CN114395441A - Extraction method of peony pistil oil - Google Patents
Extraction method of peony pistil oil Download PDFInfo
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- CN114395441A CN114395441A CN202111526096.1A CN202111526096A CN114395441A CN 114395441 A CN114395441 A CN 114395441A CN 202111526096 A CN202111526096 A CN 202111526096A CN 114395441 A CN114395441 A CN 114395441A
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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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/106—Production of fats or fatty oils from raw materials by extracting using ultra-sounds
-
- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
-
- 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
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
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- 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)
- Microbiology (AREA)
- Cosmetics (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a method for extracting peony pistil oil, which comprises the following steps: drying peony pistils, crushing and sieving; weighing a certain amount of crushed and sieved peony pistils, putting the peony pistils into a filter paper bag, adding a certain amount of absolute ethyl alcohol, and carrying out ultrasonic treatment; adding the filter paper bag subjected to ultrasonic treatment and absolute ethyl alcohol into a Soxhlet extractor, heating in a water bath, and refluxing to extract peony stamen oil; collecting ethanol in a Soxhlet extractor, and concentrating under reduced pressure to obtain crude oil of peony pistil; adding a certain amount of distilled water into the peony pistil crude oil, distilling and refining, and then carrying out oil-water separation to obtain clear and transparent peony pistil oil. According to the extraction method of the peony pistil oil, provided by the invention, the peony pistil oil is extracted from peony pistils to the maximum extent by adopting a combined extraction method of the peony pistil oil, so that the utilization rate of raw materials is improved, and impurities such as vegetable wax, sugar, protein and the like in oil are reduced.
Description
Technical Field
The invention belongs to the field of cosmetics, and particularly relates to a method for extracting peony pistil oil.
Background
The peony pistil is rich in squalene, catechin, flavone compounds, polysaccharide and other active ingredients, and contains a large amount of minerals and trace elements. There have been preliminary advances in the qualitative and quantitative studies of bioactive components in peony pistil.
At present, the extraction method of the vegetable oil mainly comprises the following steps: (1) and (3) squeezing: the working principle is that plant cells are broken through pressure, oil flows out when being squeezed, and the oil can be obtained through standing or centrifugation; (2) an aqueous enzymatic method: the working principle is that after the plant is mechanically damaged, the oil is released into the water phase by adding enzyme to inhibit emulsification or demulsification, and then the oil phase is separated from the water phase or other impurities by methods such as centrifugation. (3) Solvent extraction method: the method is a method for extracting the grease by soaking by using an organic solvent which has low boiling point, is easy to separate and has solubility to the grease; (4) supercritical carbon dioxide extraction method: a novel separation technique for extracting active substances by taking supercritical fluid as an extracting agent; (5) an ultrasonic extraction method comprises the following steps: the working principle of the sound wave is that ultrasonic waves have fluctuation duality and energy, cavitation can be generated, penetration of grease is accelerated, and extraction rate is improved.
The oil prepared by the traditional squeezing method is impure, the storage life is short, and the comprehensive utilization rate of the oil is not high; although the aqueous enzymatic method has simple process and low equipment requirement, the process needs longer time and the price of the enzyme is higher, so the aqueous enzymatic method is not suitable for large-scale production; the supercritical carbon dioxide extraction method is non-toxic and harmless, the extraction process is stable, but the equipment cost is high, and the operation is difficult; the ultrasonic extraction method has high extraction efficiency and low extraction temperature, but the volume of an ultrasonic extraction tank cannot be too large, otherwise, ultrasonic blank areas are generated; the solvent extraction method has the advantages of high oil yield, simple operation and easy large-scale production and automation, but the extracted oil may have more impurities and solvent residues.
Therefore, a method for extracting peony pistil oil is needed to solve the problems of low extraction rate, more oil impurities and solvent residues in the prior art.
Disclosure of Invention
Aiming at the problems, the invention provides a method for extracting peony pistil oil, which adopts a method for extracting peony pistil oil in a combined way, improves the extraction rate of oil by ultrasonic, extracts oil by alcohol extraction, and reduces impurities such as vegetable wax, sugar, protein and the like in the oil by a water vapor method. The high ultrasonic power can improve the mass transfer rate and accelerate the contact speed of the solvent and the plant raw materials, and meanwhile, the ultrasonic can also generate a physical shearing force on plant cell tissues to denature and break the plant cell tissues and release inclusions, thereby accelerating the extraction rate of subsequent solution leaching and improving the extraction rate.
A method for extracting peony pistil oil comprises the following steps:
drying peony pistils, crushing and sieving;
weighing a certain amount of crushed and sieved peony pistils, putting the peony pistils into a filter paper bag, adding a certain amount of absolute ethyl alcohol, and carrying out ultrasonic treatment;
adding the filter paper bag subjected to ultrasonic treatment and absolute ethyl alcohol into a Soxhlet extractor, heating in a water bath, and refluxing to extract peony stamen oil;
collecting ethanol in the Soxhlet extractor, and concentrating under reduced pressure to obtain crude oil of peony pistil;
and adding a certain amount of distilled water into the peony pistil crude oil, and performing oil-water separation after distillation refining to obtain clear and transparent peony pistil oil.
Further, the ultrasonic treatment condition is 40KHz, 50W.
Further, the time of ultrasonic treatment is 20-60 minutes.
Further, crushing and sieving are carried out after the peony pistils are dried, and the peony pistils are crushed to 40-80 meshes.
Further, the air conditioner is provided with a fan,
the mass ratio of the peony pistil to the absolute ethyl alcohol is 1: 4-1: 10.
Further, the air conditioner is provided with a fan,
the temperature of the water bath heating reflux is 50-80 ℃.
Further, the air conditioner is provided with a fan,
the extraction time for extracting the peony pistil oil by water bath heating reflux is 2-6 hours.
Further, the air conditioner is provided with a fan,
the mass ratio of the peony pistil crude oil to the distilled water is 1: 4-1: 8.
Further, the extraction rate of the peony pistil oil is calculated by adopting the following formula:
further, the air conditioner is provided with a fan,
the extraction rate of the peony pistil oil is 15.6-22.1%.
According to the extraction method of the peony pistil oil, provided by the invention, the peony pistil oil is extracted from peony pistils to the maximum extent by adopting a combined extraction method of the peony pistil oil, so that the utilization rate of raw materials is improved, and impurities such as vegetable wax, sugar, protein and the like in oil are reduced. Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. 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.
The invention provides a method for extracting peony pistil oil, which comprises the following steps:
drying the peony pistils, and then crushing and sieving the peony pistils to 40-80 meshes;
weighing a certain amount of crushed and sieved peony pistils, putting the peony pistils into a filter paper bag, adding a certain amount of absolute ethyl alcohol, and carrying out ultrasonic treatment;
wherein the ultrasonic treatment condition is 40KHz and 50W, and the ultrasonic time is 20-60 minutes; the volume ratio of the mass of the peony pistil to the absolute ethyl alcohol is 1: 4-1: 10(g: mL).
Adding the filter paper bag subjected to ultrasonic treatment and absolute ethyl alcohol into a Soxhlet extractor, and heating and refluxing in a water bath to extract the peony pistil oil, wherein the heating and refluxing temperature in the water bath is 50-80 ℃, and the extraction time for extracting the peony pistil oil is 2-6 hours;
collecting ethanol in a Soxhlet extractor, and concentrating under reduced pressure to obtain crude oil of peony pistil;
adding a certain amount of distilled water into the peony pistil crude oil, distilling and refining, and then carrying out oil-water separation to obtain clear and transparent peony pistil oil. Wherein the volume ratio of the mass of the peony pistil crude oil to the distilled water is 1: 4-1: 8.
The extraction rate of the peony pistil oil is calculated by the following formula, and the extraction rate of the peony pistil oil obtained by the method provided by the invention is 15.6-22.1%.
Example 1
Crushing the dried peony pistils and sieving the crushed peony pistils by a 40-mesh sieve; weighing 50g of crushed and sieved peony pistils, putting the peony pistils into a filter paper bag, adding 200mL of absolute ethyl alcohol, and carrying out ultrasonic treatment for 20 minutes under the conditions of 40KHz and 50W; adding the filter paper bag and absolute ethyl alcohol into a Soxhlet extractor, and extracting the peony stamen oil by water bath heating reflux (0.075MPa), wherein the water bath heating reflux temperature is 50 ℃, and the extraction time for extracting the peony stamen oil is 2 hours; collecting ethanol in a Soxhlet extractor, and concentrating under reduced pressure to obtain crude oil of peony pistil; and further adding a certain amount of distilled water into the peony pistil crude oil according to the material-liquid ratio of 1:4(g: mL), and performing oil-water separation after distillation refining to obtain clear and transparent peony pistil oil.
By the method, the extraction rate of the peony pistil oil is calculated to be 15.6%.
Example 2
Crushing the dried peony pistils, and sieving the crushed peony pistils with a 60-mesh sieve; weighing 50g of crushed and sieved peony pistils, putting the peony pistils into a filter paper bag, adding 300mL of absolute ethyl alcohol, and carrying out ultrasonic treatment for 20 minutes under the conditions of 40KHz and 50W; adding the filter paper bag and absolute ethyl alcohol into a Soxhlet extractor, heating and refluxing in water bath (0.075MPa) to extract peony stamen oil, wherein the heating and refluxing temperature in water bath is 60 ℃, and the extraction time for extracting peony stamen oil is 3 hours; collecting ethanol in a Soxhlet extractor, and concentrating under reduced pressure to obtain crude oil of peony pistil; and further adding a certain amount of distilled water into the peony pistil crude oil according to the material-liquid ratio of 1:5(g: mL), and performing oil-water separation after distillation refining to obtain clear and transparent peony pistil oil.
By the method, the extraction rate of the peony pistil oil is calculated to be 18.3%.
Example 3
Crushing the dried peony pistils, and sieving the crushed peony pistils with a 80-mesh sieve; weighing 50g of crushed and sieved peony pistils, putting the peony pistils into a filter paper bag, adding 300mL of absolute ethyl alcohol, and carrying out ultrasonic treatment for 30 minutes under the conditions of 40KHz and 50W; adding the filter paper bag and absolute ethyl alcohol into a Soxhlet extractor, heating and refluxing in a water bath (0.075MPa) to extract the peony stamen oil, wherein the heating and refluxing temperature in the water bath is 65 ℃, and the extraction time for extracting the peony stamen oil is 4 hours; collecting ethanol in a Soxhlet extractor, and concentrating under reduced pressure to obtain crude oil of peony pistil; and further adding a certain amount of distilled water into the peony pistil crude oil according to the material-liquid ratio of 1:7(g: mL), and performing oil-water separation after distillation refining to obtain clear and transparent peony pistil oil.
By the method, the extraction rate of the peony pistil oil is calculated to be 22.1%.
Example 4
Crushing the dried peony pistils, and sieving the crushed peony pistils with a 80-mesh sieve; weighing 50g of crushed and sieved peony pistils, putting the peony pistils into a filter paper bag, adding 300mL of absolute ethyl alcohol, and carrying out ultrasonic treatment for 60 minutes under the conditions of 40KHz and 50W; adding the filter paper bag and absolute ethyl alcohol into a Soxhlet extractor, heating and refluxing in water bath (0.075MPa) to extract peony stamen oil, wherein the heating and refluxing temperature in water bath is 80 ℃, and the extraction time for extracting peony stamen oil is 6 hours; collecting ethanol in a Soxhlet extractor, and concentrating under reduced pressure to obtain crude oil of peony pistil; and further adding a certain amount of distilled water into the peony pistil crude oil according to the material-liquid ratio of 1:10(g: mL), and performing oil-water separation after distillation refining to obtain clear and transparent peony pistil oil.
By the method, the extraction rate of the peony pistil oil is calculated to be 20.5%.
Example 5
Crushing the dried peony pistils, and sieving the crushed peony pistils with a 80-mesh sieve; weighing 50g of crushed and sieved peony pistil, putting the crushed and sieved peony pistil into a filter paper bag, adding 300mL of absolute ethyl alcohol, adding the filter paper bag and the absolute ethyl alcohol into a Soxhlet extractor, and heating and refluxing in a water bath to extract peony pistil oil, wherein the temperature of the heating and refluxing in the water bath (0.075MPa) is 65 ℃, and the extraction time for extracting the peony pistil oil is 4 hours; collecting ethanol in a Soxhlet extractor, and concentrating under reduced pressure to obtain crude oil of peony pistil; and further adding a certain amount of distilled water into the peony pistil crude oil according to the material-liquid ratio of 1:7(g: mL), and performing oil-water separation after distillation refining to obtain clear and transparent peony pistil oil.
By the method, the extraction rate of the peony pistil oil is calculated to be 13.5%.
Example 6
To verify the effect of distilled water on total sugar, ethanol residue and total protein content in peony pistil oil.
Crushing the dried peony pistils, and sieving the crushed peony pistils with a 80-mesh sieve; weighing 50g of crushed and sieved peony pistils, putting the peony pistils into a filter paper bag, adding 300mL of absolute ethyl alcohol, and carrying out ultrasonic treatment for 30 minutes under the conditions of 40KHz and 50W; adding the filter paper bag and absolute ethyl alcohol into a Soxhlet extractor, heating and refluxing in a water bath (0.075MPa) to extract the peony stamen oil, wherein the heating and refluxing temperature in the water bath is 65 ℃, and the extraction time for extracting the peony stamen oil is 4 hours; collecting ethanol in the Soxhlet extractor, and concentrating under reduced pressure to obtain peony pistil oil.
By the method, the extraction rate of the peony pistil oil is calculated to be 23.8%.
