CN113652305A - Elaeagnus pungens essential oil extracted by supercritical carbon dioxide fluid and preparation method thereof - Google Patents
Elaeagnus pungens essential oil extracted by supercritical carbon dioxide fluid and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- 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
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Abstract
The invention provides an elaeagnus pungens essential oil extracted by supercritical carbon dioxide fluid and a preparation method thereof, belonging to the field of agricultural deep processing and comprising the following steps: step one, picking fresh thorny elaeagnus pungens branches, removing pedicels, and only taking flower parts; step two, drying the selected elaeagnus pungens flowers by low-temperature air blasting to obtain dried elaeagnus pungens flowers; step three, putting the dried elaeagnus pungens into a supercritical carbon dioxide extraction device for extraction to obtain primary extract of the elaeagnus pungens; step four, dewaxing the primary extract of the elaeagnus pungens at low temperature; step five, adding distilled water into the dewaxed primary extract of the elaeagnus pungens, and stirring and mixing to obtain a mixture; and step six, distilling and extracting the mixture to obtain the elaeagnus pungens essential oil. The elaeagnus pungens essential oil has the characteristics of high retention rate of natural components, few derivatives and no chemical solvent addition residue.
Description
Technical Field
The invention relates to the technical field of agricultural deep processing, in particular to an elaeagnus pungens flower essential oil extracted by supercritical carbon dioxide fluid and a preparation method thereof.
Background
The principle of the supercritical carbon dioxide extraction process is that the supercritical carbon dioxide has a special dissolving effect on certain special natural products, and the relation between the dissolving capacity and the density of the supercritical carbon dioxide, namely the influence of pressure and temperature on the dissolving capacity of the supercritical carbon dioxide is utilized to carry out the supercritical carbon dioxide extraction process. In the supercritical state, supercritical carbon dioxide is contacted with the substance to be separated, so that the components with different polarity, boiling point and molecular weight are selectively extracted in sequence. Of course, the extracts obtained corresponding to each pressure range cannot be single, but the conditions can be controlled to obtain the mixed components with the optimal proportion, then the supercritical fluid is changed into the common gas by the methods of pressure reduction and temperature rise, and the extracted substances are completely or basically precipitated, so that the separation and purification purposes are achieved, so that the supercritical fluid carbon dioxide extraction process is formed by the combination of extraction and separation.
The thorny elaeagnus fruit is also called ludu fruit, sparrow crisp, sweet lollipop, goat milk seed and the like, and is a plant which is mainly grown in Hubei, Hunan, Jiangsu, Zhejiang, Fujian and other places in China and has ornamental and medicinal values. The roots, leaves and fruits of the elaeagnus pungens can be used as medicines, and have very obvious effects of reducing blood sugar, reducing blood fat, resisting lipid oxidation, resisting inflammation, relieving pain and the like.
At present, roots, leaves and fruits of the elaeagnus pungens are mainly developed in the market, but flowers of the elaeagnus pungens are rarely developed, and the development of the roots, leaves and fruits of the elaeagnus pungens into a proper product has a remarkable significance.
Disclosure of Invention
The invention aims to provide a method for extracting elaeagnus pungens essential oil by using supercritical carbon dioxide fluid, which has the characteristics of high retention rate of natural components, few derivatives and no chemical solvent addition residue, and endows elaeagnus pungens with new value functions and full component utilization, so that technology and product quality guarantee are provided for production and related product development of the elaeagnus pungens essential oil, and high-quality development of the elaeagnus pungens industry is promoted.
The technical scheme of the invention is realized as follows:
the invention provides a method for extracting elaeagnus pungens essential oil by supercritical carbon dioxide fluid, which comprises the following steps:
step one, picking fresh thorny elaeagnus pungens branches, removing pedicels, and only taking flower parts;
step two, putting the selected elaeagnus pungens into a dryer, and carrying out low-temperature blast drying to obtain dried elaeagnus pungens;
step three, putting the dried elaeagnus pungens into a supercritical carbon dioxide extraction device for extraction to obtain primary extract of the elaeagnus pungens;
putting the primary extract of the elaeagnus pungens into a refrigeration house, and dewaxing at a low temperature to obtain elaeagnus pungens wax;
step five, adding distilled water into the dewaxed primary extract of the elaeagnus pungens, and stirring and mixing uniformly to obtain a mixture;
and step six, distilling and extracting the mixture to obtain a primary distilled extract, thus obtaining the elaeagnus pungens essential oil.
As a further improvement of the invention, in the step one, the picking time of the fresh flowers is 8-10 o' clock in the morning, the maturity is from the flower opening to the beginning, fresh and full flowers without diseases and insect pests are selected, and the temperature in the constant-temperature vehicle is not higher than 20 ℃. The flowers are gradually increased along with the maturity degree, and then the volatile substances are reduced, so that the maturity of the same batch of flowers is relatively stable at constant temperature, the components of the volatile substances are stable, and the essential oil components are stable.
As a further improvement of the method, in the second step, the drying temperature of the low-temperature air blast drying is 40-45 ℃, and the drying time is 15-30 minutes. Excessive water is drained through drying so as not to wither and shrink flowers, and enzymolysis of volatile substances in cells is suspended so as to prevent volatilization of substances such as ester olefins and the like and improve the yield.
As a further improvement of the method, in the third step, the extraction pressure in the supercritical carbon dioxide extraction device is 25-26 MPa, the extraction temperature is 40-45 ℃, and the extraction time is 2-3 h. The elaeagnus pungens flower is more delicate, the cell wall is thin, the substances are easily separated, and the essential oil is more easily extracted compared with other materials.
As a further improvement of the invention, the freezing temperature of the low-temperature dewaxing in the fourth step is-5 ℃; the freezing time was 30 minutes. The elaeagnus pungens contains certain wax, the wax easily influences the quality of essential oil, and the wax is removed through low-temperature solidification, so that the product purity is improved.
As a further improvement of the invention, the volume ratio of the primary extract of elaeagnus pungens to distilled water in the step five is 1: 8-1: 10.
As a further improvement of the method, the distillation and extraction temperature in the sixth step is 50-60 ℃.
The invention further protects the elaeagnus pungens essential oil prepared by the preparation method for extracting the elaeagnus pungens essential oil by using the supercritical carbon dioxide fluid.
The invention has the following beneficial effects:
(1) the thorny elaeagnus flowers are mainly produced in the middle and southeast areas of China, and Hunan of Hubei are main native areas. The used elaeagnus pungens flowers come from local places, do not have a transgenic technology, are natural and have no preservative, and have high quality;
(2) the flowers with the maturity from blossom opening to beginning are picked from 8-10 o' clock in the morning, so that the freshness of the flowers can be ensured, and meanwhile, the influence of insect pests can be reduced;
(3) the essential oil product of the elaeagnus pungens subjected to supercritical extraction can be stored for a long time, prevents the decomposition and deterioration of the active ingredients of the essential oil product, and can be widely applied to industries such as cosmetics and foods.
(4) The supercritical extraction can avoid the essential oil component of the elaeagnus pungens from being damaged, and the yield of effective components is improved. In ester components contained in the elaeagnus pungens, ethyl acetate is easy to volatilize and also easy to hydrolyze into acetic acid and ethanol, so that direct heating cannot be realized for the time, and the extraction of fatty acids by a common extraction method is less, so that the product purity can be effectively improved by adopting the extraction method provided by the invention.
(5) The thorny elaeagnus essential oil extracted by supercritical extraction has the following properties: the grape and melon fragrance oil has a yellowish green transparent oily liquid, a grape and melon-like base note, indole-like smell, slightly sweet honey fragrance, sweet amber paste fragrance, elegant fragrance such as balsam fragrance and green-honey fragrance.
The method comprises the steps of drying and dehydrating the elaeagnus pungens, and extracting and separating the dried and dehydrated elaeagnus pungens by supercritical carbon dioxide to obtain elaeagnus pungens essential oil and byproduct elaeagnus pungens wax; wherein the supercritical carbon dioxide extraction is carried out at a low temperature; and then, the natural components of the elaeagnus pungens essential oil can be effectively protected from being damaged through steam distillation, no chemical solvent is added, and the obtained high-quality elaeagnus pungens essential oil is natural, pollution-free and pure and rich in smell.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1A method for extracting essential oil from Elaeagnus pungens by supercritical carbon dioxide fluid extraction
The method specifically comprises the following steps:
step one, picking fresh thorny elaeagnus pungens branches, removing flower stalks in a pretreatment workshop, and only taking flower parts; the fresh flower picking time is 8-10 o' clock in the morning, the maturity is from blooming to blooming, fresh and full flowers without diseases and insect pests are selected, and the temperature in the constant temperature vehicle is not higher than 20 ℃;
step two, putting the selected elaeagnus pungens into a dryer, and carrying out low-temperature blast drying at the drying temperature of 45 ℃ for 30 minutes to obtain relatively dry elaeagnus pungens;
step three, putting the particles into a supercritical carbon dioxide extraction device for extraction, wherein the extraction pressure is 26MPa, the extraction temperature is 45 ℃, and the extraction time is 3 hours, so as to obtain a primary extract of the elaeagnus pungens;
putting the primary extract of the elaeagnus pungens into a refrigeration house, and performing low-temperature dewaxing at the freezing temperature of-5 ℃; freezing for 30 minutes to obtain elaeagnus pungens wax;
step five, adding distilled water into the dewaxed primary extract of the elaeagnus pungens, wherein the volume ratio of the primary extract of the elaeagnus pungens to the distilled water is 1:10, and stirring and mixing uniformly to obtain a mixture;
and step six, distilling and extracting the mixture at the temperature of 60 ℃ to obtain a primary distilled extract, thus obtaining the elaeagnus pungens essential oil.
The primary extract of the elaeagnus pungens obtained by the supercritical carbon dioxide extraction method has the oil yield of 0.45%. After the refrigeration dewaxing treatment, each 10g of the primary product of the elaeagnus pungens contains 0.67g of elaeagnus pungens wax, and the results of the contents of various compounds and the contents of the compounds in the distilled and extracted elaeagnus pungens essential oil are that the content of esters is highest (47.32%), the content of alkane is second (23.59%), olefins (17.23%), aromatics (4.69%), phenols (3.32%), acids (2.71%) and ketones (1.97%).
The thorny elaeagnus flowers are rich in esters, alkanes and olefins, the ester content is the octyl 4-methoxycinnamate with the largest content, the alkane content is the forty-two alkanes, the pentacosane, the hexacosane and the like with the largest content, and the olefin content is the germacrene D with the largest content. The most significant of the aromatic components is octyl 4-methoxycinnamate in the ester group. The octyl 4-methoxycinnamate has the following properties that colorless to light yellow viscous liquid is insoluble in water, is dissolved in organic solvents such as ethanol and the like, is suitable for being stored in a shade place in a sealed way, has a boiling point of 198 and 200 ℃, and has no carcinogenesis, mutagenic effect, teratogenic effect and developmental toxicity. Can be used for preparing skin care cosmetics such as sunscreen cream (cream, emulsion, liquid), etc., can effectively absorb ultraviolet rays in sunlight, and can prevent human skin from being sunburned, sunburning and ink-exposed, and is also a therapeutic medicine for treating light-induced dermatitis.
The content of the octyl 4-methoxycinnamate is the highest in the elaeagnus pungens, and is very low in the leaves of the elaeagnus pungens, so that the elaeagnus pungens have strong fragrance, and the leaves have almost no fragrance.
Example 2
Compared with the embodiment 1, the extraction pressure in the supercritical carbon dioxide extraction device is 50MPa, and other conditions are not changed. The acid substances are increased by 1.83%, and the obtained oil body is dark and slightly turbid.
Example 3
Compared with the embodiment 1, the extraction pressure in the supercritical carbon dioxide extraction device is 10MPa, and other conditions are not changed. The content of ester substances is increased by 11.25%, the content of alkane substances is reduced by 4.73%, the oil body is clear, and the smell is light.
Example 4
Compared with the example 1, the extraction temperature in the supercritical carbon dioxide extraction device is 50 ℃, and other conditions are not changed. The obtained product is basically unchanged, and the ester substances are reduced by 0.92 percent.
