Process for extracting acanthopanax volatile oil by freeze-drying method

Abstract

The invention discloses a process for extracting acanthopanax volatile oil by a freeze-drying method. The process comprises the following steps: adding water into dried acanthopanax leaves, and soaking until the leaves are completely stretched; carrying out spiral extrusion treatment on the acanthopanax senticosus leaves subjected to water immersion; putting the acanthopanax leaf fragments into water with set enzyme concentration and heating in a water bath; filtering the acanthopanax senticosus leaf fragments heated in the water bath, draining water, putting into a container, and transferring into a freeze-drying device for extraction; collecting volatile oil components in the cold trap after extraction, extracting with petroleum ether, adding anhydrous sodium sulfate to remove residual moisture, concentrating, and combining volatile oil; according to the technology for extracting the acanthopanax volatile oil by the freeze-drying method, freeze-drying can not only destroy cell walls of acanthopanax leaves and improve the dissolution rate of the volatile oil, but also is beneficial to reduction of oxygenolysis and loss of the volatile oil at a low temperature, so that the stability of heat-sensitive components in the volatile oil is ensured; the biological activity is protected, so that the acanthopanax volatile oil with more chemical components is obtained, and simple and efficient extraction of the acanthopanax volatile oil is realized.

Description

Technical Field

[0001] The invention belongs to the technical field of volatile oil extraction, and particularly relates to a freeze-drying process for extracting acanthopanax senticosus volatile oil. Background Art

[0002] Acanthopanax senticosus is a plant of the Araliaceae family, distributed throughout my country, with the Northeast having the most suitable growth environment, and its production accounts for more than 90% of the country's total. Acanthopanax senticosus, as a homologous food and medicinal plant, has unique properties such as warm nature, bitter taste, slightly sweet, and non-toxicity, and can also be used as a sustainable natural plant resource. Acanthopanax senticosus volatile oil is a poorly water-soluble, volatile chemical extracted from the dry leaves of Acanthopanax senticosus, which contains a high content of active ingredients. The flavonoids in Acanthopanax senticosus volatile oil have antibacterial activity, and have antibacterial effects on a variety of fungi and bacteria and inhibit the growth of fungi; polysaccharide compounds have immune regulation, enhance the body's resistance, anti-tumor and other functions; glycoside compounds have anti-inflammatory, antioxidant, sedative and tranquilizing effects.

[0003] The main extraction methods of Acanthopanax senticosus volatile oil include steam distillation, supercritical CO2 extraction, microwave distillation, etc. Steam distillation is a common method for extracting volatile oil by manufacturers at home and abroad because of its simple equipment and low cost. However, it is difficult to destroy the plant cell wall by steam distillation, and the extraction rate of volatile oil is low. In addition, the high temperature required for distillation can easily destroy the heat-sensitive components in the dry leaves of Acanthopanax senticosus. Freeze-drying is a drying method that freezes the water in the cells of Acanthopanax senticosus into ice and sublimates, which can burst the cell wall and improve the extraction rate of volatile oil. At the same time, it effectively retains the active ingredients in the dry leaves of Acanthopanax senticosus at low temperatures, which is conducive to the extraction of chemical substances that are easily decomposed by heat. The pretreatment before freeze-drying can destroy the cell wall of Acanthopanax senticosus by spiral extrusion and enzymolysis. In addition, freeze-drying is to dry the plant at low temperature under vacuum, which can more thoroughly destroy the plant cell wall and improve the extraction efficiency of volatile oil. Freeze-drying can avoid protein denaturation in plants, maintain biological activity, and retain volatile components and heat-sensitive components in plants as much as possible. Moreover, the volume and shape of the plant remain basically unchanged after drying, and the rehydration property is good. Summary of the invention

[0004] The purpose of the present invention is to provide a freeze-drying method for extracting Acanthopanax senticosus volatile oil. The cell walls of Acanthopanax senticosus leaves are destroyed by enzymatic hydrolysis and the freeze-drying time is controlled, so as to improve the dissolution rate of volatile oil in Acanthopanax senticosus dry leaf cells and retain the heat-sensitive components therein, so as to obtain Acanthopanax senticosus dry leaf oil with more chemical substances, thereby realizing simple and efficient extraction of Acanthopanax senticosus volatile oil.

[0005] To achieve the above objectives, this application is implemented through the following technical solutions:

[0006] A freeze-drying method for extracting Acanthopanax senticosus volatile oil comprises the following steps:

[0007] S1. Raw material pretreatment: soak the dried leaves of Acanthopanax senticosus in water until the leaves are fully expanded;

[0008] S2, subjecting the soaked Acanthopanax senticosus leaves in step S1 to a spiral extrusion process;

[0009] S3, placing the Acanthopanax senticosus leaf fragments prepared in step S2 into water with set enzyme concentration and pH and heating in a water bath;

[0010] S4, filtering the Acanthopanax senticosus leaves heated in a water bath in step S3, draining the water, placing them in a container, and moving them into a freeze-drying device for extraction;

[0011] S5. After the extraction is completed, the volatile oil components in the cold trap are collected, extracted with petroleum ether, and then the residual water is removed, and the volatile oils are combined after concentration.

