阅读说明：本技术 一种桂花提取物的提取工艺 (Extraction process of sweet osmanthus extract ) 是由 周海军 于 2019-11-14 设计创作，主要内容包括：本发明公开了一种桂花提取物的提取工艺,涉及植物提取技术领域,解决了因桂花提取物仅通过水或低浓度乙醇提取获得,而导致其抑菌活性大大降低的问题,步骤如下：步骤一,粉碎干燥：将新鲜的桂花真空干燥,粉碎后过筛,得到桂花粉末；步骤二,萃取超声：将桂花粉末浸没在氯仿和乙醇溶液的混合溶液中回流萃取,得到萃取液,再向萃取液中加入乙醇溶液,进行超声处理,离心后取上层清液,得到提取液；步骤三,过滤浓缩：对提取液进行过滤,将过滤去渣后的滤液水浴浓缩,纯化后得到浓缩液；步骤四,灭菌干燥：将浓缩液进行超高压灭菌,再经过冷冻干燥和筛分后,即可得到桂花提取物。本发明提取得到的桂花提取物具有良好的抑菌活性,整体应用性好。(The invention discloses an extraction process of an osmanthus extract, relates to the technical field of plant extraction, and solves the problem that the bacteriostatic activity of the osmanthus extract is greatly reduced because the osmanthus extract is only obtained by water or low-concentration ethanol extraction, and the extraction process comprises the following steps: step one, crushing and drying: vacuum drying fresh sweet osmanthus, crushing and sieving to obtain sweet osmanthus powder; step two, extraction ultrasound: immersing sweet osmanthus powder in a mixed solution of chloroform and an ethanol solution for reflux extraction to obtain an extract, adding the ethanol solution into the extract, performing ultrasonic treatment, centrifuging, and taking supernatant to obtain an extract; step three, filtering and concentrating: filtering the extractive solution, concentrating the filtrate after filtering to remove residues in water bath, and purifying to obtain concentrated solution; step four, sterilizing and drying: and carrying out ultrahigh pressure sterilization on the concentrated solution, and carrying out freeze drying and screening to obtain the osmanthus fragrans extract. The osmanthus fragrans extract extracted by the method has good bacteriostatic activity and good overall applicability.)

1. The extraction process of the sweet osmanthus extract is characterized by comprising the following steps of:

step one, crushing and drying: vacuum drying fresh sweet osmanthus, crushing and sieving to obtain sweet osmanthus powder;

step two, extraction ultrasound: immersing sweet osmanthus powder in a mixed solution of chloroform and an ethanol solution for reflux extraction to obtain an extract, adding the ethanol solution into the extract, performing ultrasonic treatment, centrifuging, and taking supernatant to obtain an extract;

step three, filtering and concentrating: filtering the extracting solution obtained in the step two, concentrating the filtrate after filtering and removing residues in water bath, and purifying to obtain a concentrated solution;

step four, sterilizing and drying: and carrying out ultrahigh pressure sterilization on the concentrated solution, and carrying out freeze drying and screening to obtain the osmanthus fragrans extract.

2. The extraction process of the osmanthus fragrans extract according to claim 1, wherein in the second step, the volume mixing ratio of chloroform to ethanol is 1: (3-5).

3. The extraction process of the osmanthus fragrans extract according to claim 1, wherein in the second step, the ethanol solution is 70-90% by volume.

4. The extraction process of the osmanthus fragrans extract according to claim 1, wherein the third step is specifically configured to be filtration and concentration: and D, filtering the extracting solution obtained in the step two, concentrating the filtered filtrate in water bath, and purifying by using macroporous adsorption resin to obtain a concentrated solution.

5. The extraction process of osmanthus fragrans extract according to claim 4, wherein in the third step, the adsorption flow rate of the macroporous adsorption resin is 3-5BV/h, the eluent is 60-70% ethanol solution, and the elution flow rate is 1.8-2.4 BV/h.

6. The extraction process of the osmanthus fragrans extract according to claim 1, wherein the first step is specifically configured to be crushing and drying: vacuum drying fresh flos Osmanthi Fragrantis, pulverizing, and sieving with 40-80 mesh sieve to obtain flos Osmanthi Fragrantis powder.