It can be seen from examples 1-5 that sonication of the peony pistil and solvent prior to reflux extraction is helpful in increasing the extraction yield. In contrast, preferred conditions are crushing of the pistil to 80 mesh, a pistil to ethanol mass ratio of 1: 6. processing 40KW at 50Hz for 30 min, and extracting at 65 deg.C under reflux for 4 hr.
From examples 1-4, example 3 is the preferred condition for extraction of peony pistil oil, therefore, example 3 was chosen to compare with examples 5 and 6 to verify the effect of the combined extraction method on the total sugar, ethanol residue and total protein content of peony pistil oil. The total sugar content was measured by the phenol-sulfuric acid method, a standard curve was prepared using glucose as a standard, and table 1 shows the results of the total sugar content in examples 3, 5 and 6.
TABLE 1 determination of the Total sugar content in the examples
| Examples | Total sugar content (%) |
| Example 3 | 9.48 |
| Example 5 | 9.02 |
| Example 6 | 13.50 |
As can be seen from Table 1, the total sugar content in the peony pistil oil is lower in example 3 than in example 6, which shows that the total sugar content in the peony pistil oil can be effectively reduced through steam distillation; example 3 has a slightly higher total sugar content than example 5, which may be due to sonication.
The residual amount of ethanol in the peony pistil oil obtained in each example was measured by liquid chromatography, and Table 2 shows the residual amounts of ethanol in examples 3, 5 and 6.
TABLE 2 ethanol content determination for each example
| Examples | Ethanol content (%) |
| Example 3 | 0.88 |
| Example 5 | 0.85 |
| Example 6 | 2.41 |
As can be seen from Table 2, the ethanol residue in example 3 is lower than that in example 6, which shows that the ethanol residue in the peony pistil oil can be effectively reduced through steam distillation; example 3 has a slightly higher total sugar content than example 5, which may be due to sonication.
Total protein assay in peony pistil oil obtained in each example was performed using the biuret reagent method, and Table 3 shows the results of total protein assay in examples 3, 5 and 6.
TABLE 3 Total protein assay for each example
| Examples | Total protein content (%) |
| Example 3 | 10.18 |
| Example 5 | 9.67 |
| Example 6 | 10.04 |
As can be seen from Table 3, example 3 has a higher total protein content than example 5, and example 6 has a lesser yield, indicating that sonication can increase the total protein content in peony pistil oil; post-treatment steam distillation, however, had little effect on total protein content.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for extracting peony pistil oil comprises the following steps:
drying peony pistils, crushing and sieving;
weighing a certain amount of crushed and sieved peony pistils, putting the peony pistils into a filter paper bag, adding a certain amount of absolute ethyl alcohol, and carrying out ultrasonic treatment;
adding the filter paper bag subjected to ultrasonic treatment and absolute ethyl alcohol into a Soxhlet extractor, heating in a water bath, and refluxing to extract peony stamen oil;
collecting ethanol in the Soxhlet extractor, and concentrating under reduced pressure to obtain crude oil of peony pistil;
and adding a certain amount of distilled water into the peony pistil crude oil, and performing oil-water separation after distillation refining to obtain clear and transparent peony pistil oil.
2. The method for extracting peony pistil oil as claimed in claim 1,
the ultrasonic treatment conditions were 40KHz, 50W.
3. The method for extracting peony pistil oil as claimed in claim 2,
the ultrasonic treatment time is 20-60 minutes.
4. The method for extracting peony pistil oil as claimed in claim 1,
and (3) crushing and sieving the dried peony pistils, and crushing the peony pistils to 40-80 meshes.
5. The method for extracting peony pistil oil as claimed in claim 1,
the mass ratio of the peony pistil to the absolute ethyl alcohol is 1: 4-1: 10.
6. The method for extracting peony pistil oil as claimed in claim 1,
the temperature of the water bath heating reflux is 50-80 ℃.
7. The method for extracting peony pistil oil as claimed in claim 1,
the extraction time for extracting the peony pistil oil by water bath heating reflux is 2-6 hours.
8. The method for extracting peony pistil oil as claimed in claim 1,
the mass ratio of the peony pistil crude oil to the distilled water is 1: 4-1: 8.
9. The method for extracting peony pistil oil according to any one of claims 1-8,
the extraction rate of the peony pistil oil is calculated by adopting the following formula:
10. the method for extracting peony pistil oil as claimed in claim 9,
the extraction rate of the peony pistil oil is 15.6-22.1%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115181604A (en) * | 2022-07-21 | 2022-10-14 | 河南科技大学 | Peony pistil refined oil and preparation method and application thereof |
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