CN111205927A - Peony essential oil extraction method - Google Patents
Peony essential oil extraction method Download PDFInfo
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- CN111205927A CN111205927A CN202010045365.1A CN202010045365A CN111205927A CN 111205927 A CN111205927 A CN 111205927A CN 202010045365 A CN202010045365 A CN 202010045365A CN 111205927 A CN111205927 A CN 111205927A
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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
- C11B9/022—Refining
Abstract
The invention belongs to the technical field of plant extraction, and provides a peony essential oil extraction method, which comprises the following steps: s1, collecting fresh peony petals, cleaning, freezing, drying and crushing to obtain peony powder; s2, adding peony powder into the mixed solvent, and uniformly mixing to obtain a mixed material; the mixed solvent comprises the following components in parts by mass: 0.01-0.03 part of glacial acetic acid, 0.1-0.5 part of diethyl ether, 1.2-3.5 parts of polydimethylsiloxane and 2.5-6.2 parts of dichloromethane; s3, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 35-40 ℃, the extraction pressure is 25-30 MPa, the flow rate is 22-25 kg/h, and the extraction time is 1-1.5 h; s4, separating the extracted carbon dioxide fluid, wherein the flow rate of the carbon dioxide fluid is 5-13 kg/h, the pressure of the separator is 6-7 MPa, the temperature is 38-42 ℃, extracting for 1.5-2.5 h, discharging the extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil. Through above-mentioned technical scheme, solved prior art and extracted the low problem of peony essential oil productivity.
Description
Technical Field
The invention belongs to the technical field of plant extraction, and relates to a method for extracting peony essential oil.
Background
Peony is deciduous wild shrub in Ranunculaceae and Paeonia, is an important ornamental flower in China, and is endowed with elegant appearance, beautiful natural fragrance, king in flowers and other beautiful connotations by people with various varieties, beautiful flower postures, large and bright flowers and magnificent tangkuang. At present, the places such as Shandong, Shaanxi, Hebei, Anhui, Henan, Sichuan and the like are mainly at home. Due to the limitation of flowering phase, climate condition and backward deep processing technology, a large amount of peony flowers are wasted in vain every year. Therefore, the comprehensive development and application of the peony flowers become a hot point of research in recent years.
The peony essential oil is volatile oily liquid extracted and separated from peony, and most of volatile components in the peony oily liquid are substances with fragrance such as flower fragrance, fruit fragrance and the like. In addition, the peony essential oil is rich in various amino acids and trace elements required by human bodies, has the effects of resisting sensitivity, improving blood circulation, maintaining beauty and keeping young, promoting cell regeneration, relieving skin aging, regulating skin problems, balancing hormone secretion in females and the like, and can be used as a raw material of medicines, foods, beverages and cosmetics.
At present, the extraction and separation techniques of plant essential oil mainly include steam distillation, solvent extraction, microwave extraction, ultrasonic extraction, supercritical fluid extraction, and the like. The supercritical carbon dioxide extraction method is a new essential oil extraction technology, and compared with the traditional chemical extraction method, the supercritical carbon dioxide extraction method not only has high extraction efficiency and high purity of extracted essential oil, but also maximally preserves active ingredients of the essential oil. The supercritical carbon dioxide extraction method is mainly used for preparing essential oil by taking dried flowers as raw materials, and if fresh flowers are taken as raw materials, the extract obtained by extraction contains water, and oil-water separation is also needed to obtain pure essential oil. The dried flowers are generally obtained by drying fresh flowers, while volatile components in the flowers are greatly lost in the drying process, and the yield of the essential oil prepared from the dried flowers is lower than that of the essential oil prepared from the fresh flowers.
Disclosure of Invention
The invention provides a method for extracting peony essential oil, which solves the problem of low yield of peony essential oil extracted in the prior art.
The technical scheme of the invention is realized as follows:
a peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freezing, drying and crushing to obtain peony powder;
s2, adding peony powder into the mixed solvent, and uniformly mixing to obtain a mixed material; the mixed solvent comprises the following components in parts by mass: 0.01-0.03 part of glacial acetic acid, 0.1-0.5 part of diethyl ether, 1.2-3.5 parts of polydimethylsiloxane and 2.5-6.2 parts of dichloromethane;
s3, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 35-40 ℃, the extraction pressure is 25-30 MPa, the flow rate is 22-25 kg/h, and the extraction time is 1-1.5 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow rate of the carbon dioxide fluid is 5-13 kg/h, the pressure of the separator is 6-7 MPa, the temperature is 38-42 ℃, extracting for 1.5-2.5 h, discharging the extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
As a further technical scheme, the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.02 parts, diethyl ether 0.3 parts, polydimethylsiloxane 0.5 parts and dichloromethane 4.4 parts.
According to a further technical scheme, the mass ratio of the mixed solvent to the peony pollen is (1.7-3): 10.
as a further technical scheme, the mass ratio of the mixed solvent to the peony pollen is 2.3: 10.
as a further technical scheme, the freeze-drying temperature in the step S1 is-10 ℃ to-25 ℃.
The working principle and the beneficial effects of the invention are as follows:
1. according to the invention, the peony essential oil is extracted from peony petals by a supercritical carbon dioxide extraction method, before extraction, the cleaned peony petals are firstly frozen, dried and crushed into peony powder, so that volatile components in the peony petals can be well preserved, the extraction rate is improved, then the peony powder is firstly mixed with a mixed solvent, and then the supercritical carbon dioxide extraction is carried out, so that the extraction rate of the peony essential oil is obviously improved, and the yield of the peony essential oil is improved; in addition, the peony essential oil obtained by extraction has good physicochemical indexes, so that the extraction method provided by the invention improves the yield of the peony essential oil, ensures the quality of the peony essential oil, and effectively solves the problem of low yield of the peony essential oil extracted in the prior art.
2. According to the invention, the mixed solvent consists of glacial acetic acid, diethyl ether, polydimethylsiloxane and dichloromethane, and the glacial acetic acid is added to create an acidic environment for the mixed system, so that the mixed solvent is compatible with other solvents, and the extraction rate of the peony essential oil is obviously improved; the mutual compatibility of the diethyl ether, the polydimethylsiloxane and the dichloromethane well removes phthalate compounds in the peony essential oil, and the content of the phthalate compounds in the peony essential oil is remarkably reduced, so that the extracted peony essential oil is purer and has better quality.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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 1
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freeze-drying at-16 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 2.3: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.01 part, ethyl ether 0.1 part, polydimethylsiloxane 1.2 parts and dichloromethane 2.5 parts;
s3, performing continuous cyclic extraction on the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 27MPa, the flow rate is 23kg/h, and the extraction time is 1.2 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 10kg/h, the pressure of a separator is 6.5MPa, the temperature is 40 ℃, extracting for 2h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
Example 2
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freeze-drying at-16 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 2.3: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.03 part, ethyl ether 0.5 part, polydimethylsiloxane 3.5 parts and dichloromethane 6.2 parts;
s3, performing continuous cyclic extraction on the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 27MPa, the flow rate is 23kg/h, and the extraction time is 1.2 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 10kg/h, the pressure of a separator is 6.5MPa, the temperature is 40 ℃, extracting for 2h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
Example 3
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freeze-drying at-16 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 2.3: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.02 parts, diethyl ether 0.3 parts, polydimethylsiloxane 0.5 parts and dichloromethane 4.4 parts;
s3, performing continuous cyclic extraction on the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 27MPa, the flow rate is 23kg/h, and the extraction time is 1.2 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 10kg/h, the pressure of a separator is 6.5MPa, the temperature is 40 ℃, extracting for 2h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
Example 4
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freeze-drying at-16 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 1.7: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.02 parts, diethyl ether 0.3 parts, polydimethylsiloxane 0.5 parts and dichloromethane 4.4 parts;
s3, performing continuous cyclic extraction on the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 27MPa, the flow rate is 23kg/h, and the extraction time is 1.2 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 10kg/h, the pressure of a separator is 6.5MPa, the temperature is 40 ℃, extracting for 2h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
Example 5
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freeze-drying at-16 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 3: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.02 parts, diethyl ether 0.3 parts, polydimethylsiloxane 0.5 parts and dichloromethane 4.4 parts;
s3, performing continuous cyclic extraction on the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 27MPa, the flow rate is 23kg/h, and the extraction time is 1.2 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 10kg/h, the pressure of a separator is 6.5MPa, the temperature is 40 ℃, extracting for 2h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
Example 6
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freeze-drying at-10 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 2.3: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.02 parts, diethyl ether 0.3 parts, polydimethylsiloxane 0.5 parts and dichloromethane 4.4 parts;
s3, performing continuous cyclic extraction on the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 27MPa, the flow rate is 23kg/h, and the extraction time is 1.2 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 10kg/h, the pressure of a separator is 6.5MPa, the temperature is 40 ℃, extracting for 2h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
Example 7
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freeze-drying at-25 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 2.3: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.02 parts, diethyl ether 0.3 parts, polydimethylsiloxane 0.5 parts and dichloromethane 4.4 parts;
s3, performing continuous cyclic extraction on the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 27MPa, the flow rate is 23kg/h, and the extraction time is 1.2 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 10kg/h, the pressure of a separator is 6.5MPa, the temperature is 40 ℃, extracting for 2h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
Example 8
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freezing and drying at-16 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 2.3: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.02 parts, diethyl ether 0.3 parts, polydimethylsiloxane 0.5 parts and dichloromethane 4.4 parts;
s3, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 35 ℃, the extraction pressure is 30MPa, the flow rate is 22kg/h, and the extraction time is 1.5 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 5kg/h, the pressure of a separator is 6MPa, the temperature is 42 ℃, extracting for 1.5h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
Example 9
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freezing and drying at-16 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 2.3: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.02 parts, diethyl ether 0.3 parts, polydimethylsiloxane 0.5 parts and dichloromethane 4.4 parts;
s3, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 25MPa, the flow rate is 25kg/h, and the extraction time is 1 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow rate of the carbon dioxide fluid is 13kg/h, the pressure of a separator is 7MPa, the temperature is 38 ℃, extracting for 2.5h, discharging an extract from the bottom of the separator, standing, and carrying out oil-water separation to obtain the peony essential oil.
Comparative example 1
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, drying at 60 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 2.3: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.02 parts, diethyl ether 0.3 parts, polydimethylsiloxane 0.5 parts and dichloromethane 4.4 parts;
s3, performing continuous cyclic extraction on the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 27MPa, the flow rate is 23kg/h, and the extraction time is 1.2 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 10kg/h, the pressure of a separator is 6.5MPa, the temperature is 40 ℃, extracting for 2h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
Comparative example 2
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freeze-drying at-16 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 2.3: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: 0.3 part of diethyl ether, 0.5 part of polydimethylsiloxane and 4.4 parts of dichloromethane;
s3, performing continuous cyclic extraction on the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 27MPa, the flow rate is 23kg/h, and the extraction time is 1.2 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 10kg/h, the pressure of a separator is 6.5MPa, the temperature is 40 ℃, extracting for 2h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
Comparative example 3
