A method for preparing a vanilla infusion

Abstract

This invention belongs to the field of plant active ingredient extraction technology, specifically relating to a method for preparing a *Panax notoginseng* extract, comprising: washing fresh *Panax notoginseng* leaves in clean water, cutting them into sections, air-drying them, then freeze-drying them and grinding them into fine powder; adding the *Panax notoginseng* leaf powder to an ethanol-ether solution and stirring rapidly, then allowing it to stand at low temperature for 1-3 hours, sealing it under steam reflux for 20-30 minutes, and filtering it after natural cooling to obtain a first extract and a first filter residue; adding the first filter residue to an ethanol-water solution and stirring to form a slurry, then pressure filtering it; then placing the pressure-filtered residue and filtrate into an alkaline solution and microwaving it for 1-3 hours, and filtering it to obtain a second filter residue and a second filtrate; mixing the first and second filtrates and adjusting the pH to neutral with hydrochloric acid, concentrating it under reduced pressure, and then air-drying it to obtain a crude extract; then placing the crude extract into ethanol and ultrasonically dispersing it at low temperature for 20-30 minutes, filtering it, and distilling the filtrate to obtain the *Panax notoginseng* extract.

Description

Technical Field

[0001] This invention belongs to the field of plant active ingredient extraction technology, specifically relating to a method for preparing a herb extract. Background Technology

[0002] Pandanus leaves are the fresh leaves of Pandanus odoratus (also known as fragrant pandanus leaves, banyan leaves, etc.) belonging to the Pandanaceae family and the Pandanus genus. Pandanus odoratus is an evergreen herb, with leaves approximately 30cm long and 1.5cm wide. The leaf margins occasionally show small prickles, while the leaf tips have slightly denser prickles. The underside of the leaf also has small prickles. The leaf sheath has a narrow white membrane. Flowers and fruits have not been observed. It is native to the Maguru Islands of Indonesia. Studies have found that Pandanus odoratus adapts to the acidic red soils of southern my country, but due to temperature limitations, it is only suitable for growth in the southern subtropical to tropical regions of my country. Literature reports that the traditional extraction process for the volatile components of Pandanus odoratus mainly uses steam distillation, but this method has drawbacks such as low extraction efficiency and easy decomposition of heat-sensitive substances. Summary of the Invention

[0003] To address the problems in the existing technology, this invention provides a method for preparing Anemarrhena asphodeloides extract, which solves the problem of low extraction efficiency. The method uses freeze-grinding to refine the leaves of Anemarrhena asphodeloides, and forms an extract under alcohol and alkali extraction. Then, the extract is obtained by ethanol ultrasonic extraction, which greatly improves the extraction rate. Moreover, the relatively low temperature extraction environment ensures the stability of the active substances in the extract.

[0004] To achieve the above technical objectives, the technical solution of the present invention is as follows:

[0005] A method for preparing a fragrant dewdrop extract includes the following steps:

[0006] Step 1: Wash fresh Pandanus leaves in clean water, cut them into sections, and air-dry them. Then freeze-dry them and grind them into fine powder to obtain Pandanus leaf powder. The air-drying temperature is 30-50℃, the freeze-drying temperature is -30℃, and the grinding pressure is 0.4-0.6MPa. This step uses clean water to remove surface impurities, especially surface mud and sand, to achieve a clean surface. The Pandanus leaves are cut into long strips and the surface water film is removed by air-drying. During the freeze-drying process, the Pandanus leaves freeze and become brittle. During the grinding process, the grinding pressure can break the long strips of Pandanus leaves into a fragmented structure, thereby forming Pandanus leaf powder.

[0007] Step 2: Add the *Panax notoginseng* leaf powder to the ethanol-ether solution and stir rapidly. Let it stand at a low temperature for 1-3 hours, then reflux under sealed conditions for 20-30 minutes. After natural cooling, filter to obtain the first extract and the first filter residue. The volume ratio of ethanol to ether in the ethanol-ether solution is 1:4-5. The concentration of *Panax notoginseng* leaf powder in the ethanol-ether solution is 200-500 g / L. The stirring speed is 1000-1500 r / min. The temperature for standing at low temperature is 5-10℃. The temperature for reflux under sealed conditions is 40-60℃. This step utilizes the difference in permeability and boiling point between ethanol and ether to create permeation and reflux. During reflux, ethanol maintains its stability, while ether repeatedly refluxes as steam, thus forming a reflux reaction system. Ethanol and ether form different permeation and dissolution systems under different atmospheres, achieving the permeation and dissolution effect of organic solvents. It is particularly important to note that ethanol and ether form a gradient dissolution effect at different temperatures, creating a synergistic effect combining permeation and dissolution.

[0008] Step 3: Add the first filter residue to an ethanol-water solution and stir to form a slurry. Then, perform pressure filtration. Next, place the filtered residue and filtrate into an alkaline solution and microwave for 1-3 hours. Filter to obtain a second filter residue and a second filtrate. The mass ratio of the first filter residue to the ethanol-water solution is 3-5:2, the volume percentage of ethanol in the ethanol-water solution is 50-60%, the pressure for pressure filtration is 0.6-0.7 MPa, and the filtration rate is 1-5 L / min. The alkaline solution used is a sodium hydroxide solution with a pH of 8-. 8.5, the mass ratio of the filter residue to the alkaline solution is 1:3-5, the temperature of the microwave reaction is 50-70℃, and the microwave power is 200-400W. In this step, the first filter residue is added to distilled water to form a slurry, and the water in the slurry is removed by pressure filtration, which causes the cells to be squeezed and ruptured and flow out. However, the effect of dissolving intracellular substances by pressure filtration is not good. Therefore, the filter residue is microwave-treated in alkaline conditions to achieve alkaline dissolution of cell wall polysaccharides, thereby opening the cell wall and improving the alkaline dissolution effect.

[0009] Step 4: Mix the first and second filtrates and adjust the pH to neutral using hydrochloric acid. After vacuum concentration, dry the mixture to obtain a crude extract. Then, place the crude extract in ethanol and ultrasonically disperse it at low temperature for 20-30 minutes. After filtration, distill the filtrate to obtain a *Panax notoginseng* extract. The vacuum concentration pressure is 80-90% of atmospheric pressure, and the temperature is 60-70℃. The concentration of the crude extract in ethanol is 500-600 g / L. The low-temperature ultrasonic dispersion temperature is 5-10℃, the ultrasonic frequency is 50-80 kHz, and the distillation temperature is 50-60℃. This step uses vacuum concentration to remove most of the ethanol and water, and obtains a crude extract during drying. Then, the crude extract is dissolved in ethanol through ultrasonic dispersion to remove insoluble matter, improve the stability and purity of the extract, and obtain a *Panax notoginseng* extract with better purity during distillation.

[0010] The fragrant clover extract is used to flavor tobacco, and its dosage is 0.05-0.10% of the weight of tobacco leaves. Furthermore, the fragrant clover extract is diluted with ethanol and sprayed onto the tobacco leaves.

[0011] As can be seen from the above description, the present invention has the following advantages:

[0012] 1. This invention solves the problem of low extraction efficiency of Antrodia elata leaves by using freeze-grinding to refine the leaves and forming an extract under alcohol and alkali extraction. The extract is then obtained by ultrasonic extraction with ethanol, which greatly improves the extraction rate. The relatively low temperature extraction environment ensures the stability of the active substances in the extract.

[0013] 2. This invention utilizes freeze-grinding to physically refine the leaves of Pandanus odoratus without damaging the active substances. Attached Figure Description

[0014] Figure 1 This is the total ion chromatogram of the extract of *Platycodon grandiflorus* from Example 1. Implementation

[0015] Combination Figure 1 The present invention has been described in detail with reference to the embodiments, but the claims of the present invention are not intended to limit the scope of the invention.

[0016] Example 1: A method for preparing a fragrant dewdrop extract, comprising the following steps:

[0017] Step 1: Wash fresh Pandanus leaves in clean water, cut them into sections, and air-dry them. Then freeze-dry them and grind them into fine powder to obtain Pandanus leaf powder. The air-drying temperature is 30℃, the freeze-drying temperature is -30℃, and the grinding pressure is 0.4MPa.

[0018] Step 2: Add the *Panax notoginseng* leaf powder to the ethanol-ether solution and stir rapidly. Let it stand at low temperature for 1 hour, then reflux under sealed conditions for 20 minutes. After natural cooling, filter to obtain the first extract and the first filter residue. The volume ratio of ethanol to ether in the ethanol-ether solution is 1:4, the concentration of *Panax notoginseng* leaf powder in the ethanol-ether solution is 200 g / L, the stirring speed is 1000 r / min, the temperature for standing at low temperature is 5°C, and the temperature for reflux under sealed conditions is 40°C.

[0019] Step 3: Add the first filter residue to an ethanol-water solution and stir to form a slurry. Then, perform pressure filtration. Next, place the pressure-filtered residue and filtrate into an alkaline solution and microwave for 1 hour. Filter to obtain a second filter residue and a second filtrate. The mass ratio of the first filter residue to the ethanol-water solution is 3:2, the volume percentage of ethanol in the ethanol-water solution is 50%, the pressure of the pressure filtration is 0.6 MPa, and the pressure filtration rate is 1 L / min. The alkaline solution is a sodium hydroxide solution with a pH of 8. The mass ratio of the pressure-filtered residue to the alkaline solution is 1:3. The microwave reaction temperature is 50°C, and the microwave power is 200 W.

