Bitter almond extract and its preparation method and application

Abstract

The present invention relates to the technical field of traditional Chinese medicine processing, and in particular to a bitter almond extract and a preparation method and application thereof. The preparation method of the bitter almond extract comprises the following steps: taking bitter almond medicinal materials, crushing them to a particle size range of 1 mm to 20 mm, adding water equivalent to 2 to 5 times the weight of the bitter almond medicinal materials within 0 to 24 hours, soaking them for 2 to 6 hours, and then immersing them at 3 to 8 mL kg ‑1 ·min ‑1 The bitter almond extract is distilled and extracted at a speed of 10000 to 20000, and the distillate is collected in an amount equivalent to 0.8 to 1.2 times the weight of the bitter almond medicinal material. The content of hydrocyanic acid in the bitter almond extract can be maintained in the range of 0.08% to 0.12%, and has good quality stability.

Description

Technical Field

[0001] The invention relates to the technical field of traditional Chinese medicine processing, in particular to a bitter almond extract and a preparation method and application thereof. Background Art

[0002] Jianer Qingjie Liquid has the effects of clearing away heat and detoxifying, eliminating stagnation and harmonizing the stomach. It can be used for cough and sore throat, loss of appetite, and abdominal distension. It is made from 6 herbs including honeysuckle, chrysanthemum, forsythia, tangerine peel, hawthorn, and bitter almond.

[0003] Among them, bitter almonds contain amygdalin, which decomposes to produce trace amounts of hydrocyanic acid, which has an inhibitory effect on the respiratory center, achieving antitussive and antiasthmatic effects. However, excessive inhalation of hydrocyanic acid in a short period of time will inhibit respiratory enzymes, lead to intracellular suffocation, and cause poisoning. Therefore, it is of great significance to use the hydrocyanic acid content in almond extract as a quality control indicator.

[0004] Jianer Qingjie Solution currently complies with the Ministry of Health's "Chinese Medicine Formula Preparations" Volume 10 (Standard No.: WS3-B-2015-95) and Pharmacopoeia Industry Development

[2003] No. 522, and the National Drug Administration's standard (Standard No.: WS3-B-2015-2002). Among them, the standard describes the extraction of bitter almonds as "bitter almond distillation to extract aromatic water", that is, it only stipulates the extraction method of bitter almonds, and does not clearly stipulate the specific process parameters in the bitter almond extraction process. Therefore, it is particularly important to determine the parameters of the bitter almond extraction process. Summary of the invention

[0005] The present invention aims to solve at least one of the technical problems existing in the prior art. To this end, the present invention provides a bitter almond extract and a preparation method and application thereof, which can ensure the content of hydrocyanic acid in the bitter almond extract by determining the process parameters in the bitter almond extraction process, improve the extraction operability of bitter almonds, stabilize the production process, reduce batch differences, and thus stabilize product quality.

[0006] The first aspect of the present invention provides a method for preparing a bitter almond extract, comprising the following steps:

[0007] Take bitter almond medicinal material, grind it into a particle size range of 1mm to 20mm, add water equivalent to 2 to 5 times the weight of bitter almond medicinal material within 0 to 24 hours, soak for 2 to 6 hours, and then adjust the temperature according to 3 to 8mL kg -1 ·min -1 Distill and extract at a speed of , and collect distillate equivalent to 0.8 to 1.2 times the weight of the bitter almond medicinal material.

[0008] For the extraction of bitter almonds, when the bitter almonds are treated by decoction, direct heating will inactivate amygdalinase, reduce the amount of hydrocyanic acid obtained by decomposition, and affect the yield of hydrocyanic acid. Amygdalin will decompose into hydrocyanic acid under the action of amygdalinase in cold water. Therefore, the present invention adopts the soaking-distillation method to prepare bitter almond extract. Further determining the particle size of the medicinal material, the treatment time limit, the amount of soaking water, the soaking time, the distillation speed and the amount of distillate collected can effectively control the hydrocyanic acid content in the almond extract within the target range (0.08% to 0.12%).

[0009] According to some embodiments of the present invention, the step further includes: the particle size range is 1 mm to 10 mm.

[0010] The present invention uses bitter almond coarse powder with a particle size of 1mm to 10mm for feeding, which can increase the contact area between the medicinal material and the solvent and fully extract the effective component. When the bitter almond medicinal material coarse powder is less than 1mm, the specific surface area of ​​the powder increases, and the contact with the air is more sufficient during the same storage time. Amygdalin forms hydrocyanic acid under the action of enzymes and volatilizes into the air, which leads to a decrease in the effective component before water extraction. At the same time, the powder is too fine and will block the bottom filter screen of the extraction tank, resulting in difficulty in draining and affecting production efficiency. On the contrary, when the bitter almond is crushed to be greater than 10mm, the effective component is not fully and completely extracted within the same time, resulting in the hydrocyanic acid content in the extract not meeting the enterprise standard.

[0011] According to some embodiments of the present invention, the bitter almond medicinal material is soaked in water within 0 to 16 hours after being crushed.

[0012] When freshly crushed bitter almonds come into contact with moisture in the air, amygdalin is decomposed into hydrocyanic acid under the action of enzymes. Hydrocyanic acid is volatile, so storing it for too long will affect the yield of hydrocyanic acid in the almond extract. The processed coarse powder should be used within 16 hours to ensure minimal loss of active ingredients during storage.

[0013] According to some embodiments of the present invention, the soaking time is 1 to 3 hours.

[0014] Soaking for too long will increase the risk of microbial growth, resulting in reduced product quality; and it will easily cause the content of hydrocyanic acid in the distillate to increase, which will not meet quality control requirements.

[0015] According to some embodiments of the present invention, the soaking temperature is 10°C to 30°C.

[0016] According to some embodiments of the present invention, the mass ratio of the distillate to the bitter almond medicinal material is 1:1.

[0017] According to some embodiments of the present invention, the distillation rate is 3 to 8 mL·kg -1 ·min-1 Including but not limited to: 3~6mL·kg -1 ·min -1 , 3~5mL·kg -1 ·min -1 , 3~4mL·kg -1 ·min -1 , 4~8mL·kg -1 ·min -1 , 4~6mL·kg -1 ·min -1 , 4~5mL·kg -1 ·min -1 , 5~8mL·kg -1 ·min -1 , 5~6mL·kg -1 ·min -1 , 6~8mL·kg -1 ·min -1 、8mL·kg -1 ·min -1 、6mL·kg -1 ·min -1 , 5mL·kg -1 ·min -1 , 4mL·kg -1 ·min -1 、3mL·kg -1 ·min -1 .

[0018] According to some embodiments of the present invention, the distillation temperature is 90°C to 110°C.

[0019] According to some embodiments of the present invention, the cooling temperature of the distillation is 10°C to 30°C.

[0020] According to some embodiments of the present invention, the distillation is atmospheric distillation.

[0021] The second aspect of the present invention provides a bitter almond extract prepared by the above-mentioned preparation method.

[0022] According to some embodiments of the present invention, the content of hydrocyanic acid in the bitter almond extract is 0.08% to 0.12%.

[0023] According to some preferred embodiments of the present invention, the content of hydrocyanic acid in the bitter almond extract is 0.10% to 0.12%.

[0024] The internal control standard of hydrocyanic acid in the bitter kernel extract of Jianer Qingjie Solution is 0.08% to 0.12%. Hydrocyanic acid has an inhibitory effect on the respiratory center, achieving antitussive and antiasthmatic effects. Too little hydrocyanic acid will not have a therapeutic effect. On the contrary, if too much hydrocyanic acid is inhaled in a short period of time, it will inhibit respiratory enzymes, cause intracellular suffocation, and cause poisoning.

[0025] The bitter almond extract prepared by the present invention is preferably sealed and stored in a cold place to ensure the stability of the content of hydrocyanic acid in the bitter almond extract.

[0026] The third aspect of the present invention provides a Jianer Qingjie solution, comprising the bitter almond extract mentioned above.

[0027] According to some embodiments of the present invention, the content of bitter almond extract in the Jianer Qingjie solution is 15.0-45.0 μg / mL, calculated as hydrocyanic acid (HCN).

[0028] According to some embodiments of the present invention, the Jianer Qingjie solution also includes honeysuckle extract, chrysanthemum extract, forsythia extract, tangerine peel extract, and hawthorn extract.

[0029] Beneficial effects:

[0030] (1) The present invention clarifies the pretreatment method of bitter almonds, which are first crushed into coarse particles before feeding, and clarifies the shelf life after crushing, so as to avoid extraction differences caused by different crushing sizes, and also avoid the deterioration of medicinal materials due to long storage time, which affects the extraction of effective components;

[0031] (2) The present invention clarifies the key process parameters in the almond distillation extraction process, such as the type and amount of solvent added during the distillation extraction of bitter almonds, the extraction time and extraction rate during the distillation extraction process, and the amount of distillate collected at the end, which can ensure that the content of hydrocyanic acid in the almond extract is within the range of 0.08% to 0.12%, which helps to stabilize the quality of the almond extract;

[0032] (3) The present invention has the advantages of being simple to implement, highly operable, and having good reproducibility.

[0033] 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 present invention. DETAILED DESCRIPTION

[0034] The following will be combined with the embodiments to clearly and completely describe the concept of the present invention and the technical effects produced, so as to fully understand the purpose, characteristics and effects of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, other embodiments obtained by those skilled in the art without creative work are all within the scope of protection of the present invention.

[0035] It should be noted that the experimental methods described in the following examples are conventional methods unless otherwise specified, and the reagents and materials are commercially available unless otherwise specified.

[0036] The bitter almond medicinal material of the present invention is provided by Bozhou Shangpintang Chinese Medicine Pieces Co., Ltd.

[0037] Example 1

[0038] S1. Pretreatment of medicinal materials: Select bitter almond medicinal materials to remove foreign matter and impurities, and then crush or coarsely grind the medicinal materials into particles ranging from 1mm to 10mm;

[0039] S2. After 8 hours, put the processed herbs into a multifunctional extraction tank, add 4 times the weight of the herbs, that is, the total weight of herbs in each tank (kg): solvent volume (L) = 1:4, soak at room temperature for 2 hours, then start heating and distillation, the distillation temperature is 100℃, the distillation pressure is normal pressure, and the cooling temperature is room temperature. -1 ·min -1 The distillate is collected at a distillation rate of 5 mL / min. -1 ·min -1 ×Total amount of medicinal materials per can (kg);

[0040] S3. Collect the distillate, the total amount collected (kg) = the total amount of medicinal materials input (kg);

[0041] S4. The distillate is collected into a designated storage tank and mixed evenly to obtain bitter almond extract.

[0042] Example 2

[0043] S1. Pretreatment of medicinal materials: Select bitter almond medicinal materials to remove foreign matter and impurities, and then crush or coarsely grind the medicinal materials into particles ranging from 1mm to 10mm;

[0044] S2. After 4 hours, put the processed herbs into a multifunctional extraction tank, add 3 times the weight of the herbs, that is, the total weight of the herbs in each tank (kg): solvent volume (L) = 1:3, soak at room temperature for 3 hours, and start heating and distillation after soaking. The distillation temperature is 100℃, the distillation pressure is normal pressure, and the cooling temperature is room temperature. -1 ·min -1 The distillate is collected at a distillation rate of 100%, that is, the amount collected per minute (mL) = 4 mL kg -1 ·min -1 ×Total amount of medicinal materials per can (kg);

[0045] S3. Collect the distillate, the total amount collected (kg) = the total amount of medicinal materials input (kg);

[0046] S4. The distillate is collected into a designated storage tank and mixed evenly to obtain bitter almond extract.

[0047] Example 3

[0048] S1. Pretreatment of medicinal materials: Select bitter almond medicinal materials to remove foreign matter and impurities, and then crush or coarsely grind the medicinal materials into particles ranging from 1mm to 10mm;

[0049] S2. After 10 hours, put the processed herbs into a multifunctional extraction tank, add 5 times the weight of the herbs, that is, the total weight of the herbs in each tank (kg): the volume of the solvent (L) = 1:5, soak at room temperature for 2 hours, and start heating and distillation after soaking. The distillation temperature is 100℃, the distillation pressure is normal pressure, and the cooling temperature is room temperature. -1 ·min -1 The distillate is collected at a distillation rate of 100%, that is, the amount collected per minute (mL) = 6 mL kg -1 ·min -1 ×Total amount of medicinal materials per can (kg);

[0050] S3. Collect the distillate, the total amount collected (kg) = the total amount of medicinal materials input (kg);

[0051] S4. The distillate is collected into a designated storage tank and mixed evenly to obtain bitter almond extract.

[0052] Example 4

[0053] S1. Pretreatment of medicinal materials: Select bitter almond medicinal materials to remove foreign matter and impurities, and then crush or coarsely grind the medicinal materials into particles ranging from 1mm to 10mm;

[0054] S2. After 14 hours, put the processed herbs into a multifunctional extraction tank, add 5 times the weight of the herbs, that is, the total weight of the herbs in each tank (kg): the volume of the solvent (L) = 1:5, soak at room temperature for 3 hours, and start heating and distillation after soaking. The distillation temperature is 100℃, the distillation pressure is normal pressure, and the cooling temperature is room temperature. -1 ·min -1 The distillate is collected at a distillation rate of 100 mL / min, i.e., the amount collected per minute (mL) = 8 mL kg -1 ·min -1 ×Total amount of medicinal materials per can (kg);

[0055] S3. Collect the distillate, the total amount collected (kg) = the total amount of medicinal materials input (kg);

[0056] S4. The distillate is collected into a designated storage tank and mixed evenly to obtain bitter almond extract.

[0057] Example 5

[0058] S1. Pretreatment of medicinal materials: Select bitter almond medicinal materials to remove foreign matter and impurities, and then crush or coarsely grind the medicinal materials into particles ranging from 1mm to 10mm;

[0059] S2. After 6 hours, put the processed herbs into a multifunctional extraction tank, add 3 times the weight of the herbs, that is, the total weight of the herbs in each tank (kg): the volume of the solvent (L) = 1:3, soak at room temperature for 3 hours, and start heating and distillation after soaking. The distillation temperature is 100℃, the distillation pressure is normal pressure, and the cooling temperature is room temperature. -1 ·min -1 The distillate is collected at a distillation rate of 100%, that is, the amount collected per minute (mL) = 3mL·kg -1 ·min -1 ×Total amount of medicinal materials per can (kg);

[0060] S3. Collect the distillate, the total amount collected (kg) = the total amount of medicinal materials input (kg);

[0061] S4. The distillate is collected into a designated storage tank and mixed evenly to obtain bitter almond extract.

[0062] Comparative Example 1

[0063] Refer to the experimental steps of Example 1, except that the processed bitter almond medicinal material is used after being placed for 26 hours.

[0064] Comparative Example 2

[0065] Refer to the experimental steps of Example 1, except that the bitter almond medicinal material is crushed to a particle size range of 30 mm.

[0066] Comparative Example 3

[0067] Refer to the experimental steps of Example 1, except that the solid-liquid ratio of bitter almond medicinal material to water is 1:1.5 kg / L.

[0068] Comparative Example 4

[0069] Refer to the experimental steps of Example 1, except that the solid-liquid ratio of bitter almond medicinal material to water is 1:6 kg / L.

[0070] Comparative Example 5

[0071] Refer to the experimental steps of Example 1, except that the immersion time is 8 hours.

[0072] Comparative Example 6

[0073] The experimental steps of Example 1 are as follows, except that the distillation rate is 12 mL kg -1 ·min -1 .

[0074] Test Case

[0075] (1) Characteristic analysis

[0076] Sensory evaluation of the color, odor and taste of bitter almond extract.

[0077] (2) Detection of Hydrocyanic Acid Content

[0078] The detection method is as follows: accurately measure 25mL, add 100mL of water, add 2mL of potassium iodide test solution and 1mL of ammonia test solution, and slowly titrate with silver nitrate titration solution (0.1mol / L) until the yellow-white turbidity of the solution does not disappear. Each 1mL of silver nitrate titration solution (0.1mol / L) is equivalent to 5.405mg of HCN.

[0079] The bitter almond extracts obtained in Examples 1 to 5 and Comparative Examples 1 to 6 were subjected to property analysis and hydrocyanic acid content testing. The test results are shown in Table 1.

[0080] Table 1 Test results of bitter almond extracts of Examples 1 to 5 and Comparative Examples 1 to 6

[0081]

[0082]

[0083] It can be seen from the test results in Table 1 that the bitter almond extracts prepared in Examples 1 to 5 have contents controlled at 0.08% to 0.12%, which meet the quality control standards in the industry; and are all colorless clear liquids with a special odor similar to that of bitter almonds and a slightly spicy taste.

[0084] In Comparative Example 1, the bitter almond medicinal material was crushed for 26 hours before use. The bitter almond coarse powder showed a clumping phenomenon, and the hydrocyanic acid content after extraction was only 0.07%, which did not meet the enterprise standard.

[0085] The particle size of the bitter almond coarse powder in Comparative Example 2 is 30 mm, and the effective ingredients are not fully and completely extracted, resulting in the hydrocyanic acid content in the extract not meeting the enterprise standard.

[0086] In Comparative Example 3, the solid-liquid ratio of bitter almond medicinal materials to the solvent was 1:1.5. After the medicinal materials were soaked and absorbed water, they emerged from the water surface, which failed to achieve a complete soaking effect, and the hydrocyanic acid content was lower than the internal control standard. In Comparative Example 4, the solid-liquid ratio of bitter almond medicinal materials to the solvent was 1:6. During the extraction process, hydrocyanic acid dissolved in water and could not be distilled out with water vapor. The extraction was incomplete, and the hydrocyanic acid content was lower than the enterprise standard.

[0087] The soaking time of comparative example 5 is 8 hours, the number of microorganisms may increase, and the production efficiency is reduced; and the soaking time is too long, the hydrocyanic acid decomposed by amygdalin under the action of enzymes is more fully dissolved in water, and the content of hydrocyanic acid in the extract increases accordingly. However, the higher the content of hydrocyanic acid, the better. If too much hydrocyanic acid is inhaled in a short period of time, it will inhibit respiratory enzymes, cause intracellular suffocation, and cause poisoning.

[0088] The distillation rate of Comparative Example 6 is 12 mL kg -1 ·min -1 , the extraction speed is too fast, the almond extract obtained has a slight odor and a low content of hydrocyanic acid.

[0089] The above content describes the embodiments of the present invention in detail, but the present invention is not limited to the above embodiments. Various changes can be made within the knowledge of ordinary technicians in the relevant technical field without departing from the purpose of the present invention. In addition, the embodiments of the present invention and the features in the embodiments can be combined with each other without conflict.

Claims

1. A method for preparing a bitter almond extract, characterized in that: The steps include: Take bitter almond medicinal materials, grind them into particles ranging from 1mm to 10mm, put them into a multifunctional extraction tank within 0 to 16 hours, add water equivalent to 2 to 5 times the weight of bitter almond medicinal materials, soak them at 10℃ to 30℃ for 1 to 3 hours, and then adjust the temperature according to 3 to 8mL·kg -1 ·min -1 The product is extracted by distillation at a speed of 90-110°C, cooled at 10-30°C, and the distillate is collected in an amount equivalent to 0.8-1.2 times the weight of the bitter almond medicinal material. Wherein, the content of hydrocyanic acid in the bitter almond extract is 0.08% to 0.12%.

2. A bitter almond extract, characterized in that Prepared by the preparation method described in claim 1.

3. A Jianer Qingjie solution, characterized in that: The invention comprises the bitter almond extract according to claim 2.

4. The Jianer Qingjie solution according to claim 3, characterized in that Calculated in terms of hydrocyanic acid (HCN), the content of the bitter almond extract in the Jianer Qingjie solution is 15.0-45.0 μg / mL.

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