7. The extraction process of the osmanthus fragrans extract according to claim 1, wherein the second step is specifically set as extraction ultrasound: immersing the sweet osmanthus powder in a mixed solution of chloroform and an ethanol solution for reflux extraction for 3-5 times, wherein the extraction time is 20-30min each time, the extraction temperature is 30-50 ℃, obtaining an extraction liquid, adding 3-5 times of the ethanol solution into the extraction liquid, performing ultrasonic treatment for 20-30min at the temperature of 70-90 ℃, repeatedly treating for 3-5 times, centrifuging for 5-10min, and taking supernatant after centrifugation to obtain an extraction liquid.

8. The extraction process of Osmanthus fragrans extract according to claim 7, wherein in the second step, the power of ultrasonic treatment is 200-300W, the frequency is 30-50kHz, and the rotational speed of centrifugation is 2000-3000 rpm.

9. The extraction process of the osmanthus fragrans extract according to claim 1, wherein the third step is specifically configured to be filtration and concentration: and D, filtering the extracting solution in the step two, and concentrating the filtrate after filtering and deslagging in water bath at the temperature of 60-80 ℃ to 0.4-0.5mg/mL to obtain a concentrated solution.

Technical Field

The invention relates to the technical field of plant extraction, in particular to an extraction process of an osmanthus fragrans extract.

Background

The sweet osmanthus has refreshing fragrance, is helpful for eliminating fatigue and enabling people to feel like repeated release, has the function of purifying air, and can inhibit the growth and reproduction of escherichia coli, candida albicans and staphylococcus aureus.

The Chinese invention patent application with the publication number of CN105832603A discloses a preparation method of an osmanthus fragrans extract, which comprises the following steps: 1) selecting dry sweet osmanthus as a raw material, and crushing; 2) adding a solvent which is 5-20 times of the raw material obtained in the step 1), stirring and extracting the sweet osmanthus extracting solution for 30-180 minutes at 25-95 ℃, and filtering; 3) centrifuging and purifying the sweet osmanthus extracting solution obtained in the step 2), and collecting filtrate; 4) concentrating the filtrate until the specific gravity of the extract is 1.10-1.30 to obtain sweet osmanthus extract; 5) and drying the osmanthus fragrans extract to obtain the osmanthus fragrans extract.

In the above application documents, only water or low-concentration ethanol is used as an extraction solvent, and no antioxidant is required to be added, so that the osmanthus fragrans extract can be safely used in the fields of food, medicine, health care products, nursing products and cosmetics.

Disclosure of Invention

Aiming at the problem that the bacteriostatic activity of the osmanthus fragrans extract is greatly reduced because the osmanthus fragrans extract is only obtained by water or low-concentration ethanol extraction in the prior art, the invention aims to provide an extraction process of the osmanthus fragrans extract, so as to solve the technical problems, and the osmanthus fragrans extract has good bacteriostatic activity and good overall applicability.

In order to achieve the first purpose, the invention provides the following technical scheme:

an extraction process of an osmanthus extract comprises the following steps:

step one, crushing and drying: vacuum drying fresh sweet osmanthus, crushing and sieving to obtain sweet osmanthus powder;

step two, extraction ultrasound: immersing sweet osmanthus powder in a mixed solution of chloroform and an ethanol solution for reflux extraction to obtain an extract, adding the ethanol solution into the extract, performing ultrasonic treatment, centrifuging, and taking supernatant to obtain an extract;

step three, filtering and concentrating: filtering the extracting solution obtained in the step two, concentrating the filtrate after filtering and removing residues in water bath, and purifying to obtain a concentrated solution;

step four, sterilizing and drying: and carrying out ultrahigh pressure sterilization on the concentrated solution, and carrying out freeze drying and screening to obtain the osmanthus fragrans extract.

By adopting the technical scheme, the chloroform and the ethanol solution have good compatibility, a good and stable mixed solution can be formed, more interferents such as stearic acid, oleic acid and the like in the osmanthus can be dissolved by the ethanol, the capacity of the chloroform for dissolving the substances is not strong, impurities in the extract can be greatly reduced, the purification in the later period is facilitated, and the osmanthus extract has good antibacterial activity. Meanwhile, in the extraction process, the mixed solution of chloroform and ethanol solution is used for extraction for multiple times, and then the ethanol solution is used for independent ultrasonic treatment, so that the integral activity of the antibacterial active ingredients is ensured, and the harmful chloroform can be volatilized. After filtering and concentrating, freeze-drying is carried out in the sterilization and drying process, so that the osmanthus fragrans extract can keep good antibacterial activity and has good overall applicability.

More preferably, in the second step, the volume mixing ratio of chloroform to ethanol is 1: (3-5).

More preferably, in the second step, the ethanol solution with a volume fraction of 70-90% is selected.

By adopting the technical scheme, the ethanol solution with the volume parts and the chloroform and the ethanol with the volume mixing ratio are selected, so that the bacteriostatic activity of the bacteriostatic active ingredients in the osmanthus fragrans can be kept, the precipitation rate of the bacteriostatic active ingredients can be ensured, and the obtained osmanthus fragrans extract has good quality.

More preferably, the third step is specifically configured to perform filtration and concentration: and D, filtering the extracting solution obtained in the step two, concentrating the filtered filtrate in water bath, and purifying by using macroporous adsorption resin to obtain a concentrated solution.

By adopting the technical scheme, the macroporous adsorption resin has a good macroporous net structure and a larger specific surface area, has stable physicochemical property, is insoluble in acid, alkali and organic solvent, is not influenced by inorganic salts and strong ion low molecular compounds, can play a good purification effect on the extracting solution after water bath concentration, is beneficial to obtaining a relatively pure concentrated solution, and enables bacteriostatic active ingredients in the concentrated solution to keep good bacteriostatic activity.

More preferably, in the third step, the adsorption flow rate of the macroporous adsorption resin is 3-5BV/h, the eluent is 60-70% ethanol solution, and the elution flow rate is 1.8-2.4 BV/h.

By adopting the technical scheme, the parameters are selected for control to operate, so that a good elution effect can be achieved, and the osmanthus fragrans extract is guaranteed to have good quality.

More preferably, the first step is specifically configured to perform crushing and drying: vacuum drying fresh flos Osmanthi Fragrantis, pulverizing, and sieving with 40-80 mesh sieve to obtain flos Osmanthi Fragrantis powder.

Further preferably, the second step is specifically configured to extract ultrasound: immersing the sweet osmanthus powder in a mixed solution of chloroform and an ethanol solution for reflux extraction for 3-5 times, wherein the extraction time is 20-30min each time, the extraction temperature is 30-50 ℃, obtaining an extraction liquid, adding 3-5 times of the ethanol solution into the extraction liquid, performing ultrasonic treatment for 20-30min at the temperature of 70-90 ℃, repeatedly treating for 3-5 times, centrifuging for 5-10min, and taking supernatant after centrifugation to obtain an extraction liquid.

By adopting the technical scheme, in the extraction process, the extraction temperature is controlled to be 30-50 ℃, the bacteriostatic active ingredients in the osmanthus fragrans can be stably separated out and are not easy to be damaged, the impurities in the extract can be greatly reduced, after the extract liquor is combined, an ethanol solution is added for repeated ultrasonic treatment for many times, the temperature is controlled to be 70-90 ℃, the chloroform in the extract liquor can be separated out as far as possible, the bacteriostatic activity of the osmanthus fragrans extract is ensured and improved to a certain extent, and the integral applicability is good.

More preferably, in the second step, the power of the ultrasonic treatment is 200-300W, the frequency is 30-50kHz, and the rotation speed of the centrifugation is 2000-3000 rpm.

More preferably, the third step is specifically configured to perform filtration and concentration: and D, filtering the extracting solution in the step two, and concentrating the filtrate after filtering and deslagging in water bath at the temperature of 60-80 ℃ to 0.4-0.5mg/mL to obtain a concentrated solution.

By adopting the technical scheme and the parameter control, the high efficiency and stability in the whole extraction process can be kept, the antibacterial activity of the antibacterial active ingredients is not easily damaged, and the obtained osmanthus fragrans extract has high quality.

In summary, compared with the prior art, the invention has the following beneficial effects:

(1) the chloroform and the ethanol solution are mixed and then the sweet osmanthus is extracted, so that the impurities in the extract can be greatly reduced, the purification at the later stage is facilitated, the sweet osmanthus extract can have good antibacterial activity, and then the ethanol solution is used for carrying out single ultrasonic treatment, so that the chloroform which is a harmful component can be volatilized, the sweet osmanthus extract can keep good antibacterial activity, and the integral applicability is good;

(2) the macroporous adsorption resin has good purification effect on the extracting solution after water bath concentration, is beneficial to obtaining relatively pure concentrated solution, and enables the bacteriostatic active ingredients in the concentrated solution to keep good bacteriostatic activity.

Drawings

FIG. 1 is a process flow diagram of the present invention.

Detailed Description

The invention is described in detail below with reference to the figures and examples.