[0020] Step 4: Mix the first and second filtrates and adjust the pH to neutral using hydrochloric acid. After concentration under reduced pressure, dry the mixture to obtain a crude extract. Then, place the crude extract in ethanol and disperse it under low-temperature ultrasonication for 20 minutes. After filtration, distill the filtrate to obtain aromatic extract. The pressure of the reduced pressure concentration is 80% of atmospheric pressure, and the temperature is 60°C. The concentration of the crude extract in ethanol is 500 g / L. The temperature of the low-temperature ultrasonic dispersion is 5°C, the ultrasonic frequency is 50 kHz, and the distillation temperature is 50°C.

[0021] Example 2: A method for preparing a fragrant dewdrop extract, comprising the following steps:

[0022] Step 1: Wash fresh Pandanus leaves in clean water, cut them into sections, and air-dry them. Then freeze-dry them and grind them into fine powder to obtain Pandanus leaf powder. The air-drying temperature is 50℃, the freeze-drying temperature is -30℃, and the grinding pressure is 0.6MPa.

[0023] Step 2: Add the *Panax notoginseng* leaf powder to the ethanol-ether solution and stir rapidly. Let it stand at a low temperature for 1-3 hours, then reflux under sealed conditions for 30 minutes. After natural cooling, filter to obtain the first extract and the first filter residue. The volume ratio of ethanol to ether in the ethanol-ether solution is 1:5, the concentration of *Panax notoginseng* leaf powder in the ethanol-ether solution is 500 g / L, the stirring speed is 1500 r / min, the temperature for standing at low temperature is 10°C, and the temperature for reflux under sealed conditions is 60°C.

[0024] Step 3: The first filter residue is added to an ethanol-water solution and stirred to form a slurry. The slurry is then pressure filtered. The pressure-filtered residue and filtrate are then placed in an alkaline solution and microwaved for 3 hours. The mixture is then filtered to obtain a second filter residue and a second filtrate. The mass ratio of the first filter residue to the ethanol-water solution is 5:2, the volume percentage of ethanol in the ethanol-water solution is 60%, the pressure of the pressure filter is 0.7 MPa, and the pressure filter rate is 5 L / min. The alkaline solution used is a sodium hydroxide solution with a pH of 8.5. The mass ratio of the pressure-filtered residue to the alkaline solution is 1:5. The microwave reaction temperature is 70°C, and the microwave power is 400 W.

[0025] Step 4: Mix the first and second filtrates and adjust the pH to neutral with hydrochloric acid. After concentration under reduced pressure, dry the mixture to obtain a crude extract. Then, place the crude extract in ethanol and disperse it under low-temperature ultrasonication for 30 minutes. After filtration, distill the filtrate to obtain aromatic extract. The pressure of the reduced pressure concentration is 90% of atmospheric pressure, and the temperature is 70°C. The concentration of the crude extract in ethanol is 600 g / L. The temperature of the low-temperature ultrasonic dispersion is 10°C, the ultrasonic frequency is 80 kHz, and the distillation temperature is 60°C.

[0026] Example 3: A method for preparing a fragrant dewdrop extract, comprising the following steps:

[0027] Step 1: Wash fresh Pandanus leaves in clean water, cut them into sections, and air-dry them. Then freeze-dry them and grind them into fine powder to obtain Pandanus leaf powder. The air-drying temperature is 40℃, the freeze-drying temperature is -30℃, and the grinding pressure is 0.5MPa.

[0028] Step 2: Add the *Panax notoginseng* leaf powder to the ethanol-ether solution and stir rapidly. Let it stand at a low temperature for 2 hours, then reflux under sealed conditions for 25 minutes. After natural cooling, filter to obtain the first extract and the first filter residue. The volume ratio of ethanol to ether in the ethanol-ether solution is 1:5, the concentration of *Panax notoginseng* leaf powder in the ethanol-ether solution is 400 g / L, the stirring speed is 1200 r / min, the temperature for standing at low temperature is 8°C, and the temperature for reflux under sealed conditions is 50°C.

[0029] Step 3: The first filter residue is added to an ethanol-water solution and stirred to form a slurry. The slurry is then pressure filtered. The pressure-filtered residue and filtrate are then placed in an alkaline solution and microwaved for 2 hours. The mixture is then filtered to obtain a second filter residue and a second filtrate. The mass ratio of the first filter residue to the ethanol-water solution is 2:1, the volume percentage of ethanol in the ethanol-water solution is 55%, the pressure for pressure filtration is 0.7 MPa, and the filtration rate is 3 L / min. The alkaline solution used is a sodium hydroxide solution with a pH of 8. The mass ratio of the pressure-filtered residue to the alkaline solution is 1:4. The microwave reaction temperature is 60°C, and the microwave power is 300 W.

