) before introducing steam to the bottom of the extraction container, opening a circulating water switch of the volatile oil extractor, opening an air inlet valve of the volatile oil extractor, and controlling valves of pipelines on the volatile oil extractor.
The invention has the following beneficial effects:
1. according to the invention, the angelica is dried in the shade, so that the technical problem of low extraction rate of the angelica volatile oil due to the loss of the angelica volatile oil caused by traditional sun drying, baking and the like is solved;
2. the angelica and the fingered citron are cut into pieces with proper thickness, so that the volatile oil components are not damaged, the damage and the loss of the volatile oil components are avoided, and the extraction rate of the volatile oil is improved;
3. the Chinese angelica and the fingered citron are mixed to extract the volatile oil, and the extraction rate of the mixed volatile oil of the two raw materials can be improved after the medicinal materials are mixed according to a certain proportion;
4. according to the invention, the decoction pieces are soaked by using a proper amount of water, and a proper soaking time is combined, so that the loss of the volatile oil is reduced to the minimum, and the extraction rate of the volatile oil is improved;
5. the invention adopts steam to directly dry-steam the soaked decoction pieces, controls the pressure of the steam and the temperature and the pressure of condensed water, and improves the extraction rate of volatile oil. Research shows that if Chinese angelica and fingered citron decoction pieces are directly extracted, the yield of volatile oil is low, the oil yield is low, and target components cannot be obtained.
6. The method is suitable for industrial large-scale production.
The invention solves the problem that the oil is not easy to extract in the extraction and separation of angelica and fingered citron. The invention optimizes the extraction process of the angelica and fingered citron mixed volatile oil by adopting a steam dry distillation method, and lays a foundation for further improving the extraction efficiency and development value of the angelica and fingered citron volatile oil.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below with reference to the drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a diagram showing the results of thin layer chromatography of the volatile oil obtained in preferred embodiment 1 of the present invention and a reference drug;
FIG. 2 is a thin-layer chromatography result chart of the volatile oil obtained in the preferred embodiments 2 and 3 of the present invention and the reference drug.
Detailed Description
The embodiments of the invention will be described in detail below with reference to the accompanying drawings, but the invention can be embodied in many different forms, which are defined and covered by the following description.
The method for extracting the mixed volatile oil of angelica and fingered citron comprises the following steps:
(1) preparing raw materials of angelica and fingered citron:
removing impurities from fresh radix Angelicae sinensis, drying in the shade, and slicing to obtain radix Angelicae sinensis decoction pieces; taking dried fingered citron raw medicinal materials, removing impurities, and slicing to obtain fingered citron decoction pieces for later use;
the angelica raw material is dried in the shade, washing and solarization are not needed, and volatile oil can be lost through washing, solarization and drying.
Further, the angelica and the fingered citron are sliced by a medicine slicing machine, and the thickness of the slices is 0.3 cm-0.8 cm. Too thick oil yield is low and almost oil-free; too thin, on the one hand, has great processing difficulty, and on the other hand, can damage the volatile oil components and has great loss of the volatile oil.
(2) Extraction: weighing radix Angelicae sinensis decoction pieces and fructus Citri Sarcodactylis decoction pieces, mixing, adding wetting amount of water, wetting, draining off excessive water after soaking for a period of time, and placing the soaked radix Angelicae sinensis decoction pieces and fructus Citri Sarcodactylis decoction pieces in an extraction container;
further, in the step (2), the mass ratio of the angelica sinensis decoction pieces to the fingered citron decoction pieces is 1:0.5-1.5 (preferably 1:0.8-1.2, more preferably 1: 1). Too high or too low a ratio can affect the yield of the final volatile oil.
Further, in the step (2), the extraction container is a multifunctional extraction tank.
Further, in the step (2), the water with the wetting amount is the water surface covered by the medicinal materials. Preferably 0.5-1.5 times (preferably 0.8-1.2 times, more preferably 1 time) of the total weight of radix Angelicae sinensis decoction pieces and fructus Citri Sarcodactylis decoction pieces. Too much water will dissolve the volatile oil and too little water will not completely soak the decoction pieces.
Further, in the step (2), the soaking time is 5-30min (preferably 15 min). The soaking time is too long, volatile oil in the decoction pieces can be dissolved and taken away, and the yield of the obtained volatile oil can be influenced. The soaking time is too short, the decoction pieces cannot be fully soaked, so that volatile oil in the decoction pieces cannot be extracted, and the yield is also influenced.
According to the invention, the angelica sinensis decoction pieces and the fingered citron decoction pieces are mixed and put into an extraction container to extract the volatile oil, and the extraction rate and the purity of the obtained volatile oil are higher.
(3) Introducing steam from the bottom of the extraction container, directly dry-steaming the soaked radix Angelicae sinensis decoction pieces and fructus Citri Sarcodactylis decoction pieces, controlling the temperature in the extraction container, introducing steam and volatile oil into the volatile oil extractor, condensing to generate stable condensate, controlling the pressure of the introduced steam, reflux-extracting volatile oil, collecting volatile oil, and finishing oil extraction.
Further, in the step (3), the temperature in the extraction container is controlled to be 95-100 ℃, and the amount of steam introduced into the extraction container is controlled.
Further, in the step (3), the pressure of the introduced steam is controlled to be 0.05mpa or less, preferably 0.02 to 0.04mpa, more preferably 0.03 mpa. The pressure is too large to generate pressure in the tank, the volatile oil can not be volatilized, the medicinal materials can be damaged, the water outlet speed is high, the collected water is mainly water, and the target oil components can not be separated.
Further, in step (3), collecting the volatile oil with a clean jar.
Further, in the step (3), the volatile oil is extracted under reflux for 6 to 12 hours, and the optimal time is 8 hours (the time is long and no volatile oil is increased).
Further, in the step (3), the pressure of condensed water used for condensation is more than or equal to 0.2MPa, and the temperature of the condensed water is 15-20 ℃. Research shows that the pressure and the temperature of condensed water are reasonably controlled, so that the purity of the volatile oil obtained by condensation is higher, and the yield of the volatile oil is considered at the same time. The temperature of the condensed water is too low, the volatile oil contains more impurities, and the yield of the volatile oil is influenced due to the too high temperature of the condensed water.
And (3) before introducing steam to the bottom of the extraction container, opening a circulating water switch of the volatile oil extractor, opening an air inlet valve of the volatile oil extractor, and controlling valves of pipelines on the volatile oil extractor.
The embodiment has the following beneficial effects:
1. in the embodiment, the angelica is dried in the shade, so that the technical problem of low extraction rate of the angelica volatile oil due to the loss of the angelica volatile oil caused by traditional sun drying, baking and the like is solved;
2. in the embodiment, the angelica and the fingered citron are cut into pieces with proper thickness, so that the volatile oil components are not damaged, the damage and the loss of the volatile oil components are avoided, and the extraction rate of the volatile oil is improved;
3. in the embodiment, the angelica and the fingered citron are mixed to extract the volatile oil, so that a synergistic effect can be generated, and the extraction rate and the purity of the volatile oil of the two raw materials are improved;
4. in the embodiment, the decoction pieces are soaked by using water with a proper dosage and combined with proper soaking time, so that the loss of the volatile oil is reduced to the minimum, and the extraction rate of the volatile oil is improved;
5. in the embodiment, the soaked decoction pieces are directly dry-steamed by steam, and the pressure of the steam, the temperature of condensed water and the pressure are controlled, so that the extraction rate of the volatile oil is improved. Research shows that if Chinese angelica and fingered citron decoction pieces are directly extracted, the extraction rate of volatile oil is low, the oil yield is low, and target components cannot be obtained.
6. The method is suitable for industrial large-scale production.
In each example, the content of volatile oil in the raw material angelica sinensis is determined to be 0.5% (ml/g), and the content of volatile oil in the fingered citron is determined to be 0.2% (ml/g).
Example 1
The method for extracting the mixed volatile oil of angelica and fingered citron comprises the following steps:
(1) preparing raw materials of angelica and fingered citron:
taking fresh angelica, removing impurities, drying in the shade, and cutting into pieces with the thickness of 0.3-0.8 cm to obtain angelica decoction pieces for later use; taking the original dry fingered citron medicinal materials, removing impurities, and cutting into pieces with the thickness of 0.3-0.8 cm to obtain fingered citron decoction pieces for later use;
the angelica raw material is dried in the shade, washing and solarization are not needed, and volatile oil can be lost through washing, solarization and drying.
(2) Extraction: weighing 128kg of angelica decoction pieces and 64kg of fingered citron decoction pieces, mixing, putting into a multifunctional extraction tank of an extraction container, adding 256kg of water for wetting (the medicinal materials can be covered on the water surface), soaking for 15min, discharging excessive water, and leaving the soaked angelica decoction pieces and fingered citron decoction pieces in the extraction container;
the soaking time is too long, volatile oil in the decoction pieces can be dissolved and taken away, and the yield of the obtained volatile oil can be influenced. The soaking time is too short, the decoction pieces cannot be fully soaked, so that volatile oil in the decoction pieces cannot be extracted, and the yield is also influenced.
In the embodiment, the angelica sinensis decoction pieces and the fingered citron decoction pieces are mixed and put into an extraction container to extract the volatile oil, and the extraction rate and the purity of the obtained volatile oil are higher.
(3) Introducing steam from the bottom of the extraction container, directly dry-steaming the soaked angelica sinensis decoction pieces and the soaked fingered citron decoction pieces, controlling the temperature in the multifunctional extraction tank of the extraction container to be 98 ℃ by controlling the amount of the steam introduced into the extraction container, controlling the pressure of the introduced steam to be 0.05mpa after the steam and the volatile oil in the multifunctional extraction tank of the extraction container enter the volatile oil extractor and are condensed to generate stable condensate, extracting the volatile oil for 6 hours under reflux, collecting the volatile oil, and finishing oil extraction.
In the step (3), the pressure of condensed water used for condensation is 0.2MPa, and the temperature of the condensed water is 15-17 ℃. Research shows that the pressure and the temperature of condensed water are reasonably controlled, so that the purity of the volatile oil obtained by condensation is higher, and the yield of the volatile oil is considered at the same time. The temperature of the condensed water is too low, the volatile oil contains more impurities, and the yield of the volatile oil is influenced due to the too high temperature of the condensed water.
And (3) before introducing steam to the bottom of the extraction container, opening a circulating water switch of the volatile oil extractor, opening an air inlet valve of the volatile oil extractor, and controlling each pipeline valve on the volatile oil extractor.
In this example, 578ml of angelica and fingered citron volatile oil is collected. The obtained volatile oil is light yellow transparent uniform oily matter, and the extraction rate of the volatile oil is 75.3%.
Example 2
The method for extracting the mixed volatile oil of angelica and fingered citron comprises the following steps:
(1) preparing raw materials of angelica and fingered citron:
taking fresh angelica, removing impurities, drying in the shade, and cutting into pieces with the thickness of 0.3-0.8 cm to obtain angelica decoction pieces for later use; taking the original dry fingered citron medicinal materials, removing impurities, and cutting into pieces with the thickness of 0.3-0.8 cm to obtain fingered citron decoction pieces for later use;
the angelica raw material is dried in the shade, washing and solarization are not needed, and volatile oil can be lost through washing, solarization and drying.
(2) Extraction: weighing 128kg of angelica decoction pieces and 128kg of fingered citron decoction pieces, mixing, putting into a multifunctional extraction tank of an extraction container, adding 256kg of wetting water (the water surface covers the medicinal materials), wetting for 15min, discharging excessive water, and leaving the wetted angelica decoction pieces and the wetted fingered citron decoction pieces in the multifunctional extraction tank of the extraction container;
according to the invention, the angelica sinensis decoction pieces and the fingered citron decoction pieces are mixed and put into an extraction container to extract the volatile oil, and the extraction rate and the purity of the obtained volatile oil are higher.