[0012] Furthermore, in step S3, the material ratio of water to Acanthopanax senticosus dry leaves is 30:1-10:1, and the pH is adjusted to 3-7 after adding water.

[0013] Furthermore, in step S3, the enzyme preparation used is one or more of cellulase, hemicellulase, pectinase, and α-amylase.

[0014] Furthermore, in step S3, the enzyme concentration is 0.1-1.5%, the enzymatic hydrolysis time is 30-120 min, and the enzymatic hydrolysis temperature is 30-70 °C.

[0015] Furthermore, in step S4, the freeze-drying time is 6-48 hours.

[0016] Furthermore, in step S5, anhydrous sodium sulfate is used to remove residual moisture.

[0017] The beneficial effects of the present invention are:

[0018] 1. The present invention utilizes a low-temperature freezing extraction method to extract Acanthopanax senticosus volatile oil. The low-temperature freezing freezes the water in the Acanthopanax senticosus leaf cells, bursts the cell walls, and then takes out the Acanthopanax senticosus volatile oil through sublimation, thereby increasing the dissolution rate of the volatile oil in the Acanthopanax senticosus dry leaf cells, achieving a high volatile oil extraction rate, and being simple to operate, green and efficient.

[0019] 2. The present invention utilizes freeze-drying to extract Acanthopanax senticosus volatile oil. Low temperature can retain the active ingredients and more heat-sensitive components of Acanthopanax senticosus leaves, preventing them from being decomposed and oxidized by heat. GC-MS analysis identifies multiple chemical components and rich components. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 The figure is the total ion current diagram of the GC-MS of Acanthopanax senticosus volatile oil in the embodiment of the present invention.

[0021] Figure 2 This is the GC-MS total ion current diagram of Acanthopanax senticosus volatile oil extracted by steam distillation in Verification Example 1 of the present invention.

[0022] Figure 3 This is the GC-MS total ion current diagram of Acanthopanax senticosus volatile oil extracted by enzyme-assisted steam distillation in Verification Example 2 of the present invention.

[0023] Figure 4 This is the GC-MS total ion current diagram of solvent-free microwave extraction of Acanthopanax senticosus volatile oil in Verification Example 3 of the present invention.

[0024] Figure 5 It is a schematic diagram of the structure of the device of the present invention.

[0025] Description of reference numerals:

[0026] 1. Vacuum oil-free diaphragm pump; 2. Negative pressure gauge; 3. Vacuum box; 4. Sample table; 5. Coolant. DETAILED DESCRIPTION

[0027] In order to more clearly illustrate the technical solution of the present invention, the technical solution of the present invention will be described in detail through embodiments below. The following embodiments are merely exemplary and can only be used to explain and illustrate the technical solution of the present invention, and cannot be construed as limiting the technical solution of the present invention.

[0028] Unless otherwise defined, technical or scientific terms used in the present invention shall have the common meanings understood by one having ordinary skills in the field to which the present invention belongs.

[0029] Example

[0030] Take 200 g of Acanthopanax senticosus dry leaves and soak them in water until the leaves are fully stretched, then squeeze them into pieces by spiral extrusion, then take 2 g of cellulase and dissolve it in water with a pH of 5, add the Acanthopanax senticosus leaf pieces after spiral extrusion, and water bath at 50 °C for 90 min, filter, control the water, and freeze-dry in a freeze dryer for 48 h, extract the Acanthopanax senticosus volatile oil components in the cold trap, extract with petroleum ether, and add anhydrous sodium sulfate to remove residual water. The volatile oil extraction rate is calculated to be 0.0384%.

[0031] The obtained Acanthopanax senticosus volatile oil was subjected to GC-MS detection. The gas chromatography conditions were as follows: capillary J&WDB-5 (30 m×0.25 mm×0.25 µm), injection volume of 1.0 µL, injection port temperature of 230 °C; temperature program: 90 °C for 1 min, 150 °C at 5 °C / min, 1 min, 180 °C at 5 °C / min, 2 min, 230 °C at 5 °C / min, 3 min. The carrier gas was nitrogen with a flow rate of 1.0 mL / min; split ratio: 50:1.

[0032] Mass spectrometry conditions: EI+ ion source, ionization source temperature: 230 °C; electron energy 70 eV; filament flow rate 0.2 mA; interface temperature: 250 °C; mass scanning range: 20-500 amu.

[0033] The chemical components of the volatile oil from the dry leaves of Acanthopanax senticosus were analyzed. The total ion current of the volatile oil from the dry leaves of Acanthopanax senticosus was Figure 1 The specific chemical composition is shown in Table 1.

[0034] Table 1 Analysis results of chemical components of Acanthopanax senticosus volatile oil extracted by freeze-drying

[0035]

[0036] Table 1

[0037]

[0038] Verification Example 1

[0039] Process for extracting Acanthopanax senticosus volatile oil by steam distillation:

[0040] Take 50 g of Acanthopanax senticosus dry leaves and put them into a crusher to crush them into powder, pass through a 40-mesh sieve, add 750 mL of water according to the material ratio of 1:15 (mass ratio), place it under a heating jacket and heat it for 3 h to extract Acanthopanax senticosus volatile oil. After the extraction is completed, collect the volatile oil components in the upper half of the light oil extractor, and add anhydrous sodium sulfate to remove residual water. The volatile oil extraction rate is calculated to be 0.0796%.

