Composition containing semen ziziphi spinosae as well as preparation process and application of composition

Abstract

The invention relates to the technical field of semen ziziphi spinosae extraction, and provides a semen ziziphi spinosae-containing composition as well as a preparation process and application thereof. The preparation process of the spina date seed extract comprises the following steps: S1, adding spina date seeds into water, extracting and filtering to obtain first filtrate and filter residues; s2, soaking the filter residue with an acid solution, and filtering to obtain a second filtrate; s3, mixing the first filtrate and the second filtrate to obtain a mixed solution, performing alcohol precipitation by using a solvent, and performing filtration, concentration and drying to obtain a spina date seed extract; the acid solution is a mixed solution of an acetic acid aqueous solution and a lactic acid aqueous solution; the solvent comprises ethanol. According to the technical scheme, the problem that the extraction rate of spina date seeds is low in the prior art is solved.

Description

Technical Field

[0001] The invention relates to the technical field of extracting wild jujube seeds, and in particular to a composition containing wild jujube seeds, and a preparation process and application thereof. Background Art

[0002] Suanzaoren is rich in a variety of active ingredients, such as saponins, flavonoids, alkaloids, etc. These ingredients play a key role in regulating the nervous system, soothing emotions, promoting sleep, etc., and are the material basis for its effective anti-inflammatory effect. In addition to Suanzaoren, synergistic Chinese medicines such as Poria cocos and Angelica sinensis also contain unique active ingredients, which can cooperate with each other.

[0003] However, there are many challenges in extracting active ingredients from Chinese date seeds. Traditional extraction methods, such as decoction, are simple to operate and low in cost, but they have problems such as low extraction efficiency, easy loss of heat-sensitive components, and a large number of impurities, which limits the purity of active ingredients and affects the efficacy of the medicine. Although organic solvent extraction can improve the extraction rate, it is easy to leave residual organic solvents, which brings safety risks and cumbersome subsequent processing.

[0004] Therefore, it is of great significance to accurately and efficiently obtain the active ingredients in Chinese jujube seeds and improve the extraction rate. Summary of the invention

[0005] The invention provides a composition containing wild jujube seeds and a preparation process and application thereof, which solves the problem of low extraction rate of wild jujube seeds in the related art.

[0006] The technical solution of the present invention is as follows: The present invention provides a preparation process of a Chinese date seed extract, comprising the following steps: S1, adding Chinese date seeds into water, extracting, filtering, and obtaining a first filtrate and a filter residue; S2, soaking the filter residue in an acid solution, filtering, and obtaining a second filtrate; S3, mixing the first filtrate and the second filtrate to obtain a mixed solution, using a solvent to perform alcohol precipitation, filtering, concentrating, and drying to obtain a jujube seed extract; The acid solution is a mixed solution of an acetic acid aqueous solution and a lactic acid aqueous solution; The solvent includes ethanol.

[0007] As a further technical solution, the mass volume ratio of the Chinese date kernel to water is 1 g: 10-20 mL, the extraction temperature is 80-90° C., and the extraction time is 3-4 h.

[0008] As a further technical solution, the soaking temperature is 45-65° C. and the soaking time is 1-3 hours.

[0009] As a further technical solution, the concentrations of the acetic acid aqueous solution and the lactic acid aqueous solution are independently 0.005-0.015 mol / L.

[0010] As a further technical solution, the mass volume ratio of the filter residue to the acid solution is 1g:8~12mL.

[0011] As a further technical solution, the volume ratio of the acetic acid aqueous solution to the lactic acid aqueous solution is 7-9:1.

[0012] When the volume ratio of the acetic acid aqueous solution to the lactic acid aqueous solution is adjusted to 7-9:1 in the present invention, the extraction rate of the spinach seed is further improved.

[0013] As a further technical solution, the volume ratio of the mixed liquid to the solvent is 1:2-3; the temperature of the alcohol precipitation is 5-10°C, and the time is 24-36h.

[0014] As a further technical solution, the solvent also includes hydroxytyrosol, and the volume ratio of the ethanol to hydroxytyrosol is 15-20:1.

[0015] In the invention, hydroxytyrosol is added to the solvent, so that the extraction rate of the spiny jujube seeds is further improved; when the volume ratio of ethanol to hydroxytyrosol is adjusted to 15-20:1, the extraction rate of the spiny jujube seeds is further improved.

[0016] The invention also provides a composition containing Chinese jujube seeds, comprising the Chinese jujube seeds extract obtained by the preparation process of the Chinese jujube seeds extract.

[0017] The present invention also provides a composition containing Chinese jujube seeds, comprising the following components in parts by weight: 30-50 parts of Chinese jujube seed extract, 10-20 parts of Poria cocos, 5-15 parts of Angelica sinensis, 2-10 parts of Lilium, and 8-16 parts of Astragalus.

[0018] The present invention also proposes a preparation process of a composition containing spiny jujube seeds, comprising the following steps: A1. Powder Poria cocos, Chinese angelica, lily and astragalus 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, dissolving the spiny jujube seed extract in water and mixing the mixture with the mixed Chinese medicinal extract to prepare a composition containing the spiny jujube seed.

[0019] As a further technical solution, in step A2, the mass volume ratio of the mixed Chinese medicine powder and water is 1g:20~30mL.

[0020] As a further technical solution, in step A3, the mass volume ratio of the Ziziphus jujuba seed extract and water is 1 g: 10-20 mL.

[0021] The invention also proposes the application of the composition containing spinosa jujube seeds obtained by the preparation process in the field of anti-inflammation.

[0022] The working principle and beneficial effects of the present invention are: In the present invention, a mixed solution of an acetic acid aqueous solution and a lactic acid aqueous solution is used to soak the filter residue, thereby improving the extraction rate of the spinach seed and solving the problem of low extraction rate of the spinach seed. In addition, after two-step extraction and then alcohol precipitation, the extraction rate of the spinach seed is improved. DETAILED DESCRIPTION

[0023] 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.

[0024] Example 1 A preparation process of a composition containing spiny jujube seeds comprises the following steps: A1. Grind 10 parts of Poria cocos, 5 parts of Chinese Angelica sinensis, 2 parts of Lilium bulbs, and 8 parts of Astragalus membranaceus 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, after mixing 30 parts of the spiny jujube seed extract with water (the mass volume ratio of the spiny jujube seed extract to water is 1g:10mL), mixed with the mixed Chinese herbal medicine extract to prepare a composition containing the spiny jujube seed; The preparation process of the Chinese date seed extract comprises the following steps: S1. Add 100 g of spiny jujube kernels into 1 L of water, extract at 90° C. for 3 h, and filter to obtain a first filtrate and a filter residue; S2, soaking the filter residue in an acid solution at 65° C. for 1 h, with the mass volume ratio of the filter residue to the acid solution being 1 g:12 mL, and filtering to obtain a second filtrate; S3, the first filtrate and the second filtrate are mixed to obtain a mixed solution, and a solvent is used for alcohol precipitation at 10° C. for 24 hours, and the mixture is filtered, concentrated, and dried to obtain a jujube seed extract; The acid solution is a mixed solution of an acetic acid aqueous solution and a lactic acid aqueous solution in a volume ratio of 15:1; the concentrations of the acetic acid aqueous solution and the lactic acid aqueous solution are both 0.015 mol / L; The solvent is ethanol, and the volume ratio of the solvent to the mixed liquid is 1:3.

[0025] Example 2 A preparation process of a composition containing spiny jujube seeds comprises the following steps: A1. Grind 20 parts of Poria cocos, 15 parts of Chinese Angelica sinensis, 10 parts of Lilium bulbs, and 16 parts of Astragalus membranaceus 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:30 mL), collect the supernatant, filter and concentrate to obtain a mixed Chinese herbal extract; A3, after mixing 50 parts of the spinach seed extract with water (the mass volume ratio of the spinach seed extract to water is 1g:20mL), mixing with the mixed Chinese herbal medicine extract to prepare a composition containing the spinach seed; The preparation process of the Chinese date seed extract comprises the following steps: S1. Add 100 g of Chinese jujube kernels into 2 L of water, extract at 80° C. for 4 h, and filter to obtain a first filtrate and a filter residue; S2, soaking the filter residue in an acid solution at 45° C. for 3 h, with the mass volume ratio of the filter residue to the acid solution being 1 g:8 mL, and filtering to obtain a second filtrate; S3, the first filtrate and the second filtrate are mixed to obtain a mixed solution, and the mixed solution is subjected to alcohol precipitation at 5°C for 36 hours, filtered, concentrated, and dried to obtain a jujube seed extract; The acid solution is a mixed solution of an acetic acid aqueous solution and a lactic acid aqueous solution in a volume ratio of 5:1; the concentrations of the acetic acid aqueous solution and the lactic acid aqueous solution are both 0.005 mol / L; The solvent is ethanol, and the volume ratio of the solvent to the mixed liquid is 1:2.