(3) Introducing steam from the bottom of the multifunctional extraction tank of the extraction container, directly dry-steaming the soaked angelica slices and the soaked fingered citron slices, controlling the temperature in the multifunctional extraction tank of the extraction container to be 100 ℃, controlling the pressure of the introduced steam to be 0.03mpa after the steam and the volatile oil in the extraction container enter a volatile oil extractor and generate stable condensate after condensation, extracting the volatile oil for 6 hours by reflux, collecting the volatile oil by using a clean jar, and finishing oil extraction.
In the step (3), the pressure of condensed water used for condensation is 0.2MPa, and the temperature of the condensed water is 16-18 ℃. Research shows that the pressure and the temperature of condensed water are reasonably controlled, so that the purity of the volatile oil obtained by condensation is higher, and the yield of the volatile oil is considered at the same time. The temperature of the condensed water is too low, the volatile oil contains more impurities, and the yield of the volatile oil is influenced due to the too high temperature of the condensed water.
And (3) before introducing steam to the bottom of the extraction container, opening a circulating water switch of the volatile oil extractor, opening an air inlet valve of the volatile oil extractor, and controlling each pipeline valve on the volatile oil extractor.
In this example, 690ml of angelica and fingered citron volatile oil are collected. The obtained volatile oil is light yellow transparent uniform oily matter, and the extraction rate of the volatile oil is 77.0%.
Example 3
The method for extracting the mixed volatile oil of angelica and fingered citron comprises the following steps:
(1) preparing raw materials of angelica and fingered citron:
taking fresh angelica, removing impurities, drying in the shade, and cutting into pieces with the thickness of 0.3-0.8 cm to obtain angelica decoction pieces for later use; taking the original dry fingered citron medicinal materials, removing impurities, and cutting into pieces with the thickness of 0.3-0.8 cm to obtain fingered citron decoction pieces for later use;
the angelica raw material is dried in the shade, washing and solarization are not needed, and volatile oil can be lost through washing, solarization and drying.
(2) Extraction: weighing 128kg of angelica decoction pieces and 128kg of fingered citron decoction pieces, mixing, putting into a multifunctional extraction tank of an extraction container, adding 256kg of water for wetting (the medicinal materials are covered on the water surface), draining excessive water after soaking for 10min, and leaving the soaked angelica decoction pieces and fingered citron decoction pieces in the extraction container;
according to the invention, the angelica sinensis decoction pieces and the fingered citron decoction pieces are mixed and put into an extraction container to extract the volatile oil, and the extraction rate and the purity of the obtained volatile oil are higher.
(3) Introducing steam from the bottom of the extraction container, directly dry-steaming the soaked angelica sinensis decoction pieces and the soaked fingered citron decoction pieces, controlling the temperature in the extraction container to be 100 ℃ by controlling the amount of the steam introduced into the extraction container, controlling the pressure of the introduced steam to be 0.03mpa after the steam and the volatile oil in the extraction container enter a volatile oil extractor and generate stable condensate after condensation, extracting the volatile oil for 8 hours by reflux, collecting the volatile oil by using a clean wide-mouth bottle, and finishing oil extraction.
In the step (3), the pressure of condensed water used for condensation is 0.2MPa, and the temperature of the condensed water is 15-17 ℃. Research shows that the pressure and the temperature of condensed water are reasonably controlled, so that the purity of the volatile oil obtained by condensation is higher, and the yield of the volatile oil is considered at the same time. The temperature of the condensed water is too low, the volatile oil contains more impurities, and the yield of the volatile oil is influenced due to the too high temperature of the condensed water.
And (3) before introducing steam to the bottom of the extraction container, opening a circulating water switch of the volatile oil extractor, opening an air inlet valve of the volatile oil extractor, and controlling each pipeline valve on the volatile oil extractor.
In the present example, 760ml of angelica and fingered citron volatile oil is collected. The obtained volatile oil is light yellow transparent uniform oily matter, and the extraction rate of the volatile oil is 84.8%.
Comparative example 1
This comparative example differs from example 3 in that the reflux extraction time was 13 hours, and is otherwise the same as example 3.