[0041] The chemical components of the volatile oil extracted from the dry leaves of Acanthopanax senticosus were analyzed by steam distillation. The total ion current of the volatile oil in GC-MS was as follows: Figure 2 The specific chemical composition is shown in Table 2.

[0042] Table 2 Analysis results of chemical components of Acanthopanax senticosus volatile oil extracted by steam distillation

[0043]

[0044] Table 2

[0045]

[0046] Verification Example 2

[0047] Enzyme-assisted steam distillation process for extracting Acanthopanax senticosus volatile oil:

[0048] Take 50 g of Acanthopanax senticosus dry leaves and put them into a crusher to crush them into powder, pass through a 40-mesh sieve, add 750 mL of water according to the material ratio of 1:15 (mass ratio), then add 0.5 g of cellulase, put them in a 50 ℃ water bath for enzymolysis for 1.5 h, and then place them in a heating jacket for heating for 3 h to extract Acanthopanax senticosus volatile oil. After the extraction is completed, the volatile oil components in the upper half of the light oil extractor are collected, and anhydrous sodium sulfate is added to remove residual water. The volatile oil extraction rate is calculated to be 0.1154%.

[0049] The chemical components of the volatile oil extracted from the dry leaves of Acanthopanax senticosus by cellulase-assisted steam distillation were analyzed. The total ion current of the volatile oil in GC-MS was as follows: Figure 3 The specific chemical composition is shown in Table 3.

[0050] Table 3 Analysis results of chemical components of Acanthopanax senticosus volatile oil extracted by enzyme-assisted steam distillation

[0051]

[0052] Table 3 (1)

[0053]

[0054] Table 3 (2)

[0055]

[0056] Verification Example 3

[0057] Solvent-free microwave extraction of Acanthopanax senticosus volatile oil:

[0058] Take 50 g of Acanthopanax senticosus dry leaves and soak them in water until the leaves are fully expanded, filter, drain, cut into pieces, and directly put them into a flask without adding any solvent for microwave heating extraction. The microwave power is 567 W and the extraction time is 1 h. After the extraction is completed, the volatile oil components in the upper half of the light oil extractor are collected, and anhydrous sodium sulfate is added to remove residual water. The volatile oil extraction rate is calculated to be 0.0724%.

[0059] The chemical components of the volatile oil extracted from the dry leaves of Acanthopanax senticosus were analyzed by ordinary solvent-free microwave extraction. The total ion current of the volatile oil GC-MS was as follows Figure 4 The specific chemical composition is shown in Table 4.

[0060] Table 4 Analysis results of chemical components of Acanthopanax senticosus volatile oil extracted by solvent-free microwave

[0061]

[0062] Table 4 (1)

[0063]

[0064] Table 4 (2)

[0065]

[0066] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that they can still modify or replace the technical solution of the present invention with equivalents, and these modifications or equivalent replacements cannot cause the modified technical solution to deviate from the spirit and scope of the technical solution of the present invention.

Claims

1. A freeze-drying process for extracting Acanthopanax senticosus volatile oil, characterized in that: The following steps are involved: S1. Raw material pretreatment: soak the dried leaves of Acanthopanax senticosus in water until the leaves are fully expanded; S2, subjecting the soaked Acanthopanax senticosus leaves in step S1 to a spiral extrusion process; S3, placing the Acanthopanax senticosus leaf fragments prepared in step S2 into water with set enzyme concentration and pH and heating in a water bath; S4, filtering the Acanthopanax senticosus leaves heated in a water bath in step S3, draining the water, placing the leaves in a container, and transferring the containers to a freeze-drying device for extraction; S5. After the extraction is completed, the volatile oil components in the cold trap are collected, extracted with petroleum ether, and then the residual water is removed, and the volatile oils are combined after concentration.

2. The freeze-drying method for extracting Acanthopanax senticosus volatile oil according to claim 1, characterized in that: In step S3, the material ratio of water to Acanthopanax senticosus dry leaves is 30:1-10:1, and the pH is adjusted to 3-7 after adding water.

3. The freeze-drying method for extracting Acanthopanax senticosus volatile oil according to claim 1, characterized in that: In step S3, the enzyme preparation used is one or more of cellulase, hemicellulase, pectinase and α-amylase.

4. The freeze-drying method for extracting Acanthopanax senticosus volatile oil according to claim 1, characterized in that: In step S3, the enzyme concentration is 0.1-1.5%, the enzymatic hydrolysis time is 30-120 min, and the enzymatic hydrolysis temperature is 30-70 °C.

5. The freeze-drying method for extracting Acanthopanax senticosus volatile oil according to claim 1, characterized in that: In step S4, the freeze-drying time is 6-48 hours.

6. The freeze-drying method for extracting Acanthopanax senticosus volatile oil according to claim 1, characterized in that: In step S5, anhydrous sodium sulfate is used to remove residual moisture.

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