CN116784476A - Composition containing concentrated powder of Aronia melanocarpa fruit, apple, acerola cherry and mulberry, and preparation and application thereof - Google Patents

Abstract

The invention relates to a composition containing concentrated powder of rowan fruit, apple, acerola cherry and mulberry as well as its preparation and application. The preparation process of the composition of black rowanberry fruit, apple, acerola cherry and mulberry concentrated powder includes: preparation of anthocyanins in black rowan fruit; preparation of polyphenols in apple; acerola cherry Preparation of vitamin C; preparation of anthocyanins in mulberries, etc. The present invention creatively uses the concentrated powder of black fruit, apple, acerola cherry and mulberry to prepare a composition product with antioxidant, beauty and whitening, anti-inflammatory and anti-acne properties. During the preparation process, solvent extraction is creatively used. Method, ultrafiltration membrane extraction method, and microwave-assisted extraction method respectively extract polyphenols, vitamin C, anthocyanins, etc., which have the advantages of simple process technology, high extraction efficiency, and high extract quality.

Description

A combination of concentrated powders of Aroma nigrum, apple, acerola and mulberry Materials and their preparation and application

Technical field

A composition containing concentrated powder of rowan fruit, apple, acerola cherry and mulberry as well as its preparation and application belongs to the field of food technology.

Background technique

Anthocyanins have the functions of protecting cardiovascular and cerebrovascular vessels, lowering cholesterol, antioxidant, moisturizing, beautifying and whitening, etc. They are widely found in fruits, vegetables, etc. Among them, black gland-ribbed rowan fruits and mulberries are rich in polyphenols, among which anthocyanins have the highest content. Vitamin C is an essential nutrient element for the human body. It has a variety of physiological functions. It can enhance the body's resistance, prevent infections and cardiovascular system diseases, improve the utilization of iron, calcium and folic acid, and has anti-scorch and antioxidant effects. Effectively enhance human body resistance. Acerola cherries are rich in various vitamins, among which vitamin C content is relatively high, so they are also widely used in the manufacture of vitamin C products. Apples are sweet in taste, cool in nature, rich in fiber and polyphenols, and have very good effects on beautifying the skin, improving skin elasticity, and reducing wrinkles.

Anthocyanins, polyphenols, vitamin C, etc. all have beautifying, anti-oxidant, anti-inflammatory and anti-acne effects. The raw materials for their production are black rowan fruit, mulberry, apple, acerola, etc., which are widely used in beauty and other fields. raw materials. With the progress of the times, people's demand for beauty and beauty is increasing, and the invention of related concentrated health powder has attracted more and more attention from scholars. Therefore, the invented manufacturing process is simple and the composition concentrated powder process with good use effect is of great significance to the progress and development of the times.

Contents of the invention

In order to overcome the above-mentioned technical problems existing in the prior art field, the object of the present invention is to provide a preparation process flow of a composition containing concentrated powder of black fruit, apple, acerola cherry and mulberry.

A composition containing black rowanberry, apple, acerola and mulberry concentrated powder. The composition contains black rowanberry concentrated powder, apple concentrated powder and acerola concentrated powder. Powder and mulberry concentrated powder, the mass content of anthocyanins in the concentrated powder of Sorbus berries is 1% to 4%, and the mass content of polyphenols in the concentrated apple powder is 30% to 50%, The mass content of vitamin C in the concentrated acerola powder is 15-20%, and the mass content of anthocyanins in the concentrated mulberry powder is 1%-4%.

The invention provides a preparation process flow of a composition containing concentrated powder of black rowan fruit, apple, acerola cherry and mulberry, which includes the following steps:

Step (1) Preparation of anthocyanins from Sorbus nigra fruit

The fresh fruits of Sorbus nigra and the pomace after juice extraction are freeze-dried and then crushed to obtain the whole fruit and pomace powder for later use. Accurately weigh some rowan tree whole fruits and pomace powder, use different concentrations of ethanol and acetic acidified water as auxiliary catalysts, use ultrasonic-assisted extraction, centrifuge, concentrate, and freeze-dry to obtain the anthocyanins extracted from the rowan tree whole fruits and pomace. things. The concentrated anthocyanin extract is added to a column pre-packed with column chromatography packing for separation and purification. Each separated purified product is then collected and concentrated to remove residual solvent to obtain anthocyanins;

Step (2) Preparation of polyphenols in apples

Crush immature apples with a crusher into apple pomace for later use. Accurately weigh some apple pomace and put it into an Erlenmeyer flask. Add a certain amount of hydrochloric acid and a mixed solvent of ethanol and acetone, and stir and dissolve on a magnetic stirrer. a period of time. Then, after filtration, separation and purification, a glycol acidic solution rich in polyphenols is obtained. Evaporate the ethanol by heating in a magnetic stirring water bath, concentrate and freeze-dry to obtain apple polyphenols;

Step (3) Preparation of Vitamin C from Acerola Cherry

Take fresh acerola fruit and fruit pomace after juice extraction, freeze-dry and crush for later use. Accurately weigh the acerola pomace powder, add catalyst trifluoroacetic acid and ethanol, stir continuously to dissolve, and dissolve the acerola fruit. The mixture of slag is put into the membrane cavity of the ultrafiltration equipment for ultrafiltration to obtain a concentrated slurry rich in vitamin C. The low pressure and high temperature conditions of the rotary evaporator are then used to concentrate it, remove the water, and then freeze-dry to obtain a vitamin C-rich slurry. of Acerola Concentrate Powder;

Step (4) Preparation of anthocyanins in mulberries

Wash the fresh mulberries with distilled water and dry them. Put a certain amount of mulberries into a clean mortar and grind for a certain period of time until the mulberry pulp and peel are ground and evenly distributed. Pay attention to the exposure during grinding. Accurately weigh a certain amount of uniformly ground mulberry powder into an Erlenmeyer flask, add a certain mass fraction of ethanol solution and catalyst methyl tert-butyl ether, and use a microwave-assisted extraction instrument to extract for a certain period of time. Filter the extract, then put it into a rotary evaporator to concentrate, remove the water, and obtain concentrated mulberry powder containing rich anthocyanins;

Step (5) Synthesis of composition powder

Put the mixed powder of black fruit rowanberry concentrated powder, apple polyphenol concentrated powder, acerola cherry concentrated powder, and mulberry concentrated powder into the extraction tank. After extraction, add a certain pectinase solution, soak at room temperature, and filter Obtain the retentate liquid, add a certain amount of maltodextrin to the retentate liquid, and then concentrate and mix. The concentrated and mixed material is sent to the drying equipment by a high-pressure pump for drying, and is screened to obtain a concentrated powder composition.

Preferably, step (1) Preparation of anthocyanins in Sorbus nigra fruit includes taking fresh fruits of Sorbus nigra and the fruit pomace after juice extraction, freeze-drying and crushing, and passing through a 40 to 60 mesh sieve. Obtain whole fruit and pomace powder for later use. Accurately weigh 2~4g of rowan tree whole fruit and pomace powder, add 2~5mL of acetic acidified water as an auxiliary catalyst, and then use an ethanol solvent with a volume fraction of 60%~80%, ultrasonic-assisted extraction, centrifugation, concentration, and freezing. After drying, the anthocyanin extract derived from the whole rowan fruit and pomace was obtained. The concentrated anthocyanin extract is added to a column pre-packed with column chromatography packing for separation and purification. Then each separated purified product is collected and concentrated to remove the residual solvent to obtain black glandular rib rowan fruit powder containing 1% to 4% anthocyanins.

In the preparation of this method, black gland-ribbed rowan fruit is used as one of the raw material sources of anthocyanins because rowan fruits are generally dark purple and rich in polyphenols, among which the content of anthocyanins is the highest. . Anthocyanins have cardiovascular and cerebrovascular protection, cholesterol lowering, antioxidant, moisturizing and other effects, and have a protective effect on skin beautification and whitening. During the preparation process, a mixed solvent of polar ethanol with good compatibility similar to anthocyanins and auxiliary catalyst acetic acid acidified water is selected as the main extraction agent, which can avoid the decomposition of anthocyanins and the introduction of other impurities while keeping the extraction environment acidic. Improve the extraction efficiency; with the assistance of ultrasound, the anthocyanins in the rowan pomace can fully come into contact with the mixed solvent of ethanol and acetic acid acidified water and can be separated and purified. The purified mixture is further purified and concentrated through column chromatography. The operation method is simple and quickly improves the production efficiency of the product.

Preferably, the preparation of polyphenols in apples in step (2) includes crushing immature apples with a crusher into apple pomace for later use, passing them through a 40-60 mesh sieve, and accurately weighing 5-8g of apple pomace into a cone. In the bottle, add 1~3mL, 0.1~0.2mol/L hydrochloric acid and 10~15mL mixed solvent of ethanol and acetone with a volume fraction of 60%~80%, and place it on a magnetic stirrer to stir and dissolve for 30~60 minutes. Then, after filtration, separation and purification, a glycol acidic solution rich in polyphenols is obtained. The ethanol is evaporated by heating in a magnetic stirring water bath, concentrated and freeze-dried to obtain apple powder containing 30%-50% polyphenols.

In this method, a simple and efficient organic solvent extraction method is used to extract polyphenols in apples and prepare apple powder rich in polyphenols. Because the hydroxyl groups contained in the polyphenol structure of apples have a certain polarity, according to the principle of similar compatibility, the polyphenols in apples have very good compatibility with ethanol and acetone, and can be effectively extracted from the pulp tissue of apples. . A certain amount of hydrochloric acid is added during the extraction process to prevent the oxidation reaction between polyphenols and oxygen in the air during the extraction process, resulting in impure purified products.

Preferably, the preparation of vitamin C in acerola cherries in step (3) includes taking fresh acerola fruits and pomace after juice extraction, freeze-drying and crushing for later use, passing through a 40-60 mesh sieve, and weighing 6-10 g accurately. Acerola pomace powder, add 2~3mL catalyst trifluoroacetic acid and 15~20mL ethanol with a volume fraction of 60~80%, stir for 30~60min to completely dissolve, then cold soak in the dark for 3~5h, cold soak The final mixture of acerola pomace is put into the membrane cavity of the ultrafiltration equipment for ultrafiltration to obtain a concentrated slurry rich in vitamin C. The low pressure and high temperature conditions of the rotary evaporator are then used to concentrate it and remove the water. Acerola concentrated powder containing 17% to 19% vitamin C was obtained by freeze-drying. Ultrafiltration equipment parameters: diameter: 90~100, membrane area: 16.8~ ^17.2m2 , molecular weight cutoff: 10000~100000 daltons, membrane fiber diameter: outer diameter 0.5~0.8mm, inner diameter 0.2~0.4mm.

This method creatively uses advanced ultrafiltration membrane technology to separate and purify vitamin C in cherries. The ultrafiltration membrane extraction method has the advantages of high recovery rate, short production cycle, low energy consumption, and no secondary pollution, which can greatly improve the efficiency of the extraction process. During the ultrafiltration process, macromolecules such as protein and fat in the pulp can be effectively screened out to ensure the quality of the final product and improve the anti-inflammatory, acne-removing and whitening effect of the final composition. This method uses the catalyst trifluoroacetic acid in the ultrafiltration process, which can create an acidic environment for ultrafiltration to avoid product oxidation and introduce new impurities, and can also speed up the efficiency of ultrafiltration; and the raw materials are shading and cold soaked before the ultrafiltration membrane is extracted. The purpose of processing is to fully mix the pulp cells in the raw material with the solvent, which is more conducive to the subsequent ultrafiltration purification effect.

Preferably, the preparation of anthocyanins in mulberries in step (4) includes washing fresh mulberries with distilled water, drying them, putting the mulberries into a clean mortar, and grinding them for 2 to 3 hours until the mulberry pulp and peel are ground and crushed. Be even and pay attention to exposure during grinding. Accurately weigh 5~8g of uniformly ground mulberry powder into an Erlenmeyer flask, add 10~15mL of 60%~80% ethanol solution and 1~3mL of catalyst methyl tert-butyl ether, and use a microwave-assisted extraction instrument to extract 30~ 60 minutes. Filter the extract and put it into a rotary evaporator to concentrate, remove the water, and obtain concentrated mulberry powder containing 1% to 4% anthocyanins.

This method uses a microwave-assisted extraction method when extracting anthocyanins from mulberries. The purpose is to use microwaves to penetrate the extraction medium and reach the microtubule bundles and gland cell systems inside the mulberries. Since the cells absorb microwave energy, the temperature inside the cells will rapidly increase. rises, causing the pressure inside the cell to exceed the ability of the cell wall to expand; as a result, the cell ruptures, and the active ingredients inside flow out freely and are dissolved and extracted in the extraction medium at a lower temperature. The method has the advantages of short operating time and low solvent consumption. When grinding mulberry raw materials, care must be taken to avoid strong exposure to prevent the anthocyanins in the cells from being oxidized and deteriorated by strong exposure during the grinding process, leading to the introduction of unnecessary impurities.

Preferably, the synthesis of the powder of the composition in step (5) includes taking 20 to 40 g of black glandular rib rowan fruit concentrated powder, apple polyphenol concentrated powder, acerola concentrated powder, and mulberry concentrated powder that have been passed through a 30 to 50 mesh sieve. Put the mixed powder into the extraction tank, the extraction pressure is 20~30MPa, the extraction temperature is 50~70℃, the extraction time is 2~3h; then add 5~10mL pectinase solution, soak at room temperature for 30~60 minutes, filter to obtain the interception liquid, add 5 to 8 g of maltodextrin to the retentate, and then concentrate and mix. The concentrated and mixed material is sent to a drying equipment by a high-pressure pump for drying, and is sieved to obtain a concentrated powder composition.

This method uses maltodextrin in the process of preparing the concentrate combination powder. This method uses dextrin to have a chain-like molecular structure in which sugars are connected, so that the components can be better combined together and have a chain-like structure. , the physical properties of the concentrated composition are more stable and more conducive to subsequent storage.

Adopting the present invention, the composition using concentrated powder of rowan fruit, apple, acerola cherry and mulberry has the characteristics of antioxidant, moisturizing, anti-inflammatory and anti-acne, and also helps to promote human body metabolism, anti-inflammation and beauty treatment. Whitening and other effects.

Description of the drawings

Figure 1 is a flow chart of the preparation process of a composition containing concentrated powder of black fruit rowan fruit, apple, acerola cherry and mulberry.

Detailed ways

Example 1

The invention provides a preparation process flow of a composition containing concentrated powder of black rowan fruit, apple, acerola cherry and mulberry, which includes the following steps:

Step (1) Preparation of anthocyanins from Sorbus nigra fruit

Take the fresh fruits of Sorbus nigra and the pomace after juicing the fruits, freeze-dry them, crush them, pass them through a 40-mesh sieve, and obtain the whole fruit and pomace powder for later use. Accurately weigh 2g of rowan tree whole fruit and pomace powder, add 2 mL of acetic acid acidified water as an auxiliary catalyst, use an ethanol solvent with a volume fraction of 60%, use ultrasonic-assisted extraction, centrifuge, concentrate, and freeze-dry to obtain the rowan tree whole fruit and pomace powder. Pomace derived anthocyanin extract. The concentrated anthocyanin extract is added to a column pre-packed with column chromatography packing for separation and purification. Then each separated purified product is collected and concentrated to remove the residual solvent to obtain black glandular rib rowan fruit powder containing 1% anthocyanins;

Step (2) Preparation of polyphenols in apples

Crush immature apples with a crusher into apple pomace for later use. Pass through a 40-mesh sieve. Accurately weigh 5g of apple pomace and put it into an Erlenmeyer flask. Add 1mL, 0.1mol/L hydrochloric acid and 10mL with a volume fraction of 60%. Mix solvent of ethanol and acetone and stir on a magnetic stirrer for 30 minutes to dissolve. Then, after filtration, separation and purification, a glycol acidic solution rich in polyphenols is obtained. Evaporate the ethanol by heating in a magnetic stirring water bath, concentrate and freeze-dry to obtain apple powder containing 30% polyphenols;

Step (3) Preparation of Vitamin C from Acerola Cherry

Take fresh acerola fruit and fruit pomace after juice extraction, freeze-dry and crush for later use, pass through a 40-mesh sieve, accurately weigh 6g of acerola pomace powder, add 2mL of catalyst trifluoroacetic acid and 15mL of volume fraction to 60% of ethanol, stir for 30 minutes to completely dissolve, and then cold-soak in the dark for 3 hours. Put the cold-soaked acerola pomace mixture into the membrane cavity of the ultrafiltration equipment for ultrafiltration to obtain a concentrated slurry rich in vitamin C. , then use the low pressure and high temperature conditions of the rotary evaporator to concentrate, remove the water, and then freeze-dry to obtain acerola concentrated powder containing 17% vitamin C. Ultrafiltration equipment parameters: diameter: 90, membrane area: 16.8m ² , molecular weight cutoff: 10000~100000 daltons, membrane wire diameter: outer diameter 0.5mm, inner diameter 0.2mm;

Step (4) Preparation of anthocyanins in mulberries

Wash the fresh mulberries with distilled water and dry them. Put the mulberries into a clean mortar and grind them for 2 hours until the mulberry pulp and peel are ground, crushed and even. Pay attention to the exposure during grinding. Accurately weigh 5g of uniformly ground mulberry powder into an Erlenmeyer flask, add 10 mL of 60% ethanol solution and 1 mL of catalyst methyl tert-butyl ether, and use a microwave-assisted extraction instrument to extract for 30 minutes. Filter the extract, then put it into a rotary evaporator to concentrate, remove the water, and obtain concentrated mulberry powder containing 1% anthocyanins;

Step (5) Synthesis of composition powder

Take 20g of the mixed powder of black fruit rowanberry concentrated powder, apple polyphenol concentrated powder, acerola cherry concentrated powder, and mulberry concentrated powder that has passed through a 30 mesh sieve and put it into the extraction tank. The extraction pressure is 20MPa and the extraction temperature is 50°C. , extraction time 2h; then add 5mL pectinase solution, soak at room temperature for 30 minutes, filter to obtain the retentate, add 5g maltodextrin to the retentate, and then concentrate and mix. The concentrated and mixed material will be pumped by a high-pressure pump It is sent to drying equipment for drying and sieved to obtain a concentrated powder composition.

Example 2

Step (1) Preparation of anthocyanins from Sorbus nigra fruit

Take the fresh fruits of Sorbus nigra and the pomace after juicing the fruits, freeze-dry them, crush them, pass them through a 45-mesh sieve, and obtain the whole fruit and pomace powder for later use. Accurately weigh 3g of rowan tree whole fruit and pomace powder, add 3 mL of acetic acid acidified water as an auxiliary catalyst, use an ethanol solvent with a volume fraction of 65%, use ultrasonic-assisted extraction, centrifuge, concentrate, and freeze-dry to obtain the rowan tree whole fruit and pomace powder. Pomace derived anthocyanin extract. The concentrated anthocyanin extract is added to a column pre-packed with column chromatography packing for separation and purification. Then each separated purified product is collected and concentrated to remove the residual solvent to obtain black glandular rib rowan fruit powder containing 2% anthocyanins;

Step (2) Preparation of polyphenols in apples

Crush the immature apples with a crusher into apple pomace for later use. Pass through a 45-mesh sieve. Accurately weigh 6g of apple pomace and put it into an Erlenmeyer flask. Add 2mL, 0.15mol/L hydrochloric acid and 12mL with a volume fraction of 65%. Mix the solvent of ethanol and acetone, and stir and dissolve on a magnetic stirrer for 40 minutes. Then, after filtration, separation and purification, a glycol acidic solution rich in polyphenols is obtained. Evaporate the ethanol by heating in a magnetic stirring water bath, concentrate and freeze-dry to obtain apple powder containing 35% polyphenols;

Step (3) Preparation of Vitamin C from Acerola Cherry

Take fresh acerola fruit and fruit pomace after juice extraction, freeze-dry and crush for later use. Pass through a 45-mesh sieve. Accurately weigh 7g of acerola pomace powder, add 2.3mL of catalyst trifluoroacetic acid and 16mL of volume fraction 65 % ethanol, stir for 40 minutes to completely dissolve, and then cold-soak in the dark for 3.5 hours. Put the cold-soaked acerola pomace mixture into the membrane cavity of the ultrafiltration equipment for ultrafiltration to obtain vitamin C-rich Concentrate the slurry, and then use the low pressure and high temperature conditions of the rotary evaporator to concentrate, remove the water, and then freeze-dry to obtain acerola concentrated powder containing 17.5% vitamin C. Ultrafiltration equipment parameters: diameter: 90, membrane area: 17.0m ² , molecular weight cutoff: 10000~100000 daltons, membrane wire diameter: outer diameter 0.6mm, inner diameter 0.3mm;

Step (4) Preparation of anthocyanins in mulberries

Wash the fresh mulberries with distilled water and dry them. Put the mulberries into a clean mortar and grind them for 2.2 hours until the mulberry pulp and peel are ground, crushed and even. Pay attention to the exposure during grinding. Accurately weigh 6g of uniformly ground mulberry powder into an Erlenmeyer flask, add 11 mL of 65% ethanol solution and 1.5 mL of catalyst methyl tert-butyl ether, and use a microwave-assisted extraction instrument to extract for 40 minutes. Filter the extract, then put it into a rotary evaporator to concentrate, remove the water, and obtain concentrated mulberry powder containing 2% anthocyanins;

Step (5) Synthesis of composition powder

Take 25g of the mixed powder of black fruit rowanberry concentrated powder, apple polyphenol concentrated powder, acerola cherry concentrated powder, and mulberry concentrated powder that has passed through a 35-mesh sieve and put it into the extraction tank. The extraction pressure is 23MPa and the extraction temperature is 55°C. , the extraction time is 2.3h; then add 6mL of pectinase solution, soak at room temperature for 40 minutes, filter to obtain the retentate, add 6g of maltodextrin to the retentate, and then concentrate and mix. The concentrated and mixed material will be heated by high pressure The pump is sent to drying equipment for drying and sieving to obtain a concentrated powder composition.

Example 3

Step (1) Preparation of anthocyanins from Sorbus nigra fruit

Take the fresh fruits of Sorbus nigra and the pomace after juicing the fruits, freeze-dry them, crush them, pass them through a 50-mesh sieve, and obtain the whole fruit and pomace powder for later use. Accurately weigh 3g of the whole rowan fruit and pomace powder, add 4 mL of acetic acid acidified water as an auxiliary catalyst, use an ethanol solvent with a volume fraction of 70%, perform ultrasonic-assisted extraction, then centrifuge, concentrate, and freeze-dry to obtain the whole rowan fruit and pomace powder. Pomace derived anthocyanin extract. The concentrated anthocyanin extract is added to a column pre-packed with column chromatography packing for separation and purification. Then each separated purified product is collected and concentrated to remove the residual solvent to obtain black glandular rib rowan fruit powder containing 3% anthocyanins;

Step (2) Preparation of polyphenols in apples

Crush immature apples with a crusher into apple pomace for later use. Pass through a 50-mesh sieve. Accurately weigh 7g of apple pomace and put it into an Erlenmeyer flask. Add 2.5mL, 0.17mol/L hydrochloric acid and 13mL with a volume fraction of 70. % ethanol and acetone as a solvent, and stirred and dissolved on a magnetic stirrer for 50 minutes. Then, after filtration, separation and purification, a glycol acidic solution rich in polyphenols is obtained. After heating in a magnetic stirring water bath to evaporate the ethanol, concentrate and freeze-dry, apple powder containing 40% polyphenols is obtained;

Step (3) Preparation of Vitamin C from Acerola Cherry

Take fresh acerola fruit and fruit pomace after juice extraction, freeze-dry and crush for later use, pass through a 50-mesh sieve, accurately weigh 8g of acerola pomace powder, add 2.5mL of catalyst trifluoroacetic acid and 18mL with a volume fraction of 70 % ethanol, stir for 50 minutes to completely dissolve, and then cold soak in the dark for 4 hours. Put the cold-soaked acerola pomace mixture into the membrane cavity of the ultrafiltration equipment for ultrafiltration to obtain a concentrated vitamin C-rich product. The slurry is then concentrated using the low-pressure and high-temperature conditions of a rotary evaporator to remove moisture, and then freeze-dried to obtain acerola concentrated powder containing 18% vitamin C. Ultrafiltration equipment parameters: diameter: 95, membrane area: 17.0m ² , molecular weight cutoff: 10000~100000 daltons, membrane wire diameter: outer diameter 0.6mm, inner diameter 0.3mm;

Step (4) Preparation of anthocyanins in mulberries

Wash the fresh mulberries with distilled water and dry them. Put the mulberries into a clean mortar and grind them for 2.5 hours until the mulberry pulp and peel are ground, crushed and even. Pay attention to the exposure during grinding. Accurately weigh 7g of uniformly ground mulberry powder into an Erlenmeyer flask, add 12 mL of 70% ethanol solution and 2 mL of catalyst methyl tert-butyl ether, and use a microwave-assisted extraction instrument to extract for 50 minutes. Filter the extract, then put it into a rotary evaporator to concentrate, remove the water, and obtain concentrated mulberry powder containing 3% anthocyanins;

Step (5) Synthesis of composition powder

Take 30g of the mixed powder of black fruit glandular rib fruit concentrated powder, apple polyphenol concentrated powder, acerola cherry concentrated powder, and mulberry concentrated powder that has passed through a 40 mesh sieve and put it into the extraction tank. The extraction pressure is 25MPa and the extraction temperature is 60°C. , the extraction time is 2.5h; then add 8mL of pectinase solution, soak at room temperature for 50 minutes, filter to obtain the retentate, add 7g of maltodextrin to the retentate, and then concentrate and mix. The concentrated and mixed material will be processed by high pressure The pump is sent to drying equipment for drying and sieving to obtain a concentrated powder composition.

Example 4

Step (1) Preparation of anthocyanins from Sorbus nigra fruit

Take the fresh fruits of Sorbus nigra and the pomace after juicing the fruits, freeze-dry them, crush them, pass them through a 60-mesh sieve, and obtain the whole fruit and pomace powder for later use. Accurately weigh 4g of the whole rowan fruit and pomace powder, add 5 mL of acetic acidified water as an auxiliary catalyst, use an ethanol solvent with a volume fraction of 75%, perform ultrasonic-assisted extraction, then centrifuge, concentrate, and freeze-dry to obtain the whole rowan fruit and pomace powder. Pomace derived anthocyanin extract. The concentrated anthocyanin extract is added to a column pre-packed with column chromatography packing for separation and purification. Then each separated purified product is collected and concentrated to remove the residual solvent to obtain black glandular rib rowan fruit powder containing 4% anthocyanins;

Step (2) Preparation of polyphenols in apples

Crush immature apples with a crusher into apple pomace for later use. Pass through a 60-mesh sieve. Accurately weigh 8g of apple pomace and put it into an Erlenmeyer flask. Add 3mL, 0.2mol/L hydrochloric acid and 15mL with a volume fraction of 80%. Mix solvent of ethanol and acetone, and stir and dissolve on a magnetic stirrer for 60 minutes. Then, after filtration, separation and purification, a glycol acidic solution rich in polyphenols is obtained. Evaporate the ethanol by heating in a magnetic stirring water bath, concentrate and freeze-dry to obtain apple powder containing 50% polyphenols;

Step (3) Preparation of Vitamin C from Acerola Cherry

Take fresh acerola fruit and fruit pomace after juice extraction, freeze-dry and crush for later use, pass through a 60-mesh sieve, accurately weigh 9g acerola pomace powder, add 3mL catalyst trifluoroacetic acid and 20mL volume fraction to 80% of ethanol, stir for 60 minutes to completely dissolve, and then cold-soak in the dark for 4.5 hours. Put the cold-soaked acerola pomace mixture into the membrane cavity of the ultrafiltration equipment for ultrafiltration to obtain a concentrated vitamin C-rich product. The slurry is then concentrated using the low-pressure and high-temperature conditions of a rotary evaporator to remove moisture, and then freeze-dried to obtain acerola concentrated powder containing 19% vitamin C. Ultrafiltration equipment parameters: diameter: 100, membrane area: 17.2m ² , molecular weight cutoff: 10000~100000 Daltons, membrane wire diameter: outer diameter 0.8mm, inner diameter 0.4mm;

Step (4) Preparation of anthocyanins in mulberries

Wash the fresh mulberries with distilled water and dry them. Put the mulberries into a clean mortar and grind them for 3 hours until the mulberry pulp and peel are ground, crushed and even. Pay attention to the exposure during grinding. Accurately weigh 8g of uniformly ground mulberry powder into an Erlenmeyer flask, add 15 mL of 80% ethanol solution and 2.5 mL of catalyst methyl tert-butyl ether, and use a microwave-assisted extraction instrument to extract for 60 minutes. Filter the extract, then put it into a rotary evaporator to concentrate, remove the water, and obtain concentrated mulberry powder containing 5% anthocyanins;

Step (5) Synthesis of composition powder

Take 40g of the mixed powder of black fruit rowanberry concentrated powder, apple polyphenol concentrated powder, acerola cherry concentrated powder, and mulberry concentrated powder that has passed through a 50 mesh sieve and put it into the extraction tank. The extraction pressure is 30MPa and the extraction temperature is 70°C. , extraction time is 3h; then add 10mL pectinase solution, soak at room temperature for 60 minutes, filter to obtain the retentate, add 8g maltodextrin to the retentate, and then concentrate and mix. The concentrated and mixed material is pumped by a high-pressure pump It is sent to drying equipment for drying and sieved to obtain a concentrated powder composition.

Comparative example 1

Step (1) Preparation of anthocyanins from Sorbus nigra fruit

Take the fresh fruits of Sorbus nigra and the pomace after juicing the fruits, freeze-dry them, crush them, pass them through a 40-mesh sieve, and obtain the whole fruit and pomace powder for later use. Accurately weigh 5g of rowan tree whole fruit and pomace powder, use butanol solvent with a volume fraction of 60%, conduct ultrasonic-assisted extraction, centrifuge, concentrate, and freeze-dry to obtain anthocyanin extract from rowan tree whole fruit and pomace. The concentrated anthocyanin extract is added to a column pre-packed with column chromatography packing for separation and purification. Then each separated purified product is collected and concentrated to remove the residual solvent to obtain black glandular rib rowan fruit powder containing 1% anthocyanins;

Step (2) Preparation of polyphenols in apples

Crush immature apples with a crusher into apple pomace for later use. Pass through a 40-mesh sieve. Accurately weigh 5g of apple pomace and put it into an Erlenmeyer flask. Add 1mL, 0.1mol/L glacial acetic acid and 10mL with a volume fraction of 60 % butanol and stirred on a magnetic stirrer for 30 minutes. Then, after filtration, separation and purification, a glycol acidic solution rich in polyphenols is obtained. Evaporate the ethanol by heating in a magnetic stirring water bath, concentrate and freeze-dry to obtain apple powder containing 30% polyphenols;

Step (3) Preparation of Vitamin C from Acerola Cherry

Take fresh acerola fruit and fruit pomace after juice extraction, freeze-dry and crush for later use, pass through a 40-mesh sieve, accurately weigh 6g of acerola pomace powder, add 2mL of dilute acetate and 15mL of volume fraction to 60% of butanol, stir for 30 minutes to completely dissolve, and then cold-soak in the dark for 3 hours. Put the cold-soaked acerola pomace mixture into the membrane cavity of the ultrafiltration equipment for ultrafiltration to obtain a concentrated vitamin C-rich product. The slurry is then concentrated using the low-pressure and high-temperature conditions of a rotary evaporator to remove moisture, and then freeze-dried to obtain acerola concentrated powder containing 17% vitamin C. Ultrafiltration equipment parameters: diameter: 90, membrane area: 16.8m ² , molecular weight cutoff: 10000~100000 daltons, membrane wire diameter: outer diameter 0.5mm, inner diameter 0.2mm;

Step (4) Preparation of anthocyanins in mulberries

Wash the fresh mulberries with distilled water and dry them. Put the mulberries into a clean mortar and grind them for 2 hours until the mulberry pulp and peel are ground, crushed and even. Pay attention to the exposure during grinding. Accurately weigh 5g of uniformly ground mulberry powder into an Erlenmeyer flask, add 10 mL of 60% butanol solution, and use a microwave-assisted extraction instrument to extract for 30 minutes. Filter the extract, then put it into a rotary evaporator to concentrate, remove the water, and obtain concentrated mulberry powder containing 1% anthocyanins;

Step (5) Synthesis of composition powder

Take 20g of the mixed powder of black fruit rowanberry concentrated powder, apple polyphenol concentrated powder, acerola cherry concentrated powder, and mulberry concentrated powder that has passed through a 30 mesh sieve and put it into the extraction tank. The extraction pressure is 20MPa and the extraction temperature is 50°C. , the extraction time is 2h; then add 5mL of pectate enzyme solution, soak at room temperature for 30 minutes, filter to obtain the retentate, add 5g of white dextrin to the retentate, and then concentrate and mix. The concentrated and mixed material will be heated by high pressure The pump is sent to drying equipment for drying and sieving to obtain a concentrated powder composition.

Comparative example 2

Step (1) Preparation of anthocyanins from Sorbus nigra fruit

Take the fresh fruits of Sorbus nigra and the pomace after juicing the fruits, freeze-dry them, crush them, and pass them through a 55-mesh sieve to obtain the whole fruit and pomace powder for later use. Accurately weigh 8g of rowan tree whole fruit and pomace powder, use 80% butanol solvent with a volume fraction of 80%, conduct ultrasonic-assisted extraction, then centrifuge, concentrate, and freeze-dry to obtain anthocyanin extract from rowan tree whole fruit and pomace. The concentrated anthocyanin extract is added to a column pre-packed with column chromatography packing for separation and purification. Then each separated purified product is collected and concentrated to remove the residual solvent to obtain black glandular rib rowan fruit powder containing 4% anthocyanins;

Step (2) Preparation of polyphenols in apples

Crush immature apples with a crusher into apple pomace for later use. Pass through a 60-mesh sieve. Accurately weigh 8g of apple pomace and put it into an Erlenmeyer flask. Add 3mL, 0.2mol/L glacial acetic acid and 15mL with a volume fraction of 80. % butanol and stirred on a magnetic stirrer for 50 minutes. Then, after filtration, separation and purification, a glycol acidic solution rich in polyphenols is obtained. Evaporate the ethanol by heating in a magnetic stirring water bath, concentrate and freeze-dry to obtain apple powder containing 50% polyphenols;

Step (3) Preparation of Vitamin C from Acerola Cherry

Take fresh acerola fruit and fruit pomace after juice extraction, freeze-dry and crush for later use, pass through a 60-mesh sieve, accurately weigh 9g of acerola pomace powder, add 3mL of dilute acetate and 20mL of volume fraction to 80% of butanol, stir for 50 minutes to completely dissolve, and then cold-soak in the dark for 5 hours. Put the cold-soaked acerola pomace mixture into the membrane cavity of the ultrafiltration equipment for ultrafiltration to obtain a concentrated vitamin C-rich product. The slurry is then concentrated using the low-pressure and high-temperature conditions of a rotary evaporator to remove moisture, and then freeze-dried to obtain acerola concentrated powder containing 19% vitamin C. Ultrafiltration equipment parameters: diameter: 100, membrane area: 17.2m ² , molecular weight cutoff: 10000~100000 Daltons, membrane wire diameter: outer diameter 0.8mm, inner diameter 0.4mm;

Step (4) Preparation of anthocyanins in mulberries

Wash the fresh mulberries with distilled water and dry them. Put the mulberries into a clean mortar and grind them for 3 hours until the mulberry pulp and peel are ground, crushed and even. Pay attention to the exposure during grinding. Accurately weigh 8g of uniformly ground mulberry powder into an Erlenmeyer flask, add 15 mL of 80% butanol solution, and use a microwave-assisted extraction instrument to extract for 60 minutes. Filter the extract, then put it into a rotary evaporator to concentrate, remove the water, and obtain concentrated mulberry powder containing 4% anthocyanins;

Step (5) Synthesis of composition powder

Take 40g of the mixed powder of black fruit rowanberry concentrated powder, apple polyphenol concentrated powder, acerola cherry concentrated powder, and mulberry concentrated powder that has passed through a 50 mesh sieve and put it into the extraction tank. The extraction pressure is 25MPa and the extraction temperature is 60°C. , the extraction time is 3h; then add 8mL of pectate enzyme solution, soak at room temperature for 50 minutes, filter to obtain the retentate, add 8g of white dextrin to the retentate, and then concentrate and mix. The concentrated and mixed material will be processed by high pressure The pump is sent to drying equipment for drying and sieving to obtain a concentrated powder composition.

The concentrated powder compositions obtained in Examples 1 to 4 and Comparative Examples 1 and 2 were tested. The specific testing methods are as follows:

Density test

Use a BETA401Z density meter to measure the sample of the concentrated powder composition according to Archimedes' principle, and take the average value of multiple measurements.

Moisture content test

Use the SFY-20D powder moisture detector and the principle of weight loss on drying. Put different samples into the sample tray. After turning on the power, heat it to make the moisture in the sample evaporate in a short time. After the instrument test is completed, read the screen display. Number, take the average of multiple measurements.