In the comparative example, the extraction rate of the mixed volatile oil of the angelica and the fingered citron is 82.2 percent. Therefore, the extraction rate of the mixed volatile oil cannot be increased by prolonging the extraction time.
Comparative example 2
The comparative example is different from example 3 in that angelica dried at 60 ℃ is used, and the rest is the same as example 3.
In the comparative example, the yield of the mixed volatile oil of the angelica and the fingered citron is only 0.15 percent. The process is indicated by yield rate because of different treatment modes of the medicinal materials.
Comparative example 3
This comparative example is different from example 3 in that the thickness of the cut piece was 2cm, and the others were the same as example 3.
In the comparative example, the extraction rate of the mixed volatile oil of the angelica and the fingered citron is 68.7 percent. Therefore, the extraction rate of the mixed volatile oil is reduced by increasing the thickness of the medicinal materials.
The result of the detection
The volatile oil obtained in the embodiment of the invention is subjected to performance detection, and the detection result is as follows:
1. the characteristics are as follows: the product is light yellow or yellowish brown transparent uniform oily liquid, and has good fragrance.
2. And (3) identification: taking a proper amount of the product, adding 1ml of ethanol, shaking and dissolving to obtain a test solution. Another 1g of the control medicinal materials of angelica and fingered citron are prepared into the control medicinal solution by the same method. According to the test of thin layer chromatography operating procedure, 10-20 μ l of the test solution and 5 μ l of each of the radix Angelicae sinensis and fructus Citri Sarcodactylis reference solution are respectively spotted on the same silica gel G thin layer plate, and normal hexane is used: spreading ethyl acetate (9:1) as developing agent, sun drying, and viewing under ultraviolet lamp (365 nm). In the chromatogram of the test solution, fluorescent spots with the same color appear at the corresponding positions of the chromatogram of the reference solution.
FIG. 1 is a diagram showing the results of thin layer chromatography of the volatile oil obtained in preferred embodiment 1 of the present invention and a reference drug;
in the figure, 10 mul of single sample is a thin-layer chromatography result obtained by taking 10 mul of sample solution of the test article, 5 mul of fingered citron is a thin-layer chromatography result obtained by taking 5 mul of fingered citron contrast medicinal material solution, 5 mul of angelica is a thin-layer chromatography result obtained by taking 5 mul of angelica contrast medicinal material solution, and 20 mul of double sample is a thin-layer chromatography result obtained by taking 20 mul of sample solution of the test article.
FIG. 2 is a thin-layer chromatography result chart of the volatile oil obtained in the preferred embodiments 2 and 3 of the present invention and the reference drug.
Wherein 0.01g, 0.1g is a sampling amount, 0.01g is double, 0.1g is double and is a thin-layer chromatography result obtained by spotting 20 mul, 0.01g, 0.1g 10 mul are thin-layer chromatography results obtained by spotting 10 mul, the angelica contrast medicinal material is a thin-layer chromatography result obtained by spotting 5 mul of angelica contrast medicinal material solution, and the fingered citron contrast medicinal material is a thin-layer chromatography result obtained by spotting 5 mul of fingered citron contrast medicinal material solution. Wherein the right side is a thin-layer chromatography result chart of the volatile oil obtained in example 2, and the left side is a thin-layer chromatography result chart of the volatile oil obtained in example 3.
The identification result shows that the method can effectively extract the volatile oil in the angelica and the fingered citron, the extraction rate of the volatile oil reaches more than 75 percent, and the method can be applied to the industrial production of the mixed volatile oil of the angelica and the fingered citron.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The method for extracting the mixed volatile oil of the angelica and the fingered citron is characterized by comprising the following steps:
(1) preparing raw materials of angelica and fingered citron:
removing impurities from fresh radix Angelicae sinensis, drying in the shade, and slicing to obtain radix Angelicae sinensis decoction pieces; taking dried fingered citron raw medicinal materials, removing impurities, and slicing to obtain fingered citron decoction pieces for later use;
(2) extraction: weighing radix Angelicae sinensis decoction pieces and fructus Citri Sarcodactylis decoction pieces, mixing, adding wetting amount of water, wetting, draining off excessive water after soaking for a period of time, and placing the soaked radix Angelicae sinensis decoction pieces and fructus Citri Sarcodactylis decoction pieces in an extraction container;
(3) introducing steam from the bottom of the extraction container, directly dry-steaming the soaked radix Angelicae sinensis decoction pieces and fructus Citri Sarcodactylis decoction pieces, controlling the temperature in the extraction container, controlling the pressure of the introduced steam when the steam and volatile oil in the extraction container volatilize into the volatile oil extractor, condensing to generate stable condensate, reflux-extracting volatile oil, collecting volatile oil, and finishing oil extraction.
2. The method for extracting the mixed volatile oil of the angelica and the fingered citron according to claim 1, wherein in the step (1), the angelica and the fingered citron are sliced by a medicine slicing machine, and the thickness of the slices is 0.3cm to 0.8 cm.
3. The method for extracting the mixed volatile oil of the angelica and the fingered citron according to claim 1 or 2, wherein in the step (2), the mass ratio of the angelica decoction pieces to the fingered citron decoction pieces is 1: 0.5-1.5; and/or
In the step (2), the extraction container is a multifunctional extraction tank.
4. The method for extracting the mixed volatile oil of the angelica and the fingered citron as claimed in claim 3, wherein the mass ratio of the angelica decoction pieces to the fingered citron decoction pieces is 1: 0.8-1.2.
5. The method for extracting the mixed volatile oil of angelica and fingered citron according to claim 1 or 2, wherein in the step (2), the wet water is just covered by the medicinal materials on the water surface, and/or
In the step (2), the soaking time is 5-30 min.
6. The method for extracting the mixed volatile oil of angelica sinensis and fingered citron according to claim 5, wherein in the step (2), the amount of the wetting water is 0.5 to 1.5 times of the sum of the weight of the angelica sinensis decoction pieces and the weight of the fingered citron decoction pieces; and/or
In the step (2), the soaking time is 15 min.
7. The method for extracting the mixed volatile oil of the angelica and the fingered citron according to claim 1 or 2, wherein in the step (3), the temperature in the extraction container is controlled to be 95-100 ℃; and/or
In the step (3), the pressure of the introduced steam is controlled to be less than or equal to 0.05 mpa.
8. The method for extracting the mixed volatile oil of angelica and fingered citron according to claim 1 or 2, wherein in the step (3), the volatile oil is collected by a clean jar.
9. The method for extracting the mixed volatile oil of the angelica and the fingered citron according to claim 1 or 2, wherein in the step (3), the volatile oil is extracted under reflux for 6-12 hours.
10. The method for extracting the mixed volatile oil of the angelica and the fingered citron according to claim 1 or 2, wherein in the step (3), the pressure of condensed water used for condensation is more than or equal to 0.2MPa, and the temperature of the condensed water is 15-20 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110295643.3A CN113004975B (en) | 2021-03-19 | 2021-03-19 | Method for extracting mixed volatile oil of angelica and fingered citron |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110295643.3A CN113004975B (en) | 2021-03-19 | 2021-03-19 | Method for extracting mixed volatile oil of angelica and fingered citron |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113004975A true CN113004975A (en) | 2021-06-22 |
| CN113004975B CN113004975B (en) | 2022-08-02 |
Family
ID=76403129
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110295643.3A Active CN113004975B (en) | 2021-03-19 | 2021-03-19 | Method for extracting mixed volatile oil of angelica and fingered citron |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113004975B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87101266A (en) * | 1987-12-22 | 1988-09-28 | 金珍玉 | The manufacture method that contains 50% Radix Angelicae Sinensis volatile oil |
| CN1709329A (en) * | 2005-06-09 | 2005-12-21 | 武汉联绎生物科技有限公司 | Composition for treating female algomenorrhea and its preparing method |
| CN103931351A (en) * | 2013-01-18 | 2014-07-23 | 甘肃农业大学 | Angelica origin processing and quality-preservation package storage method |
| CN104523784A (en) * | 2014-12-26 | 2015-04-22 | 青岛文创科技有限公司 | Method for extracting Chinese angelica extract |
| CN105969526A (en) * | 2016-05-20 | 2016-09-28 | 中发实业集团业锐药业有限公司 | Extraction method of dalbergia odorifera volatile oil |