[0030] Step 4: Mix the first and second filtrates and adjust the pH to neutral with hydrochloric acid. After concentration under reduced pressure, dry the mixture to obtain a crude extract. Then, place the crude extract in ethanol and disperse it under low-temperature ultrasonication for 25 minutes. After filtration, distill the filtrate to obtain aromatic extract. The pressure of the reduced pressure concentration is 85% of atmospheric pressure, and the temperature is 65°C. The concentration of the crude extract in ethanol is 550 g / L. The temperature of the low-temperature ultrasonic dispersion is 8°C, the ultrasonic frequency is 70 kHz, and the distillation temperature is 55°C.

[0031] In the comparative example, fresh Pandanus leaves were washed in clean water, cut into sections, and dried. They were then microwaved in ethanol for 3 hours at a power of 300W and a temperature of 30℃. After filtration, the filtrate was distilled to obtain an extract.

[0032] Based on testing using 1 kg of Pandanus leaves as raw material and a comparative extract amount as a baseline, the following data were obtained:

[0033]

[0034] The total ion chromatogram of the extract of *Aristolochia debilis* from Example 1 is shown in the following figure. Figure 1 As shown, its varieties and contents are as follows:

[0035]

[0036] It is understood that the above detailed description of the present invention is for illustrative purposes only and is not intended to limit the technical solutions described in the embodiments of the present invention. Those skilled in the art should understand that modifications or equivalent substitutions can still be made to the present invention to achieve the same technical effects; as long as the usage requirements are met, they are all within the protection scope of the present invention.

Claims

1. A method for preparing a fragrant dewdrop extract, characterized in that: Includes the following steps: Step 1: Wash fresh Pandanus leaves in clean water, cut them into sections, and air-dry them. Then freeze-dry them and grind them into fine powder to obtain Pandanus leaf powder. The air-drying temperature is 30-50℃; the freeze-drying temperature is -30℃; and the grinding pressure is 0.4-0.6MPa. Step 2: Add the *Panax notoginseng* leaf powder to the ethanol-ether solution and stir rapidly. Let it stand at a low temperature for 1-3 hours, then reflux under sealed conditions for 20-30 minutes. After natural cooling, filter to obtain the first extract and the first filter residue. The volume ratio of ethanol to ether in the ethanol-ether solution is 1:4-5. The concentration of *Panax notoginseng* leaf powder in the ethanol-ether solution is 200-500 g / L. The stirring speed is 1000-1500 r / min. The temperature for standing at a low temperature is 5-10℃. The temperature for reflux under sealed conditions is 40-60℃. Step 3: Add the first filter residue to the ethanol aqueous solution and stir to form a slurry. Then, filter the slurry by pressure. Then, put the filter residue and filtrate into the alkaline solution and microwave react for 1-3 hours. Filter to obtain the second filter residue and the second filtrate. Step 4: Mix the first and second filtrates and adjust the pH to neutral with hydrochloric acid. After concentration under reduced pressure, dry the mixture to obtain a crude extract. Then, place the crude extract in ethanol and disperse it under low temperature and sonication for 20-30 minutes. After filtration, distill the filtrate to obtain the extract of *Aristolochia debilis*.

2. The method for preparing the *Pterocarya stenoptera* extract according to claim 1, characterized in that: In step 3, the mass ratio of the first filter residue to the ethanol-water solution is 3-5:2, the volume percentage of ethanol in the ethanol-water solution is 50-60%, the pressure of the pressure filtration is 0.6-0.7 MPa, and the pressure filtration rate is 1-5 L / min.

3. The method for preparing the *Pterocarya stenoptera* extract according to claim 1, characterized in that: The alkaline solution in step 3 is a sodium hydroxide solution with a pH of 8-8.

5. The mass ratio of the filter residue to the alkaline solution is 1:3-5. The microwave reaction temperature is 50-70℃ and the microwave power is 200-400W.

4. The method for preparing the *Panax notoginseng* extract according to claim 1, characterized in that: The pressure for vacuum concentration in step 4 is 80-90% of atmospheric pressure, and the temperature is 60-70℃.

5. The method for preparing the *Panax notoginseng* extract according to claim 1, characterized in that: In step 4, the concentration of the crude extract in ethanol is 500-600 g / L, the low-temperature ultrasonic dispersion temperature is 5-10℃, the ultrasonic frequency is 50-80 kHz, and the distillation temperature is 50-60℃.

6. The method for preparing the *Panax notoginseng* extract according to claim 1, characterized in that: The fragrant dew extract is used for flavoring tobacco, and its dosage is 0.05-0.10% of the weight of the tobacco leaves.

7. The method for preparing the *Panax notoginseng* extract according to claim 6, characterized in that: The extract of the fragrant dewdrop was diluted with ethanol and then sprayed onto the tobacco leaves.

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