Powder particle size test

Use the LT3600Plus laser particle size analyzer to disperse different sample powders in the sample cell of the instrument. After the instrument test is completed, read the display and take the average value of multiple measurements.

Skin moisture content and scale proportion test

Thirty people each from 31 to 40 years old were treated with the composition products of Examples 1-4 and Comparative Examples 1 and 2 for 30 days respectively, using CM-825 skin moisture test probe, TM-300 skin moisture loss test probe, and skin The desquamation tape and MPA 6 host (CK Company of Germany) were used to test the changes in skin moisture content and skin scale proportion of each group before and after 30 days, and the average values were recorded.

Table 1 Density test results

As can be seen from Table 1, Examples 1 to 4 all have higher densities than Comparative Examples 1 and 2. This is because the comparative example uses butanol as the main solvent of the extraction agent. Although butanol can also be used to extract and purify raw materials through similar miscibility principles, its polarity is weak and not as polar as ethanol. When cyanins, polyphenols and other substances are used, the extraction effect is not good, and an extraction auxiliary catalyst is added during the extraction process, which speeds up the extraction efficiency and quality, making the product prepared by using ethanol and auxiliary catalyst as the main solvent during extraction dense. Higher sex, higher density.

Table 2 Moisture content test results

It can be seen from the moisture content test results in Table 2 that Examples 1 to 4 all have lower moisture content than Comparative Examples 1 and 2, and meet the standard that the moisture content of food-grade composition powder is less than 9%. The lower the moisture content of the composition powder, the longer its quality, stability and storage life. From the test results, the moisture content of the final composition prepared using white dextrin is obviously higher than that of the composition prepared using maltodextrin in the embodiment. This is because maltodextrin has a chain-like molecular structure with sugars that can effectively link anthocyanins, polyphenols, vitamin C and other costs to form a network structure, which facilitates the evaporation of water during the preparation process and reduces the water content.

Table 3 Powder particle size test results

It can be seen from the powder particle size test results in Table 3 that Examples 1 to 4 all have smaller powder particle sizes than Comparative Examples 1 and 2. The larger the particle size of the powder, the greater the water absorption rate of the concentrated powder composition in actual use, resulting in poor absorption by the human body of anthocyanins, polyphenols, vitamin C and other substances in the powder of the composition. In the embodiments, maltodextrin is used that is better combined with each raw material component, so that the particle size of the powder of the prepared composition is uniform without agglomeration and other phenomena, and the average particle size of the powder is smaller.

Table 4 Test results of skin moisture content and scale proportion

It can be seen from the test results of skin moisture content and scale proportion in Table 4 that the increase in skin moisture content of the composition products prepared in Examples 1-4 corresponding to the test population is higher than the increase in skin moisture content of the test population corresponding to the comparative example. Example The composition product prepared in 1-4 has a higher reduction in the proportion of skin scaly in the test population than the comparison ratio corresponding to the reduction in the proportion of skin scaly in the test population. It shows that the Examples have better beauty, whitening and antioxidant effects than the Comparative Examples. This is because both the Examples and the Comparative Examples prepared compositions containing vitamin C, polyphenols, anthocyanins, etc. with antioxidant, beauty and whitening effects. In the examples, preparation solvents similar to each component and having better compatibility are used, and a new catalyst is added during the extraction process, so that the purity of the preparation is higher, the product quality is better, and there is better beauty in the actual use process. Whitening effect.

This specific embodiment is only an explanation of the present invention, and it is not a limitation of the present invention. Those skilled in the art can make modifications to this embodiment without creative contribution as needed after reading this description, but as long as the claims of the present invention are are protected by patent law.

Claims (8)

1. A composition containing concentrated powder of black fruit Aronia melanocarpa fruits, apples, acerola cherries and mulberries is characterized in that: the composition comprises Aronia melanocarpa fruit and berry concentrated powder, apple concentrated powder, needle cherry concentrated powder and mulberry concentrated powder, wherein the anthocyanin content in the Aronia melanocarpa fruit and berry concentrated powder is 1% -4%, the polyphenol content in the apple concentrated powder is 30% -50%, the vitamin C content in the needle cherry concentrated powder is 15% -20%, and the anthocyanin content in the mulberry concentrated powder is 1% -4%.

2. A method of preparing the composition of the concentrated powder of chokeberry, apple, acerola and mulberry of claim 1, comprising the steps of:

preparation of anthocyanin in Aronia melanocarpa fruits in step (1)

Taking fresh Aronia melanocarpa fruits and pomace obtained after juice extraction, freeze-drying and crushing to obtain whole fruits and pomace powder for later use; accurately weighing a plurality of powder of the whole fruit and the fruit residue of the Sorbus pohuashanensis, using ethanol and acetic acid acidified water with different concentrations as auxiliary catalysts, performing ultrasonic auxiliary extraction, and centrifuging, concentrating and freeze-drying to obtain the anthocyanin extract of the whole fruit and the fruit residue of the Sorbus pohuashanensis; adding the concentrated anthocyanin extract into a column which is pre-filled with column chromatography packing, and separating and purifying; collecting each separated purified product, concentrating, and removing residual solvent to obtain anthocyanin;

step (2) preparation of polyphenols in apples

Crushing immature apples into apple pomace for later use by using a crusher, accurately weighing a plurality of apple pomace, putting the apple pomace into a conical flask, adding a certain amount of mixed solvent of hydrochloric acid, ethanol and acetone, and putting the apple pomace on a magnetic stirrer for stirring and dissolving for a period of time; then filtering, separating and purifying to obtain an ethanol acidic solution rich in polyphenol; evaporating ethanol by heating in magnetic stirring water bath, concentrating, and freeze drying to obtain apple polyphenol;

step (3) preparation of vitamin C in acerola cherry

Taking fresh acerola fruits and pomace after juice extraction, freeze-drying and crushing for later use, accurately weighing acerola pomace powder, continuously stirring to dissolve the acerola pomace powder by using trifluoroacetic acid as a catalyst and ethanol as a main extractant, putting the mixture of the acerola pomace into a membrane cavity of ultrafiltration equipment for ultrafiltration to obtain concentrated slurry rich in vitamin C, concentrating the concentrated slurry by using low-pressure and high-temperature conditions of a rotary evaporator, removing water, and freeze-drying to obtain acerola concentrated powder containing the vitamin C;

preparation of anthocyanin in mulberries in step (4)