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freeze-drying at-16 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 2.3: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.02 parts, polydimethylsiloxane 0.5 parts and dichloromethane 4.4 parts;
s3, performing continuous cyclic extraction on the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 27MPa, the flow rate is 23kg/h, and the extraction time is 1.2 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 10kg/h, the pressure of a separator is 6.5MPa, the temperature is 40 ℃, extracting for 2h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
Comparative example 4
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freeze-drying at-16 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 2.3: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.02 parts, ethyl ether 0.3 parts and dichloromethane 4.4 parts;
s3, performing continuous cyclic extraction on the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 27MPa, the flow rate is 23kg/h, and the extraction time is 1.2 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 10kg/h, the pressure of a separator is 6.5MPa, the temperature is 40 ℃, extracting for 2h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
Comparative example 5
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freeze-drying at-16 ℃, and crushing to obtain peony powder;
s2, adding peony powder into a mixed solvent, wherein the mass ratio of the mixed solvent to the peony powder is 2.3: 10, uniformly mixing to obtain a mixed material;
the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.02 parts, ethyl ether 0.3 parts and polydimethylsiloxane 0.5 parts;
s3, performing continuous cyclic extraction on the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 27MPa, the flow rate is 23kg/h, and the extraction time is 1.2 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 10kg/h, the pressure of a separator is 6.5MPa, the temperature is 40 ℃, extracting for 2h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
Comparative example 6
A peony essential oil extraction method comprises the following steps:
s1, collecting fresh peony petals, cleaning, freeze-drying at-16 ℃, and crushing to obtain peony powder;
s2, adding peony pollen into n-hexane, wherein the mass ratio of the n-hexane to the peony pollen is 2.3: 10, uniformly mixing to obtain a mixed material;
s3, performing continuous cyclic extraction on the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 27MPa, the flow rate is 23kg/h, and the extraction time is 1.2 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow of the carbon dioxide fluid is 10kg/h, the pressure of a separator is 6.5MPa, the temperature is 40 ℃, extracting for 2h, discharging an extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
The peony powder and the obtained peony essential oil in the extraction methods of examples 1 to 9 and comparative examples 1 to 6 were weighed, and the extraction rate was calculated according to the following formula:
extraction rate/% (essential oil mass/g)/(peony pollen mass/g) × 100
The results are shown in the following table:
TABLE 1 extraction rates of the extraction methods of examples 1 to 9 and comparative examples 1 to 6
As can be seen from the above table, in the extraction methods of examples 1 to 9 and comparative examples 1 to 6, the extraction rate of the extraction methods of examples 1 to 9 is as high as 1.81% to 1.85%, and compared with the extraction methods of comparative examples 1 to 6, the extraction rate is significantly improved, wherein the extraction rate of the extraction method of example 3 is the highest and is as high as 1.85%, and the extraction rate is improved by 9.47 to 22.52% compared with the extraction methods of comparative examples 1 to 6. Compared with the extraction method of the embodiment 3, the extraction method of the comparative examples 1 to 6 is different in that: the extraction method of comparative example 1, in step S1, peony petals were washed and then dried at 60 ℃ instead of freeze-drying; the mixed solvent in the extraction method of comparative example 2, step S2, does not include glacial acetic acid; the mixed solvent in the extraction method of comparative example 3, step S2, does not include diethyl ether; the organic solvent in step S2 of the extraction method of comparative example 4 does not include polydimethylsiloxane; the organic solvent in step S2 of the extraction process of comparative example 5 does not include dichloromethane; the organic solvent in step S2 of the extraction method of comparative example 6 is n-hexane; in the method for extracting peony essential oil, firstly, the cleaned peony petals are freeze-dried, so that volatile components in the peony petals can be well preserved, and the extraction rate is improved; before extraction, peony powder is mixed with a mixed solvent, and then supercritical carbon dioxide extraction is carried out, wherein the mixed solvent consists of glacial acetic acid, diethyl ether, polydimethylsiloxane and dichloromethane, the glacial acetic acid is added, an acidic environment is created for a mixed system, and the peony powder and other solvents are compatible with each other, so that the extraction rate of peony essential oil is remarkably improved.
