CN112603945A - Wild jujube kernel powder and preparation method thereof - Google Patents
Wild jujube kernel powder and preparation method thereof Download PDFInfo
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
The invention discloses wild jujube kernel powder and a preparation method thereof, and the wild jujube kernel powder comprises the following steps: s1, preparing spina date seed powder for later use; s2, preparing first and second intermediate semen Ziziphi Spinosae powders; s3, preparing a third intermediate spina date seed powder; s4, weighing the second intermediate spina date seed powder prepared in the step S2 and the third intermediate spina date seed powder prepared in the step S3, respectively grinding and sieving the two powder for later use, and uniformly mixing the powder according to a proper proportion to prepare the spina date seed powder. The wild jujube kernel powder disclosed by the invention is convenient to take, fast to disperse, easy to absorb, high in bioavailability and stable in quality, can be swallowed, sucked or dispersed with water, is particularly suitable for the old and people with dysphagia, and is beneficial to popularization and application of the wild jujube kernel powder.
Description
Technical Field
The invention relates to the technical field of health food and medicine processing, in particular to wild jujube kernel powder and a preparation method thereof.
Background
With the increasing social competition, the increasing pace of work and life, and the influence of various factors such as environment, the mental stress borne by people is increasing, the incidence rate of insomnia is on a rising trend, and the insomnia is a serious problem threatening the health of the public. The long-term insomnia can cause a series of organism damages such as the reduction of attention, judgment, memory daily working capacity and the like, and seriously affect the health condition, the life quality, the working efficiency and other aspects of people, so that the development of safe and effective sedative-hypnotic natural active ingredients and products thereof has great significance.
The spina date seed is a dry mature seed of a Rhamnaceae plant spina date, is produced in northern areas of China, is a traditional natural plant food material with definite effects of nourishing the heart and soothing the nerves in China, is recorded as spina date seed porridge as early as the original generation 'diet essentials', and can treat consumptive disease, vexation and insomnia. Modern clinical and pharmacological tests prove that the spina date seed has obvious sedative-hypnotic effect and anticonvulsant effect and has the characteristics of nature, safety, high efficiency and the like. The jujuboside is the main active component of jujuboside with sedative and hypnotic effects, and many researches show that jujuboside (represented by jujuboside A, B) can achieve sedative and hypnotic effects through multiple mechanisms. The flavonoids in the spina date seeds have antioxidant activity and can effectively remove free radicals. The alkaloids compounds in semen Ziziphi Spinosae include semen Ziziphi Spinosae alkali A, B, D, E, F, Gl, G2, Ia, Ib, K, N-methyl Bapo alkali, Prunine, 5-hydroxy-6-methoxy noraporphine, Ampelopsin (ampibiine), semen Ziziphi Spinosae cyclic peptide (sanjoinenine), and magnoflorine (magnoflorine) with anticonvulsive effect. In addition, the spina date seed also contains about 32% of fatty acid components in parts by mass on average, wherein the fatty acid components comprise unsaturated fatty acids such as oleic acid, linoleic acid, palmitic acid and the like, and the unsaturated fatty acids enable the spina date seed to have the functions of resisting inflammation, oxidation, bacteria and tumors and the like. Betulinic acid in the spina date seed and spina date seed oil show good antitumor activity, and researches show that the betulinic acid in the spina date seed can inhibit the growth of more than ten tumor cells such as human colon cancer cells HT-29, human ovarian cancer cells A2780, human oral epithelial cancer cells KB and the like, and the inhibition effect is increased along with the increase of the dose of the betulinic acid. Therefore, the chemical components of the spina date seeds are very complex, the pharmacological activities and action mechanisms of various chemical components are different, and the different components can have synergistic action and adverse effects mutually.
However, the pharmacological action research on different components of the spine date seed in the prior art has obvious defects, and the self components of the dispersible tablet prepared by adopting the spine date seed extract as the main component are still complex, for example, four groups of essential components in the spine date seed dispersible tablet disclosed in the literature 'research on measuring the contents of two components in the spine date seed dispersible tablet by the HPLCELSD method' (brilliant, Asia-Pacific traditional medicine, No. 8, No. 11) comprise the bestatin, the spina date seed saponin A, B and the betulinic acid, wherein the bestatin belongs to a flavonoid compound, the spina date seed saponin A, B belongs to the spina date seed saponin, and the betulinic acid belongs to the lupane triterpenoid compound. Therefore, the spina date seed dispersible tablets in the prior art have insufficient refinement degree of spina date seed extraction, may have adverse effects among different components, and reduce the sedative and hypnotic effects of the spina date seed dispersible tablets. In addition, the common tablet in the prior art is an application form of the spina date seed saponin extract. The tablets usually affect the full absorption of the medicine due to the disintegration and slow medicine dissolution; meanwhile, when the dosage is large and the dosage needs to be taken once, the trouble is often brought to the old, children and patients with dysphagia.
Disclosure of Invention
The invention aims to provide wild jujube kernel powder and a preparation method thereof aiming at the defects in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a preparation method of wild jujube kernel powder, which comprises the following steps:
s1, drying the spina date seeds, crushing the spina date seeds into particles by using a crusher, sieving, adding the particles into petroleum ether at 70-80 ℃ to prepare a petroleum ether soaking solution, gently placing the petroleum ether soaking solution into a Soxhlet extractor for reflux extraction until the petroleum ether soaking solution is colorless, removing an extracting solution, and naturally drying the rest substances to obtain spina date seed powder for later use;
s2, mixing the wild jujube seed powder obtained after natural air drying in the step S1 with ethanol to obtain a mixed solution, then placing the mixed solution in a water bath kettle for refluxing, carrying out centrifugal filtration, and naturally air drying the obtained solid matter to obtain first middle wild jujube seed powder; collecting filtrate, rotary evaporating to remove liquid, pre-freezing the rest materials in refrigerator, and freeze drying to obtain second intermediate semen Ziziphi Spinosae powder;
s3, putting the first intermediate spina date seed powder prepared in the step S2 into a Soxhlet extractor, and refluxing with chloroform; volatilizing chloroform from the residue, placing in a round-bottom flask, reflux-extracting with methanol for 3-5 times, mixing the methanol extractive solutions, and recovering methanol under reduced pressure to dryness; dissolving the residue with water, transferring to separating funnel, extracting with water saturated n-butanol for 5-8 times, mixing the n-butanol extractive solutions, washing with n-butanol saturated ammonia solution for 2-3 times, discarding the washing solution, and evaporating the n-butanol extractive solution to dryness to obtain third intermediate semen Ziziphi Spinosae powder;
s4, weighing the second intermediate spina date seed powder prepared in the step S2 and the third intermediate spina date seed powder prepared in the step S3, respectively grinding and sieving the two powder for later use, and uniformly mixing the powder according to a proper proportion to prepare the spina date seed powder.
Preferably, in S1, the drying specifically includes: baking in an oven at 65-75 deg.C for 15-30 h.
Preferably, in S1, the sieving is performed by using a 40-60 mesh sieve.
Preferably, in S1, the reflux extraction temperature is 75-90 deg.C, and the time is 12-14 h.
Preferably, in S2, the volume percentage of ethanol is 85-90%.
Preferably, in S2, the reflux temperature is 80-95 ℃ and the time is 7-8 h.
Preferably, in S2, the pre-freezing time is 48-50 h.
Preferably, in S3, the reflux time of the chloroform is 6-10 h; the methanol reflux time is 4-7 h.
Preferably, in S4, the sieving is performed by using a 40-65 mesh sieve.
