CN103142662A - Method for extracting and purifying polyphenol from choerospondias axillaris peel - Google Patents

Abstract

The invention provides a method for extracting and purifying polyphenols from jujube peel, using ethanol to reflux to extract polyphenols from jujube peel, and extracting the polyphenol crude extract from jujube peel obtained after recovering ethanol from the extract with n-hexane, removing the extract The non-polar substances in the sample were removed by rotary evaporation to remove n-hexane, centrifuged, and the supernatant was purified by HP2MGL macroporous adsorption resin. The eluate was concentrated and freeze-dried to obtain the refined product of polyphenols from Jujube bark. The invention has the advantages of simple process, low cost, easy industrial production, less environmental pollution, high polyphenol content in the extracted and purified jujube bark, which reduces the loss of active ingredients, turns waste into treasure, and greatly increases The added value and comprehensive utilization rate of agricultural products.

Description

A method for extracting and purifying polyphenols from the bark of southern jujube

technical field

The invention belongs to a method for extracting polyphenols, in particular to a method for extracting and purifying polyphenols with jujube bark dregs.

Background technique

Suanzao is the mature fruit of Choerospondias axillaris (Roxb. ) Burttet Hill, a plant belonging to the family Anacardiaceae, also known as five-eyed fruit, mountain jujube, mountain vinegar and human face. It is mainly distributed in Hubei, Guangdong, Guangxi, Jiangxi, Fujian and other places. Southern jujube is also distributed in some countries and regions such as India and Indochina Peninsula. Mongolian medicine believes that South Suanzao has the functions of promoting qi and blood circulation, nourishing the heart and calming the nerves, and is used to treat qi stagnation and blood stasis, chest pain, palpitations, shortness of breath, and restlessness. Modern pharmacological studies have proved that Suanzao has a variety of physiological activities, especially on the cardiovascular system. In addition to its special medicinal value, southern jujube has a long-standing eating custom in Hunan, mainly used for appetizing and digestion, sobering up and so on.

Studies have found that jujube is rich in organic acids, flavonoids, sterols, lipids, sugars, amino acids and inorganic elements. The total flavonoids in jujube are considered to be its active ingredients and have various pharmacological activities. The peel of wild jujube contains a variety of organic acids mainly including citric acid, malic acid, tartaric acid and grape acid, and the content is relatively high. Nuts and seeds are rich in nutrients such as protein, amino acid, fat, vitamins and various mineral elements, as well as biologically active substances such as tannins and saponins. Among them, the polyphenols are the chemical substance basis for the strong antioxidant activity of jujube. In addition to the strong antioxidant activity of jujube polyphenols, studies have also shown that its pharmacological activity has a strong effect on the cardiovascular system, such as anti-arrhythmia Abnormal effect, protection of myocardial ischemia, anti-platelet aggregation, enhancement of immune function, and removal of free radicals in the body. At the same time, the polyphenol extract of Suanzi jujube also has anti-tumor activity. The fresh fruit of Southern jujube is sour and astringent. Because of its poor taste when eaten raw, the pulp is generally processed into jujube cakes, fruit juice drinks and other products before eating, and the by-product of processing—the peel, is directly consumed because it cannot be effectively used. It is discarded, which not only causes a waste of resources, but also pollutes the environment. Therefore, research and development of wild jujube resources, new extraction and purification process of polyphenols from wild jujube skin, comprehensive utilization of wild jujube resources, increase the income of local farmers, and the prevention of cardiovascular and cerebrovascular diseases and cancers in China, which is about to enter an aging society, In terms of maintaining the health of the body, it is of great practical significance to develop new health care medicines of traditional Chinese medicine and to find new natural antioxidants and other related products.

Contents of the invention

The technical problem to be solved by the present invention is to provide a method for extracting and purifying polyphenols from jujube bark, which is simple in operation, low in cost, easy for industrial production, safe and green, high in polyphenol extraction rate, good in purification effect, and less in environmental pollution.

The present invention solves the above-mentioned technical problems through the following technical solutions: a method for extracting and purifying polyphenols from the bark of South Suanzi jujuba, the specific steps of the process are as follows:

(1) Pretreatment: take fresh jujube bark, dry it in an oven at 50°C, crush it, and pass it through a 60-mesh sieve to get the bark bark powder.

