Honeysuckle-containing composition as well as preparation process and application thereof

Abstract

The invention relates to the technical field of honeysuckle extraction, and provides a honeysuckle-containing composition as well as a preparation process and application thereof. The preparation process of the honeysuckle flower extract comprises the following steps: S1, taking honeysuckle flowers, adding water, and extracting to obtain a first extracting solution; s2, concentrating the first extracting solution to obtain a concentrate, adding a mixed solvent, and performing ultrasonic extraction to obtain a second extracting solution; s3, concentrating the second extracting solution to obtain a honeysuckle flower extract; the mixed solvent comprises ethanol and ethylene glycol. Through the technical scheme, the problem of low chlorogenic acid content in the honeysuckle flower extract in the prior art is solved.

Description

Technical Field

[0001] The invention relates to the technical field of honeysuckle extraction, and specifically to a composition containing honeysuckle, and a preparation process and application thereof. Background Art

[0002] As a traditional Chinese medicinal material, honeysuckle is widely used in many fields such as medicine, food, and cosmetics. Its main active ingredient, chlorogenic acid, has many excellent pharmacological activities such as antibacterial, antiviral, and antioxidant. The market is in urgent need of high-content chlorogenic acid products. However, there are many limitations in the traditional honeysuckle extraction process, which makes it difficult to achieve the ideal level of chlorogenic acid in the extract. On the one hand, conventional extraction methods such as solvent extraction are difficult to accurately separate chlorogenic acid from complex plant tissues due to the extensive extraction conditions, and a large amount of chlorogenic acid remains in the drug residue; on the other hand, the process lacks systematic optimization, and the key parameters such as temperature, time, and solvent concentration in the extraction process fail to accurately adapt to the dissolution characteristics of chlorogenic acid, resulting in low extraction efficiency. In this context, it is urgent to develop a new process that can significantly increase the content of chlorogenic acid in honeysuckle extracts, which can not only meet the growing demand of various industries for high-quality honeysuckle extracts, but also promote the in-depth development of honeysuckle-related industries, and inject new impetus into the modernization of traditional Chinese medicine and the development of high value-added products.

[0003] In summary, it is crucial to develop an extraction process for honeysuckle extract with a high content of chlorogenic acid. Summary of the invention

[0004] The invention provides a composition containing honeysuckle and a preparation process and application thereof, which solves the problem of low chlorogenic acid content in honeysuckle extract in the related art.

[0005] The technical solution of the present invention is as follows: The present invention provides a preparation process of a honeysuckle extract, comprising the following steps: S1, taking honeysuckle, adding water, extracting, and obtaining a first extract; S2, concentrating the first extract to obtain a concentrate, adding a mixed solvent, and performing ultrasonic extraction to obtain a second extract; S3, concentrating the second extract to obtain the honeysuckle extract; The mixed solvent includes ethanol and ethylene glycol.

[0006] As a further technical solution, the mass volume ratio of honeysuckle to water in S1 is 1g:10~20mL, the extraction temperature is 80~90°C, and the extraction time is 1~3h.

[0007] As a further technical solution, the mass volume ratio of the concentrate to the mixed solvent in S2 is 1 g:15~25 mL, and the volume ratio of ethanol to ethylene glycol in the mixed solvent is 20:1~3.

[0008] In the present invention, the volume ratio of ethanol to ethylene glycol is adjusted to 20:1-3, thereby further improving the extraction rate of honeysuckle.

[0009] As a further technical solution, the temperature of the ultrasonic extraction in S2 is 30-50°C, the time is 0.5-1.5h, and the power is 150W.

[0010] As a further technical solution, after the concentration in S3, elution and drying are further included, and during the elution, a macroporous adsorption resin column is used, and the volume of the eluent is 3 to 5 times the volume of the macroporous adsorption resin column; The eluent includes water.

[0011] As a further technical solution, the eluent also includes an aqueous succinic acid solution and an aqueous lactic acid solution, the concentrations of the aqueous succinic acid solution and the aqueous lactic acid solution are independently 0.005-0.015 mol / L, and the volume ratio of water, succinic acid and lactic acid is 100:3-5:1.

[0012] The eluent in the present invention also includes a succinic acid aqueous solution and a lactic acid aqueous solution, and the addition of the two further improves the extraction rate of honeysuckle.

[0013] The present invention also provides a honeysuckle-containing composition, which comprises the honeysuckle extract obtained by the preparation process of the honeysuckle extract.

[0014] As a further technical solution, the honeysuckle-containing composition includes the following components in parts by weight: 35-50 parts of honeysuckle extract, 10-20 parts of licorice, 10-20 parts of isatis root, and 10-18 parts of dandelion.

[0015] The present invention also proposes a preparation process of the composition containing honeysuckle, comprising the following steps: A1. Grind liquorice, isatis root and dandelion into powder and sieve to obtain mixed Chinese medicine powder; A2, boiling the mixed Chinese herbal powder with water, collecting the supernatant, filtering and concentrating to obtain a mixed Chinese herbal extract; A3. Mix the honeysuckle extract with water and then mix it with the mixed Chinese herbal medicine extract to prepare a honeysuckle-containing composition.

[0016] The present invention also proposes the application of the honeysuckle-containing composition obtained by the preparation process of the honeysuckle-containing composition in the field of antibacterial.

[0017] The working principle and beneficial effects of the present invention are: In the present invention, a mixed solvent of ethanol and ethylene glycol is used for ultrasonic extraction, thereby improving the extraction rate of honeysuckle. In addition, through three-step extraction, the extraction rate of spinach seed is improved, thereby solving the problem of low extraction rate of the existing honeysuckle extraction process. DETAILED DESCRIPTION

[0018] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0019] Example 1 A preparation process of a composition containing honeysuckle comprises the following steps: A1. Grind 20 parts of liquorice, 20 parts of isatis root and 18 parts of dandelion into powder and sieve to obtain a mixed Chinese medicine powder; A2. Decoction the mixed Chinese herbal powder with water (the mass volume ratio of the mixed Chinese herbal powder to water is 1 g:25 mL), collect the supernatant, filter and concentrate to obtain a mixed Chinese herbal extract; A3, mixing 50 parts of honeysuckle extract with water (the mass volume ratio of honeysuckle extract to water is 1 g:15 mL), and then mixing with the mixed Chinese herbal medicine extract to prepare a composition containing honeysuckle; The preparation process of honeysuckle extract comprises the following steps: S1. Take 100 g of honeysuckle, add water, and extract at 90° C. for 1 h to obtain a first extract; S2, concentrating the first extract to obtain a concentrate, adding a mixed solvent, and ultrasonically extracting at 50° C. for 0.5 h with an ultrasonic power of 150 W to obtain a second extract; S3, concentrating the second extract to obtain a honeysuckle extract; The mass volume ratio of honeysuckle to water is 1g:20mL; The mass volume ratio of the concentrate to the mixed solvent is 1 g:25 mL, and the mixed solvent is a mixture of ethanol and ethylene glycol in a volume ratio of 4:1.

[0020] Example 2 A preparation process of a composition containing honeysuckle comprises the following steps: A1. Grind 10 parts of liquorice, 10 parts of isatis root and 10 parts of dandelion into powder and sieve to obtain a mixed Chinese medicine powder; A2. Add water to the mixed Chinese herbal powder and boil it (the mass volume ratio of the mixed Chinese herbal powder to water is 1 g:15 mL), collect the supernatant, filter and concentrate to obtain a mixed Chinese herbal extract; A3, mixing 35 parts of honeysuckle extract with water (the mass volume ratio of honeysuckle extract to water is 1 g:5 mL), and then mixing with the mixed Chinese herbal medicine extract to prepare a honeysuckle-containing composition; The preparation process of honeysuckle extract comprises the following steps: S1. Take 100 g of honeysuckle, add water, and extract at 80° C. for 3 h to obtain a first extract; S2, concentrating the first extract to obtain a concentrate, adding a mixed solvent, and ultrasonically extracting at 30° C. for 1.5 h with an ultrasonic power of 150 W to obtain a second extract; S3, concentrating the second extract to obtain a honeysuckle extract; The mass volume ratio of honeysuckle to water is 1g:10mL; The mass volume ratio of the concentrate to the mixed solvent is 1 g:15 mL, and the mixed solvent is a mixture of ethanol and ethylene glycol in a volume ratio of 40:1.

[0021] Example 3 A preparation process of a composition containing honeysuckle comprises the following steps: A1. Grind 15 parts of liquorice, 15 parts of isatis root and 15 parts of dandelion into powder and sieve to obtain a mixed Chinese medicine powder; A2. Decoction the mixed Chinese herbal powder with water (the mass volume ratio of the mixed Chinese herbal powder to water is 1 g:20 mL), collect the supernatant, filter and concentrate to obtain a mixed Chinese herbal extract; A3, mixing 45 parts of honeysuckle extract with water (the mass volume ratio of honeysuckle extract to water is 1 g: 10 mL), and then mixing with the mixed Chinese herbal medicine extract to prepare a honeysuckle-containing composition; The preparation process of honeysuckle extract comprises the following steps: S1. Take 100 g of honeysuckle, add water, and extract at 85° C. for 2 h to obtain a first extract; S2, concentrating the first extract to obtain a concentrate, adding a mixed solvent, and ultrasonically extracting at 40° C. for 1 h with an ultrasonic power of 150 W to obtain a second extract; S3, concentrating the second extract to obtain a honeysuckle extract; The mass volume ratio of honeysuckle to water is 1g:15mL; The mass volume ratio of the concentrate to the mixed solvent is 1 g:20 mL, and the mixed solvent is a mixture of ethanol and ethylene glycol in a volume ratio of 25:1.

[0022] Example 4 The only difference between this embodiment and embodiment 3 is that the mixed solvent in this embodiment is a mixture of ethanol and ethylene glycol in a volume ratio of 5:1.

[0023] Example 5 The only difference between this embodiment and embodiment 3 is that the mixed solvent in this embodiment is a mixture of ethanol and ethylene glycol in a volume ratio of 20:1.

[0024] Example 6 The only difference between this embodiment and embodiment 3 is that the mixed solvent in this embodiment is a mixture of ethanol and ethylene glycol in a volume ratio of 10:1.

[0025] Example 7 The only difference between this embodiment and embodiment 3 is that the mixed solvent in this embodiment is a mixture of ethanol and ethylene glycol in a volume ratio of 20:3.

[0026] Example 8 The only difference between this embodiment and embodiment 6 is that the preparation process of the honeysuckle extract in this embodiment includes the following steps: S1. Take 100 g of honeysuckle, add water, and extract at 85° C. for 2 h to obtain a first extract; S2, concentrating the first extract to obtain a concentrate, adding a mixed solvent, and ultrasonically extracting at 40° C. for 1 h with an ultrasonic power of 150 W to obtain a second extract; S3, concentrating the second extract, eluting with a macroporous adsorption resin column, and drying to obtain a honeysuckle extract; The volume of the eluent is 4 times the volume of the macroporous adsorption resin column, and the eluent is a mixed eluent consisting of water, succinic acid aqueous solution, and lactic acid aqueous solution in a volume ratio of 100:6:1; The mass volume ratio of honeysuckle to water in S1 is 1 g:15 mL; The mass volume ratio of the concentrate to the mixed solvent is 1 g:20 mL, and the mixed solvent is a mixture of ethanol and ethylene glycol in a volume ratio of 25:1.

[0027] Example 9 The only difference between this embodiment and embodiment 8 is that the eluent of this embodiment is a mixed eluent consisting of water, succinic acid aqueous solution and lactic acid aqueous solution in a volume ratio of 100:2:1.

[0028] Example 10 The only difference between this embodiment and embodiment 8 is that the eluent of this embodiment is a mixed eluent consisting of water, succinic acid aqueous solution and lactic acid aqueous solution in a volume ratio of 100:3:1.

[0029] Embodiment 11 The only difference between this embodiment and embodiment 8 is that the eluent of this embodiment is a mixed eluent consisting of water, succinic acid aqueous solution and lactic acid aqueous solution in a volume ratio of 100:4:1.

[0030] Example 12 The only difference between this embodiment and embodiment 8 is that the eluent of this embodiment is a mixed eluent consisting of water, succinic acid aqueous solution and lactic acid aqueous solution in a volume ratio of 100:5:1.

[0031] Comparative Example 1 The difference between this comparative example and Example 2 is that the preparation process of the honeysuckle extract in this comparative example comprises the following steps: S1. Take 100 g of honeysuckle, add water, and extract at 80° C. for 3 h to obtain a first extract; S2, concentrating the first extract to obtain a concentrate, adding ethanol, and ultrasonically extracting at 30° C. for 1.5 h with an ultrasonic power of 150 W to obtain a second extract; S3, concentrating the second extract to obtain a honeysuckle extract; The mass volume ratio of honeysuckle to water is 1g:10mL; The mass volume ratio of the concentrate to ethanol is 1 g:15 mL.

[0032] Comparative Example 2 The difference between this comparative example and Example 2 is that the preparation process of the honeysuckle extract in this comparative example comprises the following steps: S1. Take 100 g of honeysuckle, add water, and extract at 80° C. for 3 h to obtain a first extract; S2, concentrating the first extract to obtain a concentrate, adding ethylene glycol, and ultrasonically extracting at 30° C. for 1.5 h with an ultrasonic power of 150 W to obtain a second extract; S3, concentrating the second extract to obtain a honeysuckle extract; The mass volume ratio of honeysuckle to water is 1g:10mL; The mass volume ratio of the concentrate to ethylene glycol is 1 g:15 mL.

[0033] Comparative Example 3 The difference between this comparative example and Example 2 is that the preparation process of the honeysuckle extract in this comparative example comprises the following steps: S1. Take 100 g of honeysuckle, add a mixed solvent, and perform ultrasonic extraction at 30° C. for 1.5 h with an ultrasonic power of 150 W to obtain a first extract; S2, concentrating the first extract to obtain a concentrate, adding water, and extracting at 80° C. for 3 h to obtain a second extract; S3, concentrating the second extract to obtain a honeysuckle extract; The mass volume ratio of honeysuckle and the mixed solvent is 1g:15mL, and the mixed solvent is a mixture of ethanol and ethylene glycol in a volume ratio of 40:1; The mass volume ratio of the concentrate to water is 1 g:10 mL.

[0034] Test Example 1 Honeysuckle Extraction Rate Test The content of chlorogenic acid in the honeysuckle extract obtained in Examples 1 to 12 and Comparative Examples 1 to 3 was detected by high performance liquid chromatography (HPLC). The detection conditions mainly include: instrument: Waters high performance liquid chromatograph, detector: Waters 2996 diode array detector, chromatographic column: Symmetry ODS column (4.6×150 mm, 5 μm), mobile phase: acetonitrile-0.4% phosphoric acid (8:92), detection wavelength of 327 nm, flow rate: 1.0 mL / min, column temperature: 40°C, and the number of theoretical plates calculated based on the chlorogenic acid peak should not be less than 3000. The test results are shown in Table 1.

[0035]

[0036] Comparing Example 2 with Comparative Examples 1 and 2, it is shown that the present invention uses a mixed solvent of ethanol and ethylene glycol for extraction, which increases the chlorogenic acid content in the honeysuckle extract. Comparing Example 2 with Comparative Example 3, it is shown that the present invention uses the sequence of first water extraction and then alcohol extraction to increase the chlorogenic acid content in the honeysuckle extract.

[0037] Comparing Examples 5 to 7 with Examples 3 to 4, it is shown that when the volume ratio of ethanol to ethylene glycol is adjusted to 20:1 to 3 in the present invention, the chlorogenic acid content in the honeysuckle extract is further increased. Comparing Example 6 with Examples 5 and 7, it is shown that when the volume ratio of ethanol to ethylene glycol is adjusted to 10:1 in the present invention, the chlorogenic acid content in the honeysuckle extract is further increased. Comparing Examples 8 to 12 with Example 6, it is shown that the use of a mixed eluent consisting of water, an aqueous succinic acid solution, and an aqueous lactic acid solution for elution in the present invention further increases the chlorogenic acid content in the honeysuckle extract. Comparing Examples 10 to 12 with Examples 8 to 9, it is shown that when the volume ratio of water, an aqueous succinic acid solution, and an aqueous lactic acid solution is 100:3 to 5:1, the chlorogenic acid content in the honeysuckle extract is further increased. Comparing Example 11 with Examples 10 and 12, it is shown that when the volume ratio of water, an aqueous succinic acid solution, and an aqueous lactic acid solution is 100:4:1, the effect of increasing the chlorogenic acid content in the honeysuckle extract is the best.

[0038] Test Example 2 Antibacterial Effect Test The antibacterial properties of the compositions containing honeysuckle prepared in Example 2 and Comparative Examples 1-3 were determined by the following method: The antibacterial effect of the gel on the tested bacteria (ER2738 Escherichia coli, Staphylococcus aureus ATCC 22004) was determined by agar diffusion paper method and colony counting method. 8 CFU / mL of the test bacterial suspension is evenly spread on the surface of the solidified nutrient agar medium plate, 100 μL per plate; under sterile conditions, the composition containing honeysuckle is spread on a sterilized and dried filter paper with a diameter of 0.3 cm, and the prepared paper piece containing the honeysuckle (with the sterilized filter paper as a blank control) is pasted on the plate coated with the test strain, and four paper pieces are placed on each plate, and cultured at 37°C for 24 hours, and the contact surface culture is taken for gradient elution to prepare a diluted bacterial suspension, 1 mL of the diluted bacterial suspension is taken into the plate, and the plate is poured with agar, mixed, and after solidification, it is inverted and cultured at 37°C for 24 hours, and the total number of colonies is calculated. The calculation method of the total number of colonies refers to the method in GB47892-2010 "National Food Safety Standard for Determination of Total Number of Colonies in Food Microbiological Examination"; Inhibition rate (100%) = (total number of colonies in blank control - total number of colonies in gel) / total number of colonies in blank control × 100; The measurement results are shown in Table 2.

[0039] Table 2 Antibacterial test results of the gels in Example 2 and Comparative Examples 1 to 3

[0040] Comparing Example 2 with Comparative Examples 1 to 3, it is shown that the composition containing honeysuckle prepared by the present invention has a good antibacterial effect.

[0041] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A process for preparing a honeysuckle extract, characterized in that: The following steps are involved: S1, taking honeysuckle, adding water, extracting, and obtaining a first extract; S2, concentrating the first extract to obtain a concentrate, adding a mixed solvent, and performing ultrasonic extraction to obtain a second extract; S3, concentrating the second extract to obtain the honeysuckle extract; The mixed solvent includes ethanol and ethylene glycol.

2. The preparation process of the honeysuckle extract according to claim 1, characterized in that: The mass volume ratio of honeysuckle to water in S1 is 1 g: 10-20 mL, the extraction temperature is 80-90° C., and the extraction time is 1-3 h.

3. The preparation process of the honeysuckle extract according to claim 1, characterized in that: The mass volume ratio of the concentrate to the mixed solvent in S2 is 1 g:15-25 mL, and the volume ratio of ethanol to ethylene glycol in the mixed solvent is 20:1-3.

4. The preparation process of the honeysuckle extract according to claim 1, characterized in that: The temperature of the ultrasonic extraction in S2 is 30-50°C, the time is 0.5-1.5h, and the power is 150W.

5. The preparation process of the honeysuckle extract according to claim 1, characterized in that: After the concentration in S3, elution and drying are further included, wherein the elution is performed using a macroporous adsorption resin column, and the volume of the eluent is 3 to 5 times the volume of the macroporous adsorption resin column; The eluent includes water.

6. The process for preparing the honeysuckle extract according to claim 5, characterized in that: The eluent also includes a succinic acid aqueous solution and a lactic acid aqueous solution, the concentrations of the succinic acid aqueous solution and the lactic acid aqueous solution are independently 0.005-0.015 mol / L, and the volume ratio of water, the succinic acid aqueous solution and the lactic acid aqueous solution is 100:3-5:

1.

7. A composition containing honeysuckle, characterized in that A honeysuckle extract obtained by the preparation process of the honeysuckle extract according to any one of claims 1 to 6.

8. The composition containing honeysuckle according to claim 7, characterized in that: The invention comprises the following components in parts by weight: 35-50 parts of honeysuckle extract, 10-20 parts of liquorice, 10-20 parts of isatis root and 10-18 parts of dandelion.

9. The process for preparing a composition containing honeysuckle according to any one of claims 7 to 8, characterized in that: The following steps are involved: A1. Grind liquorice, isatis root and dandelion into powder and sieve to obtain mixed Chinese medicine powder; A2, boiling the mixed Chinese herbal powder with water, collecting the supernatant, filtering and concentrating to obtain a mixed Chinese herbal extract; A3. Mix the honeysuckle extract with water and then mix it with the mixed Chinese herbal medicine extract to prepare a honeysuckle-containing composition.

10. Use of the honeysuckle-containing composition according to any one of claims 7 to 8 or the honeysuckle-containing composition obtained by the preparation process according to claim 9 in the field of antibacterial.

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