Preparation method of sugarcane polyphenols with caramel flavor

Abstract

The present invention relates to the technical field of natural active substance extraction, and more particularly to a method for preparing sugarcane polyphenols with a caramