CN101658290B - Method for extracting crabapple polyphenols from crabapple skin dregs - Google Patents

Abstract

The invention relates to a method for extracting and preparing sago polyphenols from sago peel residue, which comprises the following steps: soaking dried and crushed sago peel residue with ethanol solution, ultrasonic extraction, column chromatography separation and purification, rotary evaporation concentration and vacuum drying and other procedures, the polyphenols were extracted from the sand fruit peel residue soaked in ethanol solution in an ultrasonic extraction equipment, and the ultrasonic power was 250W; the separation and purification adopted the AB-8 macroporous resin column chromatography method. The obtained sargo polyphenol is a powdery product, and its polyphenol content is 65% to 80%. The raw material used to extract polyphenols in this method is sand fruit peel residue, which not only makes use of the waste, but also reduces environmental pollution. This method also has the advantages of time saving, energy saving, high polyphenol extraction rate, and no solvent. The advantages of residues have greatly improved the added value and comprehensive utilization efficiency of agricultural and sideline products. The method solves the problems of long extraction time and low purity in conventional methods, and is easy for industrialized production.

Description

A kind of method extracting sand fruit polyphenols from sand fruit pomace

1. Technical field

The invention relates to the development and utilization of sand fruit peel residue, in particular to a method for extracting and preparing sand fruit polyphenols by using sand fruit peel residue as a raw material in the production process of sand fruit concentrated juice.

2. Background technology

Shaguo pomace is a by-product in the processing of Shaguo juice, which is rich in polyphenols. At present, a large amount of pomace in the processing of shaguo concentrated juice is discarded as garbage, which not only wastes resources but also pollutes the environment. Sargolin, as a class of biologically active natural compounds, plays a pivotal role in human health. Many studies have shown that polyphenols have a variety of health functions, such as preventing dental caries, preventing high blood pressure, anti-tumor, anti-mutation, antibacterial, scavenging free radicals, anti-oxidation and anti-aging, etc., especially its anti-oxidation ability is vitamin C. 50 times, 20 times of vitamin E. Polyphenols also have the functions of deodorization, preservation, fragrance preservation, color protection, and prevention of vitamin loss, which can prevent the deterioration of food quality. There are many studies on plant polyphenols at home and abroad, and the patents mainly focus on the preparation and application of tea polyphenols, apple polyphenols and grape seed polyphenols. However, there are no patents and related product research reports on the polyphenols of the fruit pomace residue. Sand fruit pods are rich in polyphenols. Utilizing the property that the sand fruit polyphenols are easily soluble in ethanol, ultrasonic extraction and column chromatography purification are used to extract the sand fruit polyphenols from the sand fruit pods, which has a high extraction rate and avoids the The loss of active ingredients and the advantages of no solvent residue solve the problems of long extraction time and low purity in conventional methods, and are easy for industrial production.

3. Contents of the invention

Invention content:

The purpose of the present invention is to provide a method for extracting and preparing sago polyphenols from sago peel residue.

Above-mentioned purpose realizes by following technical scheme:

The preparation method of sand fruit polyphenols comprises: taking sand fruit peel residue, drying in the sun or drying at 50-55°C, after the drying process, crushing into 80-100 mesh, sending sand fruit peel residue into ultrasonic extraction In the machine, under 250W, extract sago polyphenols, the extraction solvent is 50% to 75% ethanol, the extraction time is 20 to 30min, the extraction temperature is 50 to 55°C, the ratio of solid to liquid is 1:5 to 1:10, and the extraction time is 1 to 30 minutes. 2 times. Collect the leach liquid and concentrate it initially. AB-8 macroporous resin column chromatography is used for separation and purification, and the obtained eluate is then concentrated by rotary evaporation and vacuum-dried to obtain the sago polyphenol powder, the sago polyphenol content of which is 65% to 80%.

The preparation method of the described sago polyphenols, the AB-8 macroporous resin column chromatography method adopts wet packing (1.0×40cm), the height of the column bed is 30cm, and sago polyphenols are added at a flow rate of 1mL/min The leachate of phenol, after adsorption saturation, washes with 2BV (column bed volume) distilled water, to remove impurities such as sugar and water-soluble hemicellulose adsorbed by the resin. Then, it was eluted with 60% ethanol solution until it was colorless, and the elution flow rate was 0.5 mL/min. The eluate was collected, and the ethanol was recovered by a rotary evaporator.

In the preparation method of the sargo polyphenol, the concentration parameters are: vacuum degree 0.075-0.09MPa, evaporation temperature 50-55°C.

In the preparation method of the sargo polyphenol, the vacuum drying parameters are: vacuum degree 0.09MPa, temperature 50-55°C.

This technical solution has the following beneficial effects:

1. The present invention adopts ultrasonic extraction. Compared with conventional solvent extraction, the ultrasonic extraction method has the advantages of short extraction time, high yield, and mild conditions, which is beneficial to industrial production.

2. The whole process of extracting, purifying and concentrating polyphenols in sand fruit pomace is carried out at low temperature without damaging the chemical structure of polyphenols.

