CN114395441A - A kind of extraction method of peony stamen oil - Google Patents

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

A kind of extraction method of peony stamen oil

technical field

The invention belongs to the field of cosmetics, in particular to a method for extracting peony stamen oil.

Background technique

Peony stamens are rich in various active ingredients such as squalene, catechins, flavonoids and polysaccharides, and contain a large amount of minerals and trace elements. Preliminary progress has been made in the qualitative and quantitative research on bioactive components in peony stamens.

At present, the extraction methods of vegetable oils and fats mainly include the following: (1) Pressing method: the working principle is that the plant cells are ruptured by pressure. When pressing, the oil will flow out, and the oil can be obtained by standing or centrifuging; (2) Water enzymatic method: Its working principle is that after the plant is mechanically damaged, the oil is released into the water phase by adding enzymes to inhibit emulsification or demulsification, and then the oil phase is separated from the water phase or other impurities by centrifugation and other methods. (3) Solvent extraction method: It is a method of extracting oil by soaking by using an organic solvent with a low boiling point, easy separation and solubility in oil; (4) Supercritical carbon dioxide extraction method: using supercritical fluid as the A new separation technology for extracting active substances with extractant; (5) Ultrasonic extraction method: a sound wave greater than 20KHz, the working principle is to use ultrasonic waves with duality and energy, which can produce cavitation, accelerate oil penetration, and improve extraction rate.

The oil prepared by the traditional pressing method is impure, the shelf life is short, and the comprehensive utilization rate of oil plants is not high; although the water enzymatic method has a simple process and low equipment requirements, the process requires a long time and the price of the enzyme is high, which is not suitable for large-scale production. Production; supercritical carbon dioxide extraction method is non-toxic and harmless, and the extraction process is stable, but the equipment cost is high and it is not easy to operate; the ultrasonic extraction method has high extraction efficiency and low extraction temperature, but the volume of the ultrasonic extraction tank should not be too large, otherwise an ultrasonic blank area will be generated ; The solvent extraction method has high oil yield, simple operation, easy large-scale production and automation, but the extracted oil may have many impurities and solvent residues.

Therefore, there is an urgent need to provide a method for extracting peony stamen oil to solve the problems of low extraction rate, many grease impurities and solvent residues in the prior art.

SUMMARY OF THE INVENTION

In view of the above problems, the present invention provides a method for extracting peony stamen oil, which adopts a combined method for extracting peony stamen oil, improves the oil extraction rate by ultrasound, extracts oil by alcohol leaching, and then uses water vapor to reduce vegetable wax in oil, Impurities such as sugars and proteins. High ultrasonic power can increase the mass transfer rate and speed up the contact speed between the solvent and the plant raw material. At the same time, the ultrasonic will also produce a physical shear force on the plant cell tissue, denature and break it, and release the contents, which will speed up the subsequent soaking of the solution. Improve the extraction rate and improve the extraction rate.

A kind of extraction method of peony stamen oil, described extraction method comprises the following steps:

After drying the peony stamens, pulverize and sieve;

Weigh a certain amount of pulverized and sieved peony stamens into a filter paper bag, add a certain amount of absolute ethanol, and carry out ultrasonic treatment;

The filter paper bag after ultrasonic treatment and absolute ethanol are added to the Soxhlet extractor, and the peony stamen oil is extracted by heating and refluxing in a water bath;

The ethanol in the Soxhlet extractor is collected, and concentrated under reduced pressure to obtain the crude oil of peony stamens;

A certain amount of distilled water is added to the crude oil of peony stamens, and oil-water separation is carried out after distillation and refining to obtain clear and transparent peony stamen oil.

Further, the conditions of the ultrasonic treatment are 40KHz, 50W.

Further, the time of the ultrasonic treatment is 20-60 minutes.

Further, the dried peony stamens are crushed and sieved, and the peony stamens are crushed to 40-80 mesh.

further,

The mass ratio of the peony stamens to the volume of absolute ethanol is 1:4 to 1:10.

further,

The temperature at which the water bath is heated and refluxed is 50-80°C.

further,

The extraction time of the water bath heating and refluxing to extract the peony stamen oil is 2-6 hours.

further,

The mass ratio of the crude oil of peony stamens to the volume ratio of distilled water is 1:4-1:8.

Further, the extraction rate of peony stamen oil is calculated by the following formula:

further,

The extraction rate of the peony stamen oil is 15.6%-22.1%.

The invention provides a method for extracting peony stamen oil, which adopts a combined extraction method for extracting peony stamen oil, extracts peony stamen oil from peony stamens to the maximum extent, improves the utilization rate of raw materials, and reduces vegetable waxes and sugars in oils and fats. and impurities such as protein. Other features and advantages of the present invention will be set forth in the description which follows, and in part will be apparent from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure pointed out in the description and claims.