(2) Extraction: The ethanol reflux extraction method is used to extract the powder of the jujube bark obtained in step (1), specifically, 50%~60% ethanol in an amount 30~35 times the weight of the dry bark powder is used as Extracting agent, reflux extraction 3 times, the extraction temperature is 40-80 degrees Celsius, and the reflux time is 1h each time. After the extraction is completed, the extract is combined, and the ethanol in the extract is recovered by rotary evaporation, and then extracted with n-hexane to remove non- For polar substances, remove a small amount of n-hexane by rotary evaporation again, centrifuge, and take the supernatant to obtain the concentrated solution of polyphenols from jujube bark.

(3) Purification: Use HP2MGL macroporous adsorption resin to purify the concentrated solution obtained in step (2). Specifically, take the polyphenol concentrated solution of jujube bark and dilute it with an appropriate amount of 50% ethanol aqueous solution to make the concentration of the sample solution The total polyphenol content is between 3~4mg/mL, and the sample is loaded on a macroporous adsorption resin column (2.6×30cm resin height 26cm) at a sample rate of 1~1.5mL/min, and it is allowed to stand for 0.5h after sample loading. Complete adsorption; wash with distilled water until the effluent is clear, then elute with 55% ethanol aqueous solution at an elution rate of 1mL/min, collect the eluate, concentrate and recover ethanol, and obtain a brown-yellow powder after freeze-drying the concentrated solution Refined product of polyphenols from jujube bark.

According to the present invention, a method for extracting and purifying polyphenols from jujube peel has the following advantages: the preparation process is simple, the alcohol extraction is green and safe, the prepared polyphenols have a high content of active ingredients, reflux extraction and ethanol elution have little environmental pollution, And the price is low, recyclable, and easy to industrialized production; the HP2MGL type macroporous adsorption resin has high purification efficiency, and can be recycled, which can further reduce the production cost; The total polyphenol content of refined phenolic products can reach 76%, turning the waste of jujube bark into treasure without wasting resources of jujube bark.

Description of drawings

Figure 1 is a process diagram of the present invention.

Detailed ways

Embodiment one

Pretreatment: drying the fresh jujube bark in an oven at 50°C, pulverizing it with a pulverizer and passing it through a 60-mesh sieve to obtain the bark bark powder.

Extraction: Weigh 1 kg of the above-mentioned southern jujube peel powder, and use the ethanol reflux extraction method to extract it, specifically: add 35 L of 55% ethanol aqueous solution, reflux extraction 3 times, the extraction temperature is 60 degrees Celsius, 1 hour each time, and combine after the extraction is completed extract solution, recover the ethanol in the extract solution by rotary evaporation, then use n-hexane extraction to remove non-polar substances in the extract solution, continue rotary evaporation to remove residual n-hexane, centrifuge, and take the supernatant, which is the southern jujube bark Phenol concentrate.

Purification: adopt HP2MGL type macroporous adsorption resin to purify the concentrated solution of the southern jujube bark obtained above, specifically: the concentrated solution obtained above is dissolved with an appropriate amount of 50% ethanol aqueous solution, so that the total polyphenol content of the sample solution is Between 3~4mg/mL, the sample is loaded on the macroporous adsorption resin column (2.6×30cm resin height 26cm) at the adsorption rate of 1mL/min: after the adsorption is completed, let it stand for 0.5h, and then wash with distilled water until the effluent is free After turbidity, elute with 55% ethanol aqueous solution at the elution rate of 1mL/min, collect the eluate, concentrate, freeze-dry, and obtain the refined polyphenols of jujube bark as a brown yellow powder. It is known that the purity of polyphenols in Jujube bark in this example is 78.66% by using the Folin phenol method

Embodiment two

Pretreatment: drying the fresh jujube bark in an oven at 50°C, pulverizing it with a pulverizer and passing it through a 60-mesh sieve to obtain the bark bark powder.

Extraction: Weigh 1 kg of the above-mentioned southern jujube peel powder, and use the ethanol reflux extraction method to extract it, specifically: add 60% ethanol aqueous solution 30L, reflux extraction 3 times, the extraction temperature is 40 degrees Celsius, 1 hour each time, and combine after the extraction is completed The extract solution is recovered by rotary evaporation to recover the ethanol in the extract solution, and then extracted with n-hexane to remove the non-polar substances in the extract solution. After continuing the rotary evaporation to remove the residual n-hexane, centrifuge and take the supernatant, which is the southern jujube bark. Phenol concentrate.