Example 5
Compared with the example 1, the extraction temperature in the supercritical carbon dioxide extraction device is 35 ℃, and other conditions are not changed. The ester substances are increased by 9.62 percent, the olefins are reduced by 1.86 percent, the alkanes are reduced by 1.53 percent, and the odor is light.
Example 6
Compared with the embodiment 1, the extraction time in the supercritical carbon dioxide extraction device is 4h, and other conditions are not changed. The acid substances are increased by 1.95 percent, and the oil body is slightly dark.
Example 7
Compared with the embodiment 1, the extraction time in the supercritical carbon dioxide extraction device is 2h, and other conditions are not changed. The esters are increased by 7.39 percent, the acids are less, and the oil body is more transparent. The smell was slightly less.
Comparative example 1
In comparison with example 1, no low temperature dewaxing step was performed, and the other conditions were not changed.
Step one, picking fresh thorny elaeagnus pungens branches, removing flower stalks in a pretreatment workshop, and only taking flower parts; the fresh flower picking time is 8-10 o' clock in the morning, the maturity is from blooming to blooming, fresh and full flowers without diseases and insect pests are selected, and the temperature in the constant temperature vehicle is not higher than 20 ℃;
step two, putting the selected elaeagnus pungens into a dryer, and carrying out low-temperature blast drying at the drying temperature of 45 ℃ for 30 minutes to obtain relatively dry elaeagnus pungens;
step three, putting the particles into a supercritical carbon dioxide extraction device for extraction, wherein the extraction pressure is 26MPa, the extraction temperature is 45 ℃, and the extraction time is 3 hours, so as to obtain a primary extract of the elaeagnus pungens;
step four, adding distilled water into the primary extract of the elaeagnus pungens, wherein the volume ratio of the primary extract of the elaeagnus pungens to the distilled water is 1:10, and stirring and mixing uniformly to obtain a mixture;
and step five, distilling and extracting the mixture at the temperature of 60 ℃ to obtain a primary distilled extract, thus obtaining the elaeagnus pungens essential oil.
The primary extract of the elaeagnus pungens obtained by the supercritical carbon dioxide extraction method has the oil yield of 0.45%. The essential oil of Elaeagnus pungens without distillation contains the following compounds with highest ester content and second alkane content, and then sequentially contains olefins, acids, aromatics, phenols and ketones.
Compared with the prior art, the method disclosed by the invention has the advantages that the elaeagnus pungens are dried and dehydrated, and then extracted and separated by supercritical carbon dioxide to obtain the elaeagnus pungens essential oil and the byproduct of the elaeagnus pungens waxy substance; wherein the supercritical carbon dioxide extraction is carried out at a low temperature; and then, the natural components of the elaeagnus pungens essential oil can be effectively protected from being damaged through steam distillation, no chemical solvent is added, and the obtained high-quality elaeagnus pungens essential oil is natural, pollution-free and pure and rich in smell. The extracted high-quality elaeagnus pungens essential oil has the characteristics of high retention rate of natural components, few derivatives and no chemical solvent addition residue. Endows the wild plant elaeagnus pungens with new value and function, and utilizes the full components efficiently, thereby providing technology and product quality assurance for the production of the elaeagnus pungens essential oil and the development of related products, and realizing the high-quality development of industries such as the elaeagnus pungens agriculture.
The invention has the following beneficial effects:
(1) the thorny elaeagnus flowers are mainly produced in the middle and southeast areas of China, and Hunan of Hubei are main native areas. The used elaeagnus pungens flowers come from local places, do not have a transgenic technology, are natural and have no preservative, and have high quality;
(2) the flowers with the maturity from blossom opening to beginning are picked from 8-10 am, so that the freshness of the flowers can be ensured, the influence of insect pests can be reduced, and the cleanness of essential oil raw materials can be ensured;
(3) the essential oil product of the elaeagnus pungens subjected to supercritical extraction can be stored for a long time, prevents the decomposition and deterioration of the active ingredients of the essential oil product, and can be widely applied to industries such as cosmetics and foods.
(4) The supercritical extraction can avoid the essential oil component of the elaeagnus pungens from being damaged, and the yield of effective components is improved. In ester components contained in the elaeagnus pungens, ethyl acetate is easy to volatilize and also easy to hydrolyze into acetic acid and ethanol, so that direct heating cannot be realized for the time, and the extraction of fatty acids by a common extraction method is less, so that the product purity can be effectively improved by adopting the extraction method provided by the invention.
(5) The thorny elaeagnus essential oil extracted by supercritical extraction has the following properties: the grape and melon fragrance oil has a yellowish green transparent oily liquid, a grape and melon-like base note, indole-like smell, slightly sweet honey fragrance, sweet amber paste fragrance, elegant fragrance such as balsam fragrance and green-honey fragrance.
The method comprises the steps of drying and dehydrating the elaeagnus pungens, and extracting and separating the dried and dehydrated elaeagnus pungens by supercritical carbon dioxide to obtain elaeagnus pungens essential oil and byproduct elaeagnus pungens wax; wherein the supercritical carbon dioxide extraction is carried out at a low temperature; and then, the natural components of the elaeagnus pungens essential oil can be effectively protected from being damaged through steam distillation, no chemical solvent is added, and the obtained high-quality elaeagnus pungens essential oil is natural, pollution-free and pure and rich in smell.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A preparation method for extracting elaeagnus pungens essential oil by supercritical carbon dioxide fluid is characterized by comprising the following steps:
step one, picking fresh thorny elaeagnus pungens branches, removing pedicels, and only taking flower parts;
step two, putting the selected elaeagnus pungens into a dryer, and carrying out low-temperature blast drying to obtain dried elaeagnus pungens;
step three, putting the dried elaeagnus pungens into a supercritical carbon dioxide extraction device for extraction to obtain primary extract of the elaeagnus pungens;
putting the primary extract of the elaeagnus pungens into a refrigeration house, and dewaxing at a low temperature to obtain elaeagnus pungens wax;
step five, adding distilled water into the dewaxed primary extract of the elaeagnus pungens, and stirring and mixing uniformly to obtain a mixture;
and step six, distilling and extracting the mixture to obtain a primary distilled extract, thus obtaining the elaeagnus pungens essential oil.
2. The preparation method for extracting the essential oil of the elaeagnus pungens with the supercritical carbon dioxide fluid according to claim 1, wherein in the step one, the picking time of the fresh flowers is 8-10 o' clock in the morning, the maturity is from blossom to blossom, fresh and full flowers without plant diseases and insect pests are selected, and the temperature in the constant-temperature vehicle is not higher than 20 ℃.
3. The preparation method for extracting the elaeagnus pungens essential oil by using the supercritical carbon dioxide fluid according to claim 1, wherein the drying temperature of the low-temperature air drying in the second step is 40-45 ℃, and the drying time is 15-30 minutes.
4. The preparation method for extracting the elaeagnus pungens essential oil by using the supercritical carbon dioxide fluid according to claim 1, wherein in the third step, the extraction pressure in the supercritical carbon dioxide extraction device is 25-26 MPa, the extraction temperature is 40-45 ℃, and the extraction time is 2-3 hours.
5. The method for preparing the essential oil of the elaeagnus pungens by supercritical carbon dioxide fluid extraction according to claim 1, wherein the freezing temperature of the low-temperature dewaxing in the fourth step is 0 to-5 ℃; the freezing time is 20-30 minutes.
6. The method for preparing the essential oil of the elaeagnus pungens by supercritical carbon dioxide fluid extraction according to claim 1, wherein the volume ratio of the primary extract of the elaeagnus pungens to the distilled water in the step five is 1: 8-1: 10.
7. The preparation method for extracting the elaeagnus pungens essential oil by using the supercritical carbon dioxide fluid according to claim 1, wherein the distillation and extraction temperature in the sixth step is 50-60 ℃.
8. An elaeagnus pungens essential oil obtained by the method for preparing elaeagnus pungens essential oil by supercritical carbon dioxide fluid extraction according to any one of claims 1 to 7.
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CN103087821A (en) * | 2013-01-15 | 2013-05-08 | 武汉工业学院 | Rice bran oil refining method for reserving oryzanol |
CN107488509A (en) * | 2016-06-13 | 2017-12-19 | 新疆恒远中汇科技开发有限公司 | Using supercritical CO2The method that fluids extraction extracts russianolive flower essential oil |
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