The following physicochemical index tests were performed on the peony essential oil obtained by the extraction methods of examples 1 to 9 and comparative examples 1 to 6:
(1) fragrance: evaluating the fragrance of the peony essential oil according to a method specified in GB/T14454.2-2008 & lt perfume fragrance evaluation method & gt; the aroma assessment results are expressed in scores: the score of 39.1-40.0 represents pure, the score of 36.0-39.0 represents pure, and the score of 32.0-35.9 represents pure; 28.0 to 31.9 points of the total amount of the composition; 24.0-27.9 points represent passing; a score of 24.0 or less indicates a failure;
(2) color: inspecting the color of the peony essential oil according to a method specified in GB/T14454.3-2008 'perfume color inspection method';
(3) refractive index: testing the refractive index of the peony essential oil according to the method specified in GB/T14454.4-2008 'determination of refractive index of spice';
(4) optical rotation: testing the optical rotation of the peony essential oil according to a method specified in GB/T14454.5-2008 'determination of optical rotation of spice';
(5) relative density: testing the relative density of the peony essential oil according to the method specified in GB/T11540-;
the test results are given in the following table:
TABLE 2 physicochemical indices of the extracted peony essential oils of examples 1 to 9 and comparative examples 1 to 6
The data in the table show that the peony essential oil obtained by the extraction method of the embodiments 1-9 is yellow clear liquid, the smell is pure, and the physicochemical indexes such as the refractive index, the optical rotation and the relative density meet the standard, which indicates that the peony essential oil obtained by the extraction method of the invention has good physicochemical indexes.
The peony essential oils extracted in examples 1 to 9 and comparative examples 1 to 6 were subjected to GC-MS analysis by using a gas chromatography-tandem mass spectrometry (GC-MS) detector, and were subjected to quantitative treatment by using an area normalization method, and the total content of phthalate compounds (dimethyl phthalate, diethyl phthalate, allyl ethyl phthalate, diisobutyl phthalate) in the peony essential oils extracted in examples 1 to 9 and comparative examples 1 to 6 is shown in the following table:
TABLE 3 content of phthalate-based compound in peony essential oil extracted in examples 1 to 9 and comparative examples 1 to 6
As can be seen from the above table, compared with the extraction methods of comparative examples 1 to 6, the content of the phthalate compounds in the peony essential oil obtained by the extraction methods of examples 1 to 9 is significantly reduced, which indicates that the extraction method of the present invention can significantly remove the phthalate compounds in the peony essential oil, so that the extracted peony essential oil is purer and better in quality.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The method for extracting peony essential oil is characterized by comprising the following steps:
s1, collecting fresh peony petals, cleaning, freezing, drying and crushing to obtain peony powder;
s2, adding peony powder into the mixed solvent, and uniformly mixing to obtain a mixed material; the mixed solvent comprises the following components in parts by mass: 0.01-0.03 part of glacial acetic acid, 0.1-0.5 part of diethyl ether, 1.2-3.5 parts of polydimethylsiloxane and 2.5-6.2 parts of dichloromethane;
s3, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 35-40 ℃, the extraction pressure is 25-30 MPa, the flow rate is 22-25 kg/h, and the extraction time is 1-1.5 h;
s4, separating the extracted carbon dioxide fluid, wherein the flow rate of the carbon dioxide fluid is 5-13 kg/h, the pressure of the separator is 6-7 MPa, the temperature is 38-42 ℃, extracting for 1.5-2.5 h, discharging the extract from the bottom of the separator, standing, and performing oil-water separation to obtain the peony essential oil.
2. The method for extracting peony essential oil according to claim 1, wherein the mixed solvent comprises the following components in parts by mass: glacial acetic acid 0.02 parts, diethyl ether 0.3 parts, polydimethylsiloxane 0.5 parts and dichloromethane 4.4 parts.
3. The peony essential oil extraction method according to claim 2, wherein the mass ratio of the mixed solvent to the peony pollen is (1.7-3): 10.
4. the method for extracting peony essential oil according to claim 3, wherein the mass ratio of the mixed solvent to the peony pollen is 2.3: 10.
5. the method for extracting peony essential oil according to claim 1, wherein the freeze-drying temperature in step S1 is from-10 ℃ to-25 ℃.
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