| CN107296819A (en) * | 2017-06-20 | 2017-10-27 | 王逸帆 | A kind of processing method for improving Chinese angelica volatile oil content |
| CN110801477A (en) * | 2019-11-22 | 2020-02-18 | 湖南安邦制药有限公司 | Preparation method of particles for stopping bleeding and regulating menstruation |
-
2021
- 2021-03-19 CN CN202110295643.3A patent/CN113004975B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87101266A (en) * | 1987-12-22 | 1988-09-28 | 金珍玉 | The manufacture method that contains 50% Radix Angelicae Sinensis volatile oil |
| CN1709329A (en) * | 2005-06-09 | 2005-12-21 | 武汉联绎生物科技有限公司 | Composition for treating female algomenorrhea and its preparing method |
| CN103931351A (en) * | 2013-01-18 | 2014-07-23 | 甘肃农业大学 | Angelica origin processing and quality-preservation package storage method |
| CN104523784A (en) * | 2014-12-26 | 2015-04-22 | 青岛文创科技有限公司 | Method for extracting Chinese angelica extract |
| CN105969526A (en) * | 2016-05-20 | 2016-09-28 | 中发实业集团业锐药业有限公司 | Extraction method of dalbergia odorifera volatile oil |
| CN107296819A (en) * | 2017-06-20 | 2017-10-27 | 王逸帆 | A kind of processing method for improving Chinese angelica volatile oil content |
| CN110801477A (en) * | 2019-11-22 | 2020-02-18 | 湖南安邦制药有限公司 | Preparation method of particles for stopping bleeding and regulating menstruation |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113004975B (en) | 2022-08-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101358158A (en) | Method for preparing fresh aromatic essential oil | |
| CN102559384A (en) | Method for extracting cinnamon oil | |
| KR101604158B1 (en) | Method for extracting materials and a device for implementing same | |
| CN109609276A (en) | A kind of extracting method of oil camphor tree leaf essential oil | |
| CN109135930B (en) | A method of using steam distillation-destructive distillation fir system for multiple product | |
| CN109504540A (en) | A kind of agilawood essential oil extracting method | |
| CN103194312A (en) | Method for extracting essential oil from cypress leaves | |
| CN109201025A (en) | A kind of regeneration method of petroleum-type spent bleaching clay | |
| CN108998205A (en) | A kind of lacquer tree seed nuclei benevolence olein smelting method | |
| CN205473649U (en) | Distillation apparatus for producing of agalloch eaglewood essential oil | |
| CN112111324A (en) | Extraction method of peony flower stock solution with low cost and high extraction efficiency | |
| CN108300568A (en) | A kind of production method of fir essential oil | |
| CN113004975B (en) | Method for extracting mixed volatile oil of angelica and fingered citron | |
| CN105419946B (en) | A kind of method that super-pressure joint steam distillation extracts Rosa Damascana | |
| CN112094699B (en) | Method for extracting camphor tree hydrosol | |
| CN113773908A (en) | Preparation method and application of jasmine extract with antioxidant activity | |
| CN103897799A (en) | Use of isopropyl acetate as leaching solvent in plant oil and fat leaching and oil and fat leaching method using isopropyl acetate | |
| Van Dries et al. | A simple method for detection of glycosidic bound monoterpenes and other volatile compounds occurring in fresh plant material | |
| Rayner et al. | Solvent extraction of aflatoxins from contaminated agricultural products | |
| CN102260145B (en) | Method for continuous fractional separation and purification of effective ingredients of star anise | |
| WO2020211562A1 (en) | Method for extracting volatile oil from cannabis and application of volatile oil | |
| CN106433988A (en) | Extraction method of cinnamon spices | |
| CN113637810A (en) | Large biological leather with functions of removing peculiar smell and absorbing formaldehyde | |
| CN208511920U (en) | A kind of movable plant essential oil extracting device | |
| CN109321366A (en) | A method of extracting wormwood hydrosol |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |