A kind of liquorice processing method and application thereof

Abstract

The present invention belongs to the technical field of traditional Chinese medicine processing, and in particular, relates to a method for preparing licorice extract by processing licorice and its application. The present invention first pre-treats licorice slices with cold plasma, further adds 60-95% ethanol in a microwave reactor to microwave the licorice slices, and then repeatedly extracts them with hot reflux under the protection of an antioxidant, and finally separates and concentrates the extract to prepare an extract. In the present invention, the roasted licorice does not need to be crushed, and the active energy particles in the cold plasma are used to react with the surface of the licorice to produce surface etching, and at the same time, a large number of free radicals can be generated on the surface of the licorice to significantly increase wettability and hydrophilicity, and further cracks are generated in the microwave extraction, so that the solvent enters the interior of the licorice material and releases glycyrrhizic acid. The method of the present invention has high extraction efficiency and few impurities, and the prepared licorice extract can be widely used in various pharmaceutical preparations.

Description

Technical Field

[0001] The invention belongs to the technical field of traditional Chinese medicine processing, and in particular relates to a method for preparing liquorice extract by processing liquorice and application thereof. Background Art

[0002] Chinese medicine extract refers to the extract that is concentrated into a thick paste, block or powder after the effective ingredients in the Chinese medicinal materials are extracted with a suitable solvent, and part or all of the solvent is evaporated. Each 1 ml is equivalent to 2-5g of the original medicinal materials. Licorice extract is an extract made from licorice after processing. The common method for preparing licorice extract is the hot reflux method, which is a traditional process. Licorice is a rhizome medicinal material with a structure mainly composed of cellulose, hemicellulose and lignin. They are tightly combined and entangled with each other to form coarse fibers, which makes it difficult for the solvent to infiltrate and contact the effective ingredients, seriously affecting the extraction efficiency of the effective ingredients. In order to improve the yield, the existing technology usually extracts after crushing to increase the contact area. There is also ultrasound-assisted extraction. CN201510276959.2 grinds the licorice powder into powder and then ultrasonically treats it in 70% ethanol solvent for 60 minutes to obtain a licorice extract. The ultrasonic power is 80W and the ultrasonic frequency is 30kHz. The solid-liquid ratio of licorice powder to ethanol solvent is 1:10 (m / v); there is also a method of stirring while reflux extraction. CN201711113654.5 discloses a method for extracting bulk Chinese medicine, which uses a reflux method to extract bulk Chinese medicine, adds a composite solution with a weight ratio of 1:15-20 to the Chinese medicine, and refluxes and extracts for 2-4 hours at 60-70°C and a stirring speed of 50-100 revolutions, repeatedly extracts 3-5 times, filters the liquid medicine, and evaporates the liquid medicine to obtain the finished Chinese medicine extract. The composite solution includes methanol, ethanol, acetone, and ether. However, the extraction of licorice extract in the prior art is still not satisfactory, and there are problems such as long time, low extraction efficiency, and some methods use hazardous solvents to pollute the environment. Summary of the invention

[0003] Further improving the extraction efficiency of licorice extract, reducing energy consumption and extraction time has positive significance for the modernization of the traditional Chinese medicine industry represented by licorice. The present invention has found through repeated research and practice that in actual operation, licorice materials are usually extracted after being crushed, resulting in increased dissolved impurities, complex components in the extract, high content of starch, colloid, and flavonoid impurities, and long time consumption, high crushing energy consumption, and fine drug residues also cause pressure on filtration.

[0004] At the same time, the present invention also found in the experiment that the glycyrrhizic acid molecule is unstable and easily decomposed and oxidized. It is easy to react chemically with oxygen in the air to hydrolyze to produce two molecules of glucuronic acid and one molecule of 18β-glycyrrhetinic acid, thereby resulting in a decrease in yield and the introduction of new impurities, further reducing the purity.

[0005] Based on this, the present invention proposes the following technical solutions based on the research of these two aspects.

[0006] A liquorice processing method comprises the following steps:

[0007] (1) Cold plasma pretreatment;

[0008] (2) hot reflux extraction;

[0009] (3) Concentrate and prepare extract.

[0010] One embodiment of the present invention discloses a method for processing licorice, comprising the following steps: (1) cold plasma pretreatment; the cold plasma pretreatment comprises: placing the licorice slices into a reaction chamber of a cold plasma modification device, introducing a working gas and maintaining a certain pressure in the system, turning on the device to excite and generate plasma, and taking out the sample after treating it for a certain period of time.

[0011] Preferably, the working parameters of the cold plasma modification equipment are: input voltage 80-100V; output power 100-300W; vacuum degree 5-15Pa; working gas is one of argon and oxygen; and processing time is 5-20min.

[0012] (2) Hot reflux extraction: The hot reflux extraction is to place the cold plasma pretreated licorice slices in a microwave reactor, add 60-95% ethanol, adjust the pH to pH7.0-8.5 with sodium bicarbonate, and perform microwave treatment. Then, add 1-3% antioxidant to the microwave-treated solution, and reflux extract at 85-98°C for 1-5 hours. Microwave treatment is performed at a power of 100-1400W for 10s-300s, and set aside. Preferably, the microwave power of the microwave treatment is 800-1000w, and the microwave time is 40-120s. If the time is prolonged, the wettability will decrease.

[0013] (3) Concentrate and prepare extract.

[0014] The product after microwave reflux extraction is filtered, the filter residue is discarded, the filtrate is retained, and the condensed paste is concentrated and then dried to obtain the licorice extract. The relative density of the condensed paste is 18-20 degrees Baume (60-70°C); preferably, the drying temperature is 55-70°C and the drying time is 5-8 hours.

[0015] In the present invention, the roasted licorice root does not need to be crushed.

[0016] In the present invention, the antioxidant is selected from one or more of thiourea dioxide, sodium sulfite, sodium bisulfite, sodium thiosulfate, ferrous sulfate, vitamin C (ascorbic acid) and vitamin E.

[0017] One aspect of the present invention relates to a liquorice extract, which is prepared by the aforementioned liquorice processing method.

[0018] In one aspect of the present invention, the present invention also relates to an application of a licorice extract in preparing a medicine, wherein the medicine comprises the licorice extract product prepared by the present invention.

[0019] In one aspect of the present invention, the present invention also relates to a medicament, wherein the medicament contains licorice extract, and the licorice extract is prepared by the licorice processing method of the present invention.

[0020] The plasma treatment in the present invention utilizes active energy particles in cold plasma to react with the surface of licorice to produce surface etching, and at the same time can generate a large number of free radicals on the surface of licorice to significantly increase wettability and hydrophilicity; during the microwave extraction process, water absorbs energy in the microwave field, so that the microstructure of the licorice that has undergone surface etching further produces cracks, so that the solvent can easily enter the interior of the medicinal material through the microscopic cracks, thereby further improving the wettability of the solvent to the roasted licorice, thereby significantly improving the extraction efficiency.

[0021] On the other hand, since higher extraction temperature can significantly improve the yield, thermal energy can cause overall or local temperature increase, which affects the stability of glycyrrhizic acid. The addition of antioxidants for synergistic treatment can significantly improve the stability of glycyrrhizic acid, thereby increasing the yield.

[0022] Beneficial Effects

[0023] The present invention uses low-temperature plasma treatment in the pre-treatment step in conjunction with microwave treatment in hot reflux extraction to treat the licorice slices, which is to facilitate the dissolution of effective ingredients in the extraction process without the need for crushing, and to reduce the dissolution rate of impurities, while shortening the extraction time and reducing the filtration pressure. At the same time, antioxidants are added during the extraction process in order to protect the effective ingredients while extracting efficiently, and further improve the yield and purity of the extracted substances. DETAILED DESCRIPTION

[0024] Embodiment 1:

[0025] A liquorice processing method comprises the following steps:

[0026] 1) Cold plasma pretreatment: Place the licorice slices into the reaction chamber of the cold plasma modification equipment, introduce the working gas argon and maintain a certain pressure in the system, turn on the equipment to excite and generate plasma, and take out the sample after treating it for 5 minutes. The working parameters of the cold plasma modification equipment are input voltage 90V, output power 150W, and vacuum degree 10pa;

[0027] 2) Hot reflux extraction: Place the cold plasma pretreated licorice slices in a microwave reactor, add 95% ethanol, adjust the pH to pH 7.0 with sodium bicarbonate, and enter microwave treatment. Then add 1.5% antioxidant sodium bisulfite to the microwave-treated solution, and reflux extract at 90°C for 3 hours. The microwave reactor is set to 800W power and 120s for standby.

[0028] 3) Concentrate and prepare extract.

[0029] The product after microwave heat reflux extraction is filtered, the filter residue is discarded, the filtrate is retained, and concentrated into a paste, and then dried at a temperature of 65°C and a drying time of 6 hours. The licorice extract is obtained. The relative density of the condensed paste is 18-20 degrees Baume (60-70°C).

[0030] Embodiment 2:

[0031] A liquorice processing method comprises the following steps:

[0032] 1) Cold plasma pretreatment: Place the licorice slices into the reaction chamber of the cold plasma modification equipment, introduce the working gas argon and maintain a certain pressure in the system, turn on the equipment to excite and generate plasma, and take out the sample after treating it for 10 minutes. The working parameters of the cold plasma modification equipment are input voltage 90V, output power 200W, and vacuum degree 10pa;

[0033] 2) Hot reflux extraction: Place the cold plasma pretreated licorice slices in a microwave reactor, add 70% ethanol, adjust the pH to pH 7.0 with sodium bicarbonate, and perform microwave treatment. Then add 1.5% antioxidant vitamin C (ascorbic acid) to the microwave-treated solution, and reflux extract at 90° C. for 3 hours. The microwave reactor is set to a power of 1000 W, and the microwave treatment time is 100 s for standby use.

[0034] 3) Concentrate and prepare extract.

[0035] The product after microwave heat reflux extraction is filtered, the filter residue is discarded, the filtrate is retained, and concentrated into a paste, and then dried at a temperature of 65°C and a drying time of 6 hours. The licorice extract is obtained. The relative density of the condensed paste is 18-20 degrees Baume (60-70°C).

[0036] Example 3

[0037] A liquorice processing method comprises the following steps:

[0038] 1) Cold plasma pretreatment: Place the licorice slices into the reaction chamber of the cold plasma modification equipment, introduce the working gas argon and maintain a certain pressure in the system, turn on the equipment to excite and generate plasma, and take out the sample after treating it for 20 minutes. The working parameters of the cold plasma modification equipment are input voltage 100V, output power 250W, and vacuum degree 15pa;

[0039] 2) Hot reflux extraction: Place the cold plasma pretreated licorice slices in a microwave reactor, add 60% ethanol, adjust the pH to pH 8.0 with sodium bicarbonate, and perform microwave treatment. Then add 3% antioxidant sodium sulfite to the above solution, and reflux extract at 95°C for 2 hours. The microwave reactor is set to 800W, and the microwave treatment time is 60s for standby use.

[0040] 3) Concentrate and prepare extract.

[0041] The product after microwave heat reflux extraction is filtered, the filter residue is discarded, the filtrate is retained, and concentrated into a paste, and then dried at a temperature of 70°C and a drying time of 5 hours. The licorice extract is obtained. The relative density of the condensed paste is 18-20 degrees Baume (60-70°C).

[0042] Example 4

[0043] A liquorice processing method comprises the following steps:

[0044] 1) Cold plasma pretreatment: Place the licorice slices into the reaction chamber of the cold plasma modification equipment, introduce the working gas argon and maintain a certain pressure in the system, turn on the equipment to excite and generate plasma, and take out the sample after treating it for 7 minutes. The working parameters of the cold plasma modification equipment are input voltage 80V, output power 100W, and vacuum degree 5pa;

[0045] 2) Hot reflux extraction: Place the cold plasma pretreated licorice slices in a microwave reactor, add 70% ethanol, adjust the pH to pH 7.0 with sodium bicarbonate, and perform microwave treatment. Then add 1% antioxidant vitamin C (ascorbic acid) to the microwave-treated solution, and reflux extract at 85°C for 5 hours. The microwave reactor is set to a power of 900W, and the microwave treatment time is 100s for standby use.

[0046] 3) Concentrate and prepare extract.

[0047] The product after microwave heat reflux extraction is filtered, the filter residue is discarded, the filtrate is retained, and concentrated into a paste, and then dried at a temperature of 65°C and a drying time of 6 hours. The licorice extract is obtained. The relative density of the condensed paste is 18-20 degrees Baume (60-70°C).

[0048] Example 5

[0049] A liquorice processing method comprises the following steps:

[0050] 1) Cold plasma pretreatment: Place the licorice slices into the reaction chamber of the cold plasma modification equipment, introduce the working gas argon and maintain a certain pressure in the system, turn on the equipment to excite and generate plasma, and take out the sample after treating it for 20 minutes. The working parameters of the cold plasma modification equipment are input voltage 100V, output power 250W, and vacuum degree 15pa;

[0051] 2) Hot reflux extraction: Place the cold plasma pretreated licorice slices in a microwave reactor, add 70% ethanol, adjust the pH to pH 8.0 with sodium bicarbonate, and perform microwave treatment. Then add 3% antioxidant sodium sulfite to the above solution, and reflux extract at 95°C for 2 hours. The microwave reactor is set to 800W, and the microwave treatment time is 60s for standby use.

[0052] 3) Concentrate and prepare extract.

[0053] The product after microwave heat reflux extraction is filtered, the filter residue is discarded, the filtrate is retained, and concentrated into a paste, and then dried at a temperature of 70°C and a drying time of 5 hours. The licorice extract is obtained. The relative density of the condensed paste is 18-20 degrees Baume (60-70°C).

[0054] Comparative Example 1:

[0055] A method for processing licorice, which differs from Example 3 in that there is no cold plasma pretreatment step, but the licorice pieces are directly subjected to heat reflux treatment and then concentrated to prepare an extract. That is:

[0056] A liquorice processing method comprises the following steps:

[0057] 1) Hot reflux extraction: Place the licorice slices in a microwave reactor, add 60% ethanol, adjust the pH to pH 8.0 with sodium bicarbonate, and perform microwave treatment. Then add 3% antioxidant sodium sulfite to the above solution, and reflux extract at 95° C. for 2 hours. The microwave reactor is set to 800 W, and the microwave treatment time is 60 s, and then set aside.

[0058] 2) Concentrate and prepare extract.

[0059] The product after microwave heat reflux extraction is filtered, the filter residue is discarded, the filtrate is retained, and concentrated into a paste, and then dried at a temperature of 70°C and a drying time of 5 hours. The licorice extract is obtained. The relative density of the condensed paste is 18-20 degrees Baume (60-70°C).

[0060] Comparative Example 2:

[0061] A method for processing liquorice, which differs from Example 3 in that microwave treatment is not used in the heat reflux treatment after the cold plasma pretreatment step, and then the extract is concentrated to prepare.

[0062] A liquorice processing method comprises the following steps:

[0063] 1) Cold plasma pretreatment: Place the licorice slices into the reaction chamber of the cold plasma modification equipment, introduce the working gas argon and maintain a certain pressure in the system, turn on the equipment to excite and generate plasma, and take out the sample after treating it for 20 minutes. The working parameters of the cold plasma modification equipment are input voltage 100V, output power 250W, and vacuum degree 15pa;

[0064] 2) Hot reflux extraction: Place the licorice slices pretreated with low-temperature plasma in a reactor, add 60% ethanol, and adjust the pH to 8.0 with sodium bicarbonate. Then add 3% antioxidant sodium sulfite to the solution and reflux extract at 95°C for 2 hours.

[0065] 3) Concentrate and prepare extract.

[0066] The product after hot reflux extraction is filtered, the filter residue is discarded, the filtrate is retained, and concentrated into a paste, and then dried at a temperature of 70°C and a drying time of 5 hours. The licorice extract is obtained. The relative density of the condensed paste is 18-20 degrees Baume (60-70°C).

[0067] Comparative Example 3:

[0068] A method for processing liquorice, which differs from Example 3 in that no antioxidant is added during the heat reflux treatment, and then the extract is concentrated to prepare the extract.

[0069] A liquorice processing method comprises the following steps:

[0070] 1) Cold plasma pretreatment: Place the licorice slices into the reaction chamber of the cold plasma modification equipment, introduce the working gas argon and maintain a certain pressure in the system, turn on the equipment to excite and generate plasma, and take out the sample after treating it for 20 minutes. The working parameters of the cold plasma modification equipment are input voltage 100V, output power 250W, and vacuum degree 15pa;

[0071] 2) Hot reflux extraction: Place the licorice slices pretreated with low-temperature plasma in a microwave reactor, add 60% ethanol, adjust the pH to pH 8.0 with sodium bicarbonate, and perform microwave treatment. Then, reflux extraction is performed at 95°C for 2 hours. The microwave reactor is set to a power of 800W, and the microwave treatment time is 60s, and then set aside.

[0072] 3) Concentrate and prepare extract.

[0073] The product after microwave heat reflux extraction is filtered, the filter residue is discarded, the filtrate is retained, and concentrated into a paste, and then dried at a temperature of 70°C and a drying time of 5 hours. The licorice extract is obtained. The relative density of the condensed paste is 18-20 degrees Baume (60-70°C).

[0074] Table 1 Licorice extract and glycyrrhizic acid and impurity content

[0075]

[0076]

[0077] It can be seen from the table that plasma combined with microwave treatment can significantly improve the yield of licorice extract and increase the content of glycyrrhizic acid, the active ingredient. The addition of antioxidants can reduce the oxidation of the active ingredient during extraction, resulting in a decrease in content. In addition, it can be seen from the table that the concentration of the organic solvent also affects the extraction efficiency of the active ingredient.

[0078] The above content is a further detailed description of the present invention in combination with specific implementation methods. It cannot be determined that the specific implementation of the present invention is limited to these descriptions. For ordinary technicians in the technical field to which the present invention belongs, several simple deductions or substitutions can be made without departing from the concept of the present invention, which should be regarded as belonging to the scope of protection determined by the claims submitted for the present invention.

Claims

1. A method for processing liquorice, characterized in that: The method comprises the following steps: (1) Cold plasma pretreatment: Place the licorice slices into the reaction chamber of the cold plasma modification equipment, introduce the working gas and maintain the system at a certain pressure, turn on the equipment to excite and generate plasma, and the working parameters of the cold plasma modification equipment are: input voltage 80~100V; output power 100~300W; vacuum degree 5~15Pa, the working gas is one of argon and oxygen; the sample processing time is 5~20min; (2) Hot reflux extraction: Place the cold plasma pretreated licorice slices in a microwave reactor, add 60-95% ethanol, adjust the pH to pH 7.0-8.5 with sodium bicarbonate, and perform microwave treatment. The microwave power of the microwave treatment is 800-1000w and the microwave time is 40-120s. Then, add 1-3% antioxidant to the microwave-treated solution and reflux extract at 85-98°C for 1-5 hours. (3) Concentrating to prepare extract: filtering the product after microwave reflux extraction, discarding the filter residue, retaining the filtrate, concentrating it into a paste, and then drying it at a temperature of 55-70°C and a drying time of 5-8 hours to obtain the licorice extract, wherein the relative density of the condensed paste is 18-20 degrees Baume.

2. A liquorice extract, characterized in that: The licorice extract is prepared by the method according to claim 1.

3. The use of liquorice extract in preparing a medicament, characterized in that: The licorice extract is prepared by the method according to claim 1.

4. A medicament containing liquorice extract, characterized in that: The licorice extract is prepared by the method according to claim 1.

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