[0026] Example 3 A preparation process of a composition containing spiny jujube seeds comprises the following steps: A1. Grind 15 parts of Poria cocos, 10 parts of Chinese Angelica sinensis, 6 parts of Lilium bulbs, and 12 parts of Astragalus membranaceus 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, after mixing 40 parts of the spiny jujube seed extract with water (the mass volume ratio of the spiny jujube seed extract to water is 1g:15mL), mixed with the mixed Chinese herbal medicine extract to prepare a composition containing the spiny jujube seed; The preparation process of the Chinese date seed extract comprises the following steps: S1. Add 100 g of spinach kernels into 1.5 L of water, extract at 85° C. for 3.5 h, and filter to obtain a first filtrate and a filter residue; S2, soaking the filter residue in an acid solution at 55° C. for 2 h, with the mass volume ratio of the filter residue to the acid solution being 1 g:10 mL, and filtering to obtain a second filtrate; S3, the first filtrate and the second filtrate are mixed to obtain a mixed solution, and a solvent is used for alcohol precipitation at 8°C for 30 hours, and the mixture is filtered, concentrated, and dried to obtain a jujube seed extract; The acid solution is a mixed solution of an acetic acid aqueous solution and a lactic acid aqueous solution in a volume ratio of 6:1; the concentrations of the acetic acid aqueous solution and the lactic acid aqueous solution are both 0.010 mol / L; The solvent is ethanol.

[0027] Example 4 The only difference between this embodiment and embodiment 3 is that the acid solution in this embodiment is a mixed solution of an acetic acid aqueous solution and a lactic acid aqueous solution in a volume ratio of 10:1.

[0028] Example 5 The only difference between this embodiment and embodiment 4 is that the acid solution in this embodiment is a mixed solution of an acetic acid aqueous solution and a lactic acid aqueous solution in a volume ratio of 7:1.

[0029] Example 6 The only difference between this embodiment and embodiment 4 is that the acid solution in this embodiment is a mixed solution of an acetic acid aqueous solution and a lactic acid aqueous solution in a volume ratio of 8:1.

[0030] Example 7 The only difference between this embodiment and embodiment 4 is that the acid solution in this embodiment is a mixed solution of an acetic acid aqueous solution and a lactic acid aqueous solution in a volume ratio of 9:1.

[0031] Example 8 The only difference between this embodiment and embodiment 6 is that, in this embodiment, the solvent further includes hydroxytyrosol, and the volume ratio of ethanol to hydroxytyrosol is 25:1.

[0032] Example 9 The only difference between this embodiment and embodiment 6 is that, in this embodiment, the solvent further includes hydroxytyrosol, and the volume ratio of ethanol to hydroxytyrosol is 10:1.

[0033] Example 10 The only difference between this embodiment and embodiment 6 is that, in this embodiment, the solvent further includes hydroxytyrosol, and the volume ratio of ethanol to hydroxytyrosol is 15:1.

[0034] Embodiment 11 The only difference between this embodiment and embodiment 6 is that, in this embodiment, the solvent further includes hydroxytyrosol, and the volume ratio of ethanol to hydroxytyrosol is 17:1.

[0035] Example 12 The only difference between this embodiment and embodiment 6 is that, in this embodiment, the solvent further includes hydroxytyrosol, and the volume ratio of ethanol to hydroxytyrosol is 20:1.

[0036] Comparative Example 1 The only difference between this comparative example and Example 2 is that the acid solution is an aqueous solution of acetic acid with a concentration of 0.005 mol / L.

[0037] Comparative Example 2 The only difference between this comparative example and Example 2 is that the acid solution is a lactic acid aqueous solution with a concentration of 0.005 mol / L.

[0038] Comparative Example 3 The only difference between this comparative example and Example 2 is that the acid solution is a mixed solution of an acetic acid aqueous solution and an formic acid aqueous solution in a volume ratio of 5:1; the concentrations of the acetic acid aqueous solution and the formic acid aqueous solution are both 0.005 mol / L.

[0039] Comparative Example 4 The only difference between this comparative example and Example 2 is that the acid solution is a mixed solution of an acetic acid aqueous solution and a propionic acid aqueous solution in a volume ratio of 5:1; the concentrations of the acetic acid aqueous solution and the propionic acid aqueous solution are both 0.005 mol / L.

[0040] Comparative Example 5 The only difference between this comparative example and Example 2 is that the acid solution is a mixed solution of an acetic acid aqueous solution and a malic acid aqueous solution in a volume ratio of 5:1; the concentrations of the acetic acid aqueous solution and the malic acid aqueous solution are both 0.005 mol / L.

[0041] Comparative Example 6 The only difference between this comparative example and Example 2 is that the acid solution is a mixed solution of an acetic acid aqueous solution and a citric acid aqueous solution in a volume ratio of 5:1; the concentrations of the acetic acid aqueous solution and the citric acid aqueous solution are both 0.005 mol / L.

[0042] Comparative Example 7 The only difference between this comparative example and Example 2 is that the acid solution is a mixed solution of an acetic acid aqueous solution and a hydrochloric acid aqueous solution in a volume ratio of 5:1; the concentrations of the acetic acid aqueous solution and the hydrochloric acid aqueous solution are both 0.005 mol / L.

[0043] Comparative Example 8 The difference between this comparative example and Example 2 is that in this comparative example, the preparation process of the spiny jujube seed extract comprises the following steps: S1. Add 100 g of Chinese jujube kernels into 2 L of water, extract at 80 °C for 4 h, and filter to obtain a filtrate and a filter residue; S2, using a solvent to precipitate the filtrate with alcohol at 5°C for 36 hours, filtering, concentrating, and drying to obtain a Ziziphus jujuba seed extract; The solvent includes ethanol, and the volume ratio of the solvent to the filtrate is 1:2.

[0044] Test Example 1: Extraction rate test of spinach seed The extracts of the Chinese jujube seeds obtained in Examples 1 to 12 and Comparative Examples 1 to 8 were tested to detect the content of Chinese jujube saponin in the Chinese jujube seed extract. The test method is as follows: The content of Chinese jujube saponin A and Chinese jujube saponin B in the Chinese jujube seed extract was simultaneously determined by high performance liquid chromatography-mass spectrometry, and the chromatographic conditions were as follows: octadecylsilane bonded silica gel was filled, 0.1wt% formic acid solution was used as mobile phase A, acetonitrile was used as mobile phase B, isocratic elution was performed, and the flow rate was 0.15mL / min. The test results are shown in Table 1.

[0045] The extraction rate of jujube saponin A is a (mg / g), a=(1000×a 1 ×m) / 100g; Extraction rate of jujube saponin B b (mg / g), b = (1000 × b 1 ×m) / 100g; a 1 (g / g) is the concentration of jujuboside A in the sample measured by HPLC-MS, b 1 (g / g) is the concentration of jujube seed saponin B in the sample measured by HPLC-MS / MS, and m (g) is the total amount of jujube seed extract; Table 1 Extraction rates of jujuboside A and jujuboside B from jujube seeds

[0046] The mixed solution of the solution is used to soak the filter residue, thereby improving the extraction rate of the spinach seed. Comparing Example 2 with Comparative Example 8, it is shown that the present invention improves the extraction rate of the spinach seed by two-step extraction and then alcohol precipitation.

[0047] Comparing Examples 5 to 7 with Examples 3 to 4, it is shown that when the volume ratio of the aqueous acetic acid solution to the aqueous lactic acid solution is 7 to 9:1, the extraction rate of the Chinese jujube seeds is further improved. Comparing Example 6 with Examples 5 and 7, it is shown that when the volume ratio of the aqueous acetic acid solution to the aqueous lactic acid solution is 8:1, the extraction rate of the Chinese jujube seeds is further improved. Comparing Example 6 with Examples 8 to 12, it is shown that when the solvent also includes hydroxytyrosol, the extraction rate of the Chinese jujube seeds is further improved. Comparing Examples 10 to 12 with Examples 8 to 9, it is shown that when the volume ratio of ethanol to hydroxytyrosol is adjusted to 15 to 20:1 in the present invention, the extraction rate of the Chinese jujube seeds is further improved. Comparing Example 11 with Examples 10 and 12, it is shown that when the volume ratio of ethanol to hydroxytyrosol is adjusted to 17:1 in the present invention, the effect of improving the extraction rate of the Chinese jujube seeds is the best, solving the problem of low extraction rate of the Chinese jujube seeds.

[0048] Test Example 2 Anti-inflammatory Effect Test 80 mice, half male and half female, were randomly divided into 4 groups, i.e. 20 mice in each group, including a blank control group (administered with an equal amount of physiological saline), Example 1 group (the Chinese medicine composition used was the Chinese medicine composition prepared in Example 1), Example 2 group (the Chinese medicine composition used was the Chinese medicine composition prepared in Example 2), and Example 3 group (the Chinese medicine composition used was the Chinese medicine composition prepared in Example 3). The mice were given 0.5 g / 10 g of the drug for 7 consecutive days. 30 minutes after the last administration, xylene was applied to both sides of the right ear at 0.03 mL / mouse, and the left ear was used as a control. The mice were killed by cervical dislocation 30 minutes later, and both ears were cut off along the baseline of the auricle. The ear pieces were removed and weighed at the symmetrical positions of the left and right ears using a 7 mm diameter puncher. The swelling of the auricle of the mice was observed, and the swelling inhibition rate was calculated; Ear swelling (mg) = right auricle mass - left auricle mass; Swelling inhibition rate (%) = (average ear swelling degree of blank control group - average ear swelling degree of drug-treated group) / average ear swelling degree of blank control group × 100%.

[0049] Table 2 Effect of xylene-induced ear swelling in mice

[0050] The anti-inflammatory test results shown in Table 2 show that the composition containing Semen Ziziphi Spinosae prepared by the present invention can inhibit xylene-induced ear swelling in mice and has a good anti-inflammatory effect.

[0051] 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 preparation process of a Chinese date seed extract, characterized in that: The following steps are involved: S1, adding Chinese date seeds into water, extracting, filtering, and obtaining a first filtrate and a filter residue; S2, soaking the filter residue in an acid solution, filtering, and obtaining a second filtrate; S3, mixing the first filtrate and the second filtrate to obtain a mixed solution, using a solvent to perform alcohol precipitation, filtering, concentrating, and drying to obtain a jujube seed extract; The acid solution is a mixed solution of an acetic acid aqueous solution and a lactic acid aqueous solution; The solvent includes ethanol.

2. The preparation process of the Chinese date seed extract according to claim 1, characterized in that: The mass volume ratio of the sour jujube kernel to water is 1g:10-20mL, the extraction temperature is 80-90°C, and the extraction time is 3-4h.

3. The preparation process of the Chinese date seed extract according to claim 1, characterized in that: The soaking temperature is 45-65°C and the soaking time is 1-3 hours; Preferably, the concentrations of the acetic acid aqueous solution and the lactic acid aqueous solution are independently 0.005-0.015 mol / L; Preferably, the mass volume ratio of the filter residue to the acid solution is 1 g:8-12 mL.

4. The preparation process of the Chinese date seed extract according to claim 3, characterized in that: The volume ratio of the acetic acid aqueous solution to the lactic acid aqueous solution is 7-9:

1.

5. The preparation process of the Chinese date seed extract according to claim 1, characterized in that: The volume ratio of the mixed solution to the solvent is 1:2-3; the temperature of the alcohol precipitation is 5-10°C, and the time is 24-36h.

6. The preparation process of the Chinese date seed extract according to claim 1, characterized in that: The solvent also includes hydroxytyrosol, and the volume ratio of the ethanol to the hydroxytyrosol is 15-20:

1.

7. A composition containing Semen Ziziphi Spinosae, characterized in that: The invention relates to a Chinese jujube seed extract obtained by the preparation process of a Chinese jujube seed extract according to any one of claims 1 to 6.

8. The composition containing Semen Ziziphi Spinosae according to claim 7, characterized in that: The invention comprises the following components in parts by weight: 30-50 parts of spinosa jujube seed extract, 10-20 parts of tuckahoe, 5-15 parts of angelica sinensis, 2-10 parts of lily and 8-16 parts of astragalus.

9. The process for preparing a composition containing spiny jujube seeds according to any one of claims 7 to 8, characterized in that: The following steps are involved: A1. Powder Poria cocos, Chinese angelica, lily and astragalus 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. Mixing the spiny jujube seed extract with water and then mixing with the mixed Chinese medicinal extract to prepare a composition containing the spiny jujube seed.

10. Use of the composition containing spiny jujube seeds according to any one of claims 7 to 8 or the composition containing spiny jujube seeds obtained by the preparation process according to claim 9 in the field of anti-inflammatory.

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