Detailed ways

In order to make the objectives, technical solutions and advantages of the present invention clearer, the technical solutions in the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, and Not all examples. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

The invention provides a method for extracting peony stamen oil, which comprises the following steps:

After drying the peony stamens, crush and sieve, and crush the peony stamens to 40-80 mesh;

Weigh a certain amount of pulverized and sieved peony stamens into a filter paper bag, add a certain amount of absolute ethanol, and carry out ultrasonic treatment;

Wherein, the conditions of ultrasonic treatment are 40KHz, 50W, and the ultrasonic time is 20-60 minutes; the mass ratio of peony stamens to the volume of absolute ethanol is 1:4-1:10 (g:mL).

The filter paper bag after the ultrasonic treatment and absolute ethanol are added to the Soxhlet extractor, and the peony stamen oil is extracted by heating and refluxing in a water bath, wherein the temperature of the water bath heating and refluxing is 50-80 DEG C, and the extraction time for extracting the peony stamen oil is 2-6 Hour;

The ethanol in the Soxhlet extractor was collected, and concentrated under reduced pressure to obtain the crude oil of peony stamens;

A certain amount of distilled water is added to the crude oil of peony stamens, and oil-water separation is carried out after distillation and refining to obtain clear and transparent peony stamen oil. Wherein, the mass ratio of the crude oil of peony stamens to the volume of distilled water is 1:4 to 1:8.

The extraction rate of peony stamen oil is calculated by the following formula, and the extraction rate of peony stamen oil obtained by the method provided by the present invention is 15.6% to 22.1%.

Example 1

The dried peony stamens were pulverized and passed through a 40-mesh sieve; 50g of pulverized and sieved peony stamens were weighed and put into a filter paper bag, 200 mL of absolute ethanol was added, and sonicated for 20 minutes at 40KHz, 50W; then the above-mentioned filter paper bag and anhydrous Ethanol was added to the Soxhlet extractor, and the peony stamen oil was extracted by heating and refluxing in a water bath (0.075MPa), wherein the temperature of the water bath heating and refluxing was 50°C, and the extraction time for extracting the peony stamen oil was 2 hours; the ethanol in the Soxhlet extractor was collected. , concentrated under reduced pressure to obtain peony stamen crude oil; and then add a certain amount of distilled water to the peony stamen crude oil by a material-to-liquid ratio of 1:4 (g:mL), and carry out oil-water separation after distillation and refining to obtain clear and transparent peony stamen oil.

Through the above method, the extraction rate of peony stamen oil was calculated to be 15.6%.

Example 2

The dried peony stamens were pulverized and passed through a 60-mesh sieve; 50g of pulverized and sieved peony stamens were weighed and put into a filter paper bag, 300 mL of absolute ethanol was added, and sonicated for 20 minutes at 40KHz, 50W; then the above-mentioned filter paper bag and anhydrous Ethanol was added to the Soxhlet extractor, and the peony stamen oil was extracted by heating and refluxing in a water bath (0.075MPa), wherein the temperature of the water bath heating and refluxing was 60°C, and the extraction time for extracting the peony stamen oil was 3 hours; the ethanol in the Soxhlet extractor was collected. , concentrated under reduced pressure to obtain peony stamen crude oil; and then add a certain amount of distilled water to the peony stamen crude oil by a material-to-liquid ratio of 1:5 (g:mL), and carry out oil-water separation after distillation and refining to obtain clear and transparent peony stamen oil.

Through the above method, the extraction rate of peony stamen oil was calculated to be 18.3%.

Example 3

The dried peony stamens were pulverized and passed through an 80-mesh sieve; 50g of pulverized and sieved peony stamens were weighed and put into a filter paper bag, 300 mL of absolute ethanol was added, and sonicated for 30 minutes at 40KHz, 50W; then the above-mentioned filter paper bag and anhydrous Ethanol was added to the Soxhlet extractor, and the peony stamen oil was extracted by heating and refluxing in a water bath (0.075MPa), wherein the temperature of the water bath heating and refluxing was 65°C, and the extraction time for extracting the peony stamen oil was 4 hours; the ethanol in the Soxhlet extractor was collected. , concentrated under reduced pressure to obtain peony stamen crude oil; then add a certain amount of distilled water to the peony stamen crude oil by a material-to-liquid ratio of 1:7 (g:mL), and carry out oil-water separation after distillation and refining to obtain clear and transparent peony stamen oil.

Through the above method, the extraction rate of peony stamen oil was calculated to be 22.1%.

Example 4

The dried peony stamens were pulverized and passed through an 80-mesh sieve; 50g of pulverized and sieved peony stamens were weighed and put into a filter paper bag, 300 mL of absolute ethanol was added, and sonicated for 60 minutes at 40KHz, 50W; then the above-mentioned filter paper bag and anhydrous Ethanol was added to the Soxhlet extractor, and the peony stamen oil was extracted by heating and refluxing in a water bath (0.075MPa), wherein the temperature of the water bath heating and refluxing was 80°C, and the extraction time for extracting the peony stamen oil was 6 hours; the ethanol in the Soxhlet extractor was collected. , concentrated under reduced pressure to obtain peony stamen crude oil; then add a certain amount of distilled water to the peony stamen crude oil by a material-to-liquid ratio of 1:10 (g:mL), and carry out oil-water separation after distillation and refining to obtain clear and transparent peony stamen oil.

Through the above method, the extraction rate of peony stamen oil was calculated to be 20.5%.

Example 5

The dried peony stamens were pulverized and passed through an 80-mesh sieve; 50 g of pulverized and sieved peonies were weighed and put into a filter paper bag, 300 mL of absolute ethanol was added, the above-mentioned filter paper bag and absolute ethanol were added to a Soxhlet extractor, and the extraction was performed by heating and refluxing in a water bath. Peony stamen oil, wherein, the temperature of heating and refluxing (0.075MPa) in a water bath is 65° C., and the extraction time for extracting peony stamen oil is 4 hours; the ethanol in the Soxhlet extractor is collected, and concentrated under reduced pressure to obtain peony stamen crude oil; A certain amount of distilled water is added to the crude oil of peony stamens according to a material-liquid ratio of 1:7 (g:mL), and after distillation and refining, oil-water separation is carried out to obtain clear and transparent peony stamen oil.

Through the above method, the extraction rate of peony stamen oil was calculated to be 13.5%.

Example 6

In order to verify the effect of adding distilled water on the content of total sugar, ethanol residue and total protein in peony oil.

The dried peony stamens were pulverized and passed through an 80-mesh sieve; 50g of pulverized and sieved peony stamens were weighed and put into a filter paper bag, 300 mL of absolute ethanol was added, and sonicated for 30 minutes at 40KHz, 50W; then the above-mentioned filter paper bag and anhydrous Ethanol was added to the Soxhlet extractor, and the peony stamen oil was extracted by heating and refluxing in a water bath (0.075MPa), wherein the temperature of the water bath heating and refluxing was 65°C, and the extraction time for extracting the peony stamen oil was 4 hours; the ethanol in the Soxhlet extractor was collected. , concentrated under reduced pressure to obtain peony stamen oil.

Through the above method, the extraction rate of peony stamen oil was calculated to be 23.8%.

From Examples 1-5, it can be concluded that ultrasonic treatment of peony stamens and solvent before reflux extraction is helpful to improve the extraction rate. In contrast, the preferred conditions are that the stamens are crushed to 80 mesh, the mass ratio of stamens to ethanol is 1:6, 40 KW, 50 Hz treatment for 30 minutes, and heating and refluxing extraction at 65°C for 4 hours.

As can be seen from Examples 1-4, Example 3 is the optimal condition for the extraction of peony oil. Therefore, Example 3 was selected to compare with Example 5 and Example 6 to verify that the combined extraction method had a significant effect on the total sugar, total sugar in peony oil, Effects of ethanol residues and total protein content. The total sugar content was measured by the phenol-sulfuric acid method, and a standard curve was prepared with glucose as the standard substance. Table 1 shows the results of the total sugar content of Examples 3, 5 and 6.

Table 1 Determination of total sugar content of each embodiment

Example Total sugar content (%) Example 3 9.48 Example 5 9.02 Example 6 13.50

As can be drawn from Table 1, the total sugar content of Example 3 is lower than that of Example 6, which shows that the total sugar content in the peony stamen oil can be effectively reduced through steam distillation; the total sugar content of Example 3 is slightly higher than that of Example 5. Possibly due to ultrasound.

The residual ethanol in the peony oil obtained in each example was determined by liquid chromatography. Table 2 shows the residual amount of ethanol in Examples 3, 5 and 6.

Table 2 Determination of ethanol content of each embodiment

Example Ethanol content (%) Example 3 0.88 Example 5 0.85 Example 6 2.41

It can be drawn from Table 2 that the ethanol residue in Example 3 is lower than that in Example 6, which shows that the ethanol residue in the peony stamen oil can be effectively reduced through steam distillation; the total sugar content of Example 3 is slightly higher than that of Example 5, which may be due to ultrasound.

The biuret reagent method was used to determine the total protein in the peony oil obtained in each example, and Table 3 shows the total protein determination results of Examples 3, 5 and 6.

Table 3 Determination of total protein content of each embodiment

Example Total protein content (%) Example 3 10.18 Example 5 9.67 Example 6 10.04

As can be drawn from Table 3, the total protein content of Example 3 is higher than that of Example 5, and is not much different from that of Example 6, which shows that ultrasonic treatment can improve the total protein content in the peony oil; The content has little effect.

Although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: it is still possible to modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements to some of the technical features; and these Modifications or substitutions do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the 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%.