Washing fresh mulberries with distilled water, airing, putting a certain amount of mulberries into a clean mortar, grinding for a certain time until the pulp of the mulberries and the peel are ground, crushed and uniform, and paying attention to exposure during grinding; accurately weighing certain grinding uniform mulberry powder and a conical flask, adding ethanol solution with certain mass fraction and catalyst methyl tertiary butyl ether, and extracting for a certain time by using a microwave auxiliary extraction instrument; filtering the extracting solution, concentrating in a rotary evaporator, and removing water to obtain mulberry concentrated powder rich in anthocyanin;

synthesis of the composition powder of step (5)

Adding mixed powder of Aronia melanocarpa fruit concentrated powder, apple polyphenol concentrated powder, acerola cherry concentrated powder and mulberry concentrated powder into an extraction tank, extracting, adding a certain pectase solution, soaking at room temperature, filtering to obtain trapped liquid, adding a certain maltodextrin into the trapped liquid, concentrating and mixing, feeding the concentrated and mixed material into drying equipment by a high-pressure pump, drying, and sieving to obtain a concentrated powder composition.

3. The preparation of the composition containing the concentrated powder of Aronia melanocarpa fruits, apples, acerola cherries and mulberries according to claim 2, which is characterized in that: the preparation of anthocyanin in the Aronia melanocarpa fruits comprises the steps of taking fresh Aronia melanocarpa fruits and pomace obtained after juicing the fruits, freeze-drying, crushing, and sieving with a 40-60-mesh sieve to obtain whole fruits and pomace powder for later use; accurately weighing 2-4 g of the powder of the whole fruit and the fruit residue of the Sorbus pohuashanensis, adding 2-5 mL of acetic acid water as an auxiliary catalyst, performing ultrasonic auxiliary extraction by using an ethanol solvent with the volume fraction of 60% -80%, and centrifuging, concentrating and freeze-drying to obtain the anthocyanin extract of the whole fruit and the fruit residue of the Sorbus pohuashanensis; adding the concentrated anthocyanin extract into a column which is pre-filled with column chromatography packing, and separating and purifying; and then collecting each separated purified product, concentrating, and removing residual solvent to obtain the Aronia melanocarpa fruit powder containing 1% -4% of anthocyanin.

4. The preparation of the composition containing the concentrated powder of Aronia melanocarpa fruits, apples, acerola cherries and mulberries according to claim 2, which is characterized in that: the preparation of polyphenol in apples comprises the steps of crushing immature apples into apple residues by a crusher for standby, sieving the apple residues by a 40-60-mesh sieve, accurately weighing 5-8 g of apple residues, putting the apple residues into a conical flask, adding 1-3 mL of 0.1-0.2 mol/L hydrochloric acid and 10-15 mL of ethanol and acetone mixed solvent with volume fraction of 60% -80%, and stirring and dissolving the apple residues on a magnetic stirrer for 30-60 minutes; then filtering, separating and purifying to obtain an ethanol acidic solution rich in polyphenol; evaporating ethanol by heating in magnetic stirring water bath, concentrating, and freeze drying to obtain apple powder containing 30% -50% polyphenol.

5. The method for preparing the composition containing the concentrated powder of the black chokeberry, the apple, the acerola cherry and the mulberry, as claimed in claim 4, which is characterized in that: the preparation of vitamin C in acerola cherry comprises the steps of taking fresh acerola cherry fruits and pomace after juice squeezing, freeze-drying and crushing for later use, sieving with a 40-60-mesh sieve, accurately weighing 6-10 g of acerola cherry pomace powder, adding 2-3 mL of catalyst trifluoroacetic acid and 15-20 mL of ethanol with volume fraction of 60-80%, stirring for 30-60 min to completely dissolve, then carrying out light-proof cold soaking for 3-5 h, putting the mixture of the cold soaked acerola cherry pomace into a membrane cavity of ultrafiltration equipment for ultrafiltration to obtain concentrated slurry rich in vitamin C, concentrating the concentrated slurry under the low-pressure and high-temperature conditions of a rotary evaporator, removing moisture, and carrying out freeze-drying to obtain acerola cherry concentrated powder containing 17% -19% of vitamin C; ultrafiltration device parameters: diameter: 90-100, membrane area: 16.8 to 17.2m ² Molecular weight cut-off: 10000-100000 daltons, membrane filament diameter: the outer diameter is 0.5-0.8 mm, and the inner diameter is 0.2-0.4 mm.

6. The preparation of the composition containing the concentrated powder of Aronia melanocarpa fruits, apples, acerola cherries and mulberries according to claim 2, which is characterized in that: the preparation of anthocyanin in the mulberries in the step (4) comprises the steps of washing fresh mulberries with distilled water, airing, taking mulberries, putting the mulberries into a clean mortar, grinding for 2-3 hours until the pulp of the mulberries and the peel are ground, crushed and uniform, and paying attention to exposure during grinding; accurately weighing 5-8 g of uniformly ground mulberry powder and a conical flask, adding 10-15 mL of ethanol solution with volume fraction of 60% -80% and 1-3 mL of catalyst methyl tertiary butyl ether, and extracting for 30-60 minutes by using a microwave-assisted extraction instrument; filtering the extracting solution, concentrating the extracting solution in a rotary evaporator, and removing water to obtain mulberry concentrated powder containing 1% -4% anthocyanin.

7. The preparation of the composition containing the concentrated powder of Aronia melanocarpa fruits, apples, acerola cherries and mulberries according to claim 2, which is characterized in that: the synthesis of the composition powder in the step (5) comprises the steps of taking 20-40 g of mixed powder of Aronia melanocarpa fruit concentrated powder, apple polyphenol concentrated powder, acerola cherry concentrated powder and mulberry concentrated powder which are sieved by a 30-50 mesh sieve, and putting the mixed powder into an extraction tank, wherein the extraction pressure is 20-30 MPa, the extraction temperature is 50-70 ℃, and the extraction time is 2-3 hours; then adding 5-10 mL of pectase solution, soaking for 30-60 minutes at room temperature, filtering to obtain trapped fluid, adding 5-8 g of maltodextrin into the trapped fluid, concentrating and mixing, conveying the concentrated and mixed material into a drying device by a high-pressure pump for drying, and sieving to obtain a concentrated powder composition.

8. Use of the composition comprising concentrated powder of chokeberry, apple, acerola and mulberry of claim 1, characterized in that: the product can be used for caring skin, resisting oxidation, and whitening skin.