3. The technology of the present invention can obtain higher purity sargo polyphenols products. In the process of separation and purification, the macroporous resin AB-8 is used to separate and purify the crude extract of sargassum polyphenols, which has the characteristics of good selectivity, fast adsorption speed, easy analysis, simple regeneration treatment, and high product purity. The present invention also includes optimal separation condition parameters: adsorption and elution at normal temperature, adding the leaching solution of sargo polyphenols at a flow rate of 1mL/min, and washing with 2BV (column bed volume) distilled water after adsorption saturation. Then it was eluted with 60% ethanol at a flow rate of 0.5 mL/min. After hundreds of exploration experiments and improvements, the specific process parameters adopted in the present invention greatly improve the purity of the sargo polyphenols.

4. The technical cost of the present invention is relatively low, all solvents used can be recovered, and the product has no solvent residue, which provides an operational route for the industrialized production of sago polyphenols.

5. The raw material used for the extraction of polyphenols in the present invention is the pomace residue, which can only be used as feed or fertilizer usually, and its higher added value has not been brought into play. The invention provides a new way for the utilization of sand fruit peel residue, not only makes full use of the waste, but also reduces environmental pollution and brings greater economic benefits to related processing enterprises.

4. Specific implementation

Example 1: Preparing sago polyphenols with sago peel residue as raw material.

Get 80 mesh dry sand fruit peel residues, in an ultrasonic extractor, extract sand fruit polyphenols under 250W ultrasonic power, the extraction solvent is 50% ethanol, the extraction time is 30min, the extraction temperature is 50°C, the ratio of solid to liquid is 1:5, and the extraction time is 2 Second-rate. Collect the leach liquid and concentrate it initially.

Separation and purification adopt the AB-8 macroporous resin column chromatography method, adopt wet packing (1.0 × 40cm), column bed height 30cm, add the leaching solution of sargo polyphenols at a flow rate of 1mL/min, after adsorption saturation, use 2

BV (column bed volume) was washed with distilled water to remove impurities such as sugar and water-soluble hemicellulose adsorbed by the resin. Then, it was eluted with 60% ethanol solution until it was colorless, and the elution flow rate was 0.5 mL/min, and the eluate was collected.

The obtained eluate is concentrated by rotary evaporation at a vacuum degree of 0.09MPa and an evaporation temperature of 50°C, and then vacuum-dried at a vacuum degree of 0.09MPa and a temperature of 50°C to obtain sargopolyphenol powder, which has a sagopolyphenol content of 65%. .

Example 2: Preparing sago polyphenols with sago peel residue as raw material.

Get 100 mesh dry sand fruit peel residues, in an ultrasonic extractor, extract sand fruit polyphenols under 250W ultrasonic power, the extraction solvent is 60% ethanol, the extraction time is 25min, the extraction temperature is 55°C, the ratio of solid to liquid is 1:8, and the extraction time is 25 minutes. Second-rate. Collect the leach liquid and concentrate it initially.

Separation and purification are the same as in Example 1.

The obtained eluate is concentrated by rotary evaporation at a vacuum degree of 0.09MPa and an evaporation temperature of 55°C, and then vacuum-dried at a vacuum degree of 0.09MPa and a temperature of 55°C to obtain sargopolyphenol powder, which has a sagopolyphenol content of 72%. .

Example 3: Preparing sago polyphenols with sago peel residue as raw material.

Take 80 mesh dry sand fruit peel residues, in an ultrasonic extractor, extract sand fruit polyphenols under 250W ultrasonic power, the extraction solvent is 75% ethanol, the extraction time is 30min, the extraction temperature is 50°C, the ratio of solid to liquid is 1:10, and the extraction time is 1 Second-rate. Collect the leach liquid and concentrate it initially.

Separation and purification are the same as in Example 1.

The obtained eluate is concentrated by rotary evaporation at a vacuum degree of 0.075MPa and an evaporation temperature of 55°C, and then vacuum-dried at a vacuum degree of 0.09MPa and a temperature of 50°C to obtain sago polyphenol powder, which has a sago polyphenol content of 80%. .

Claims (3)

1. A preparation method of sargo polyphenols, comprising: sargo peel residue, dried in the sun or dried at 50-55°C, characterized in that: after the drying process, it is pulverized into 80-100 meshes, and the Put the sand fruit peel residue into the ultrasonic extractor, extract the sand fruit polyphenols at 250W, the extraction solvent is 50%-75% ethanol, the extraction time is 20-30min, the temperature is 50-55°C, and the solid-liquid ratio is 1:5-1 : 10, extract 1 to 2 times; collect the leached liquid, and preliminarily concentrate; separation and purification adopts the AB-8 macroporous resin column chromatography method, and the obtained eluate is then concentrated by rotary evaporation and vacuum-dried to obtain sargopolyphenols Powder, its polyphenol content is 65%～80%; The described AB-8 macroporous resin column chromatography method adopts wet packing, the column is 1.0×40cm, the column bed height is 30cm, and sand is added at a flow rate of 1mL/min. The leachate of fruit polyphenols, after saturated adsorption, is washed with distilled water with a column bed volume of 2BV to remove the sugar and water-soluble hemicellulose impurities adsorbed by the resin; then eluted with 60% ethanol solution until it is colorless, and The flow rate was 0.5mL/min, and the eluate was collected and concentrated by a rotary evaporator to recover ethanol. 2. The preparation method of sago polyphenols according to claim 1, characterized in that: the concentration parameters are: vacuum degree 0.075-0.09MPa, evaporation temperature 50-55°C. 3. The preparation method of sago polyphenol according to claim 1, characterized in that: the vacuum drying parameters are: vacuum degree 0.09MPa, temperature 50-55°C.