The invention provides a wild jujube kernel powder prepared according to the method, which comprises the following components in percentage by weight: 5-15% of the second intermediate spina date seed powder and 85-95% of the third intermediate spina date seed powder.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the preparation method of the wild jujube kernel powder refines the traditional wild jujube kernel extraction, removes the components in the wild jujube kernel which are not related to sedation and hypnosis, retains the components which are the main effective components with the sedation and hypnosis functions, and overcomes the adverse pharmacological effects of various components in the natural wild jujube kernel extract. In addition, the spina date seed extract is powdery, and has the characteristics of rapid dispersion and high bioavailability; meanwhile, due to the uniform dispersion, adverse reaction caused by overhigh local concentration due to the instantaneous local release of the tablet in the body is avoided; meanwhile, the defects of poor stability, inconvenient storage and transportation and the like of liquid preparation medicines are avoided. The wild jujube kernel powder disclosed by the invention is convenient to take, fast to disperse, easy to absorb, high in bioavailability and stable in quality, can be swallowed, sucked or dispersed with water, is particularly suitable for the old and people with dysphagia, and is beneficial to popularization and application of the wild jujube kernel powder.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
Example 1
The embodiment provides a preparation method of wild jujube kernel powder, which comprises the following steps:
s1, drying the spina date seeds in a 65 ℃ oven for 15h, crushing the spina date seeds into particles by using a crusher, sieving the particles by using a 40-mesh sieve, adding the particles into petroleum ether at 70 ℃ to prepare a petroleum ether soaking solution, gently placing the petroleum ether soaking solution into a Soxhlet extractor for reflux extraction at the temperature of 75 ℃ for 12h until the petroleum ether soaking solution is colorless, removing an extracting solution, and naturally drying the rest substances to obtain spina date seed powder for later use;
s2, mixing the spina date seed powder obtained after natural air drying in the step S1 with 85% ethanol in volume percentage to obtain a mixed solution, then placing the mixed solution in a water bath kettle for refluxing at the refluxing temperature of 80 ℃ for 7 hours, carrying out centrifugal filtration, and naturally air drying the obtained solid matter to obtain first intermediate spina date seed powder; collecting filtrate, rotary evaporating to remove liquid, pre-freezing the rest materials in refrigerator for 48 hr, and freeze drying to obtain second intermediate semen Ziziphi Spinosae powder;
s3, putting the first intermediate spina date seed powder prepared in the step S2 into a Soxhlet extractor, and refluxing with chloroform for 6 hours; volatilizing chloroform from the residue, placing in a round-bottom flask, reflux-extracting with methanol for 3 times (4 hr), mixing the methanol extractive solutions, and recovering methanol under reduced pressure to dryness; dissolving the residue with water, transferring to separating funnel, extracting with water saturated n-butanol for 5 times, mixing the n-butanol extractive solutions, washing with n-butanol saturated ammonia solution for 2 times, discarding the washing solution, and evaporating the n-butanol extractive solution to dryness to obtain third intermediate semen Ziziphi Spinosae powder;
s4, weighing the second intermediate spina date seed powder prepared in the step S2 and the third intermediate spina date seed powder prepared in the step S3, respectively grinding the second intermediate spina date seed powder and the third intermediate spina date seed powder into fine powder, sieving the fine powder with a 40-mesh sieve for later use, and uniformly mixing the fine powder and the third intermediate spina date seed powder according to a proper proportion to prepare the spina date seed powder, wherein the spina date seed powder comprises the following components in percentage by: 5% of second intermediate spina date seed powder and 95% of third intermediate spina date seed powder.
Example 2
The embodiment provides a preparation method of wild jujube kernel powder, which comprises the following steps:
s1, drying the spina date seeds in an oven at 70 ℃ for 25h, crushing the spina date seeds into particles by using a crusher, sieving the particles with a 50-mesh sieve, adding the particles into petroleum ether at 75 ℃ to prepare a petroleum ether soaking solution, gently placing the petroleum ether soaking solution into a Soxhlet extractor for reflux extraction at 78 ℃ for 13h until the petroleum ether soaking solution is colorless, removing an extracting solution, and naturally drying the rest substances to obtain spina date seed powder for later use;
s2, mixing the spina date seed powder obtained after natural air drying in the step S1 with 87 volume percent of ethanol to obtain a mixed solution, then placing the mixed solution in a water bath kettle for refluxing at 90 ℃ for 7 hours, carrying out centrifugal filtration, and naturally air drying the obtained solid matter to obtain first intermediate spina date seed powder; collecting filtrate, rotary evaporating to remove liquid, pre-freezing the rest materials in refrigerator for 49 hr, and freeze drying to obtain second intermediate semen Ziziphi Spinosae powder;
s3, putting the first intermediate spina date seed powder prepared in the step S2 into a Soxhlet extractor, and refluxing with chloroform for 8 hours; volatilizing chloroform from the residue, placing in a round-bottom flask, reflux-extracting with methanol for 4 times (6 hr), mixing the methanol extractive solutions, and recovering methanol under reduced pressure to dryness; dissolving the residue with water, transferring to separating funnel, extracting with water saturated n-butanol for 7 times, mixing the n-butanol extractive solutions, washing with n-butanol saturated ammonia solution for 2 times, discarding the washing solution, and evaporating the n-butanol extractive solution to dryness to obtain third intermediate semen Ziziphi Spinosae powder;
s4, weighing the second intermediate spina date seed powder prepared in the step S2 and the third intermediate spina date seed powder prepared in the step S3, respectively grinding the second intermediate spina date seed powder and the third intermediate spina date seed powder into fine powder, sieving the fine powder with a 50-mesh sieve for later use, and uniformly mixing the fine powder and the third intermediate spina date seed powder according to a proper proportion to prepare the spina date seed powder, wherein the spina date seed powder comprises the following components in percentage by: 10% of second intermediate spina date seed powder and 90% of third intermediate spina date seed powder.
Example 3
The embodiment provides a preparation method of wild jujube kernel powder, which comprises the following steps:
s1, drying the spina date seeds in an oven at 75 ℃ for 30h, crushing the spina date seeds into particles by using a crusher, sieving the particles by using a 60-mesh sieve, adding the particles into petroleum ether at 80 ℃ to prepare a petroleum ether soaking solution, gently placing the petroleum ether soaking solution into a Soxhlet extractor for reflux extraction at the temperature of 90 ℃ for 14h until the petroleum ether soaking solution is colorless, removing an extracting solution, and naturally drying the rest substances to obtain spina date seed powder for later use;
s2, mixing the spina date seed powder obtained after natural air drying in the step S1 with 90% ethanol in volume percentage to obtain a mixed solution, then placing the mixed solution in a water bath kettle for refluxing at the refluxing temperature of 95 ℃ for 8 hours, carrying out centrifugal filtration, and naturally air drying the obtained solid matter to obtain first intermediate spina date seed powder; collecting filtrate, rotary evaporating to remove liquid, pre-freezing the rest materials in refrigerator for 50 hr, and freeze drying to obtain second intermediate semen Ziziphi Spinosae powder;
s3, putting the first intermediate spina date seed powder prepared in the step S2 into a Soxhlet extractor, and refluxing with chloroform for 10 hours; volatilizing chloroform from the residue, placing in a round-bottom flask, reflux-extracting with methanol for 5 times (7 hr), mixing the methanol extractive solutions, and recovering methanol under reduced pressure to dryness; dissolving the residue with water, transferring to a separating funnel, extracting with water saturated n-butanol for 8 times, mixing the n-butanol extractive solutions, washing with n-butanol saturated ammonia solution for 3 times, discarding the washing solution, and evaporating the n-butanol extractive solution to dryness to obtain third intermediate semen Ziziphi Spinosae powder;
s4, weighing the second intermediate spina date seed powder prepared in the step S2 and the third intermediate spina date seed powder prepared in the step S3, respectively grinding the second intermediate spina date seed powder and the third intermediate spina date seed powder into fine powder, sieving the fine powder with a 65-mesh sieve for later use, and uniformly mixing the fine powder and the third intermediate spina date seed powder according to a proper proportion to prepare the spina date seed powder, wherein the spina date seed powder comprises the following components in percentage by: 15% of second intermediate spina date seed powder and 85% of third intermediate spina date seed powder.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of wild jujube kernel powder is characterized by comprising the following steps:
s1, drying the spina date seeds, crushing the spina date seeds into particles by using a crusher, sieving, adding the particles into petroleum ether at 70-80 ℃ to prepare a petroleum ether soaking solution, gently placing the petroleum ether soaking solution into a Soxhlet extractor for reflux extraction until the petroleum ether soaking solution is colorless, removing an extracting solution, and naturally drying the rest substances to obtain spina date seed powder for later use;
s2, mixing the wild jujube seed powder obtained after natural air drying in the step S1 with ethanol to obtain a mixed solution, then placing the mixed solution in a water bath kettle for refluxing, carrying out centrifugal filtration, and naturally air drying the obtained solid matter to obtain first middle wild jujube seed powder; collecting filtrate, rotary evaporating to remove liquid, pre-freezing the rest materials in refrigerator, and freeze drying to obtain second intermediate semen Ziziphi Spinosae powder;
s3, putting the first intermediate spina date seed powder prepared in the step S2 into a Soxhlet extractor, and refluxing with chloroform; volatilizing chloroform from the residue, placing in a round-bottom flask, reflux-extracting with methanol for 3-5 times, mixing the methanol extractive solutions, and recovering methanol under reduced pressure to dryness; dissolving the residue with water, transferring to separating funnel, extracting with water saturated n-butanol for 5-8 times, mixing the n-butanol extractive solutions, washing with n-butanol saturated ammonia solution for 2-3 times, discarding the washing solution, and evaporating the n-butanol extractive solution to dryness to obtain third intermediate semen Ziziphi Spinosae powder;
s4, weighing the second intermediate spina date seed powder prepared in the step S2 and the third intermediate spina date seed powder prepared in the step S3, respectively grinding and sieving the two powder for later use, and uniformly mixing the powder according to a proper proportion to prepare the spina date seed powder.
2. The method of claim 1, wherein in step S1, the drying process comprises: baking in an oven at 65-75 deg.C for 15-30 h.
3. The method of claim 1, wherein the sieving in S1 is performed with a 40-60 mesh sieve.
4. The method of claim 1, wherein the reflux extraction temperature of S1 is 75-90 ℃ for 12-14 hours.
5. The method of claim 1, wherein the ethanol is 85-90% by volume of S2.
6. The method of claim 1, wherein the reflux temperature is 80-95 ℃ for 7-8 hours at S2.
7. The method of preparing the wild jujube kernel powder of claim 1, wherein the prefreezing time is 48-50 hours in S2.
8. The method of preparing the wild jujube kernel powder of claim 1, wherein in S3, the chloroform refluxing time is 6-10 h; the methanol reflux time is 4-7 h.
9. The method of claim 1, wherein the sieving in S4 is performed with a 40-65 mesh sieve.
10. A spine date seed powder prepared according to the method of any of claims 1-9, comprising the following components in weight percent: 5-15% of the second intermediate spina date seed powder and 85-95% of the third intermediate spina date seed powder.
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| CN105770052A (en) * | 2016-04-14 | 2016-07-20 | 天津商业大学 | Preparation method of semen ziziphi spinosae dispersible tablets and semen ziziphi spinosae dispersible tablets |
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| CN105770052A (en) * | 2016-04-14 | 2016-07-20 | 天津商业大学 | Preparation method of semen ziziphi spinosae dispersible tablets and semen ziziphi spinosae dispersible tablets |
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Application publication date: 20210406 |