Purification: adopt HP2MGL type macroporous adsorption resin to purify the concentrated solution of polyphenols from jujube bark obtained above, specifically: dissolve the concentrated solution obtained above with an appropriate amount of 50% aqueous ethanol to make the total polyphenols in the sample solution The content is between 3~4mg/mL, and the sample is loaded on the macroporous adsorption resin column (2.6×30cm resin height 26cm) at the adsorption rate of 1.5mL/min: after the adsorption is completed, let it stand for 0.5h, and then wash it with distilled water until After the effluent was free from turbidity, it was eluted with 55% ethanol aqueous solution at an elution rate of 1 mL/min, the eluate was collected, concentrated, and freeze-dried to obtain a brownish yellow powder of refined polyphenols from jujube bark. The purity of the polyphenols in the bark of Jujube jujuba in this example is 76.23% according to the Folin phenol method.

In summary, the preparation process of the present invention is simple, the extraction and purification efficiency is high, and the use of ethanol reflux extraction method and ethanol elution not only has little environmental pollution, but also is cheap, recyclable, and easy to industrialized production; and the HP2MGL macroporous adsorption resin column can be regenerated Utilization can further reduce the cost; in addition, the method has good stability and reproducibility, and the total polyphenol content of the polyphenol refined product of the jujube bark can reach 76%, turning the bark of the jujube into treasure without causing the The waste of wild jujube resources provides a certain scientific basis for the industrial production of polyphenols from the bark of wild jujube and the development of related functional health products.

Claims (3)

1. a method for extracting and purifying polyphenols in South Suanziza husk, is characterized in that: Pretreatment: take fresh South Suanzao skin, dry it in an oven at 50°C, crush it, and pass it through a 60-mesh sieve to obtain South Suanzao skin powder; Extraction: Extract the powder of the jujube bark obtained in step (1) by using the ethanol reflux extraction method, specifically, use 50%~60% ethanol as the extractant in an amount 30~35 times the weight of the dried bark powder, Reflux extraction 3 times, the extraction temperature is 40-80 degrees Celsius, each reflux time is 1h, after the extraction is completed, the extracts are combined, the ethanol in the extract is recovered by rotary evaporation, and then extracted with n-hexane to remove the non-polar substances in the extract , after removing a small amount of n-hexane by rotary evaporation again, centrifuge, and take the supernatant to obtain the concentrated solution of polyphenols from jujube bark; Purification: Use HP2MGL macroporous adsorption resin to purify the concentrated solution obtained in step (2). Specifically, take the concentrated solution of polyphenols from jujube bark and dilute it with an appropriate amount of 50% ethanol aqueous solution to make the total polyphenols in the sample solution The content is between 3~4mg/mL, and the sampling rate is 1~1.5mL/min. The sample is loaded on the macroporous adsorption resin column (2.6×30cm resin height 26cm). Wash with distilled water until the effluent is clarified, then elute with 55% ethanol aqueous solution at an elution rate of 1mL/min, collect the eluate, concentrate and reclaim ethanol, and obtain the Nanzizao bark of brown yellow powder after freeze-drying the concentrated solution Refined polyphenols. 2. the method for extracting and purifying polyphenols in a kind of southern jujube peel according to claim 1, is characterized in that: described extraction method is heat reflux extraction, and extraction solvent is ethanol, and extraction frequency is 3 times, and extraction solvent consumption is raw material 30 to 35 times the weight; the temperature is 40 to 80 degrees Celsius, and the extraction time is 1 hour; after extraction, ethanol recovery treatment is required, the temperature is controlled below 50 degrees Celsius, and the vacuum degree is controlled above 0.06Mpa. 3. according to claim 1, the method for extracting and purifying polyphenols in a kind of southern jujube skin is characterized in that: the purification method is a macroporous adsorption resin method; resin used is HP2MGL type, and its purification steps are: A The extract is concentrated, ethanol is recovered, extracted, and centrifuged to obtain a concentrated solution of jujube bark. After dissolving with 50% ethanol aqueous solution, the total polyphenol content of the sample solution is between 3 and 4 mg/mL; the sample rate is 1～1.5mL/min is loaded on the macroporous adsorption resin column (2.6×30cm resin height 26cm); the so-called concentration is vacuum concentration, the concentration temperature is controlled below 50 degrees Celsius, and the centrifugal speed is 5000r/ min; B After loading the sample, let it stand for 0.5h to complete the adsorption; then wash with distilled water until the effluent is clear; C was eluted with 55% ethanol aqueous solution at an elution rate of 1mL/min, and the collected eluent was 2 to 4 times the amount of resin; D Concentrate the obtained ethanol eluent, control the concentration temperature below 50 degrees Celsius, and vacuum degree at 0.06-0.1Mpa, freeze-dry the concentrated solution to obtain the refined product of brown yellow jujube bark polyphenols, the total polyphenols measured by Folin’s phenol method The phenol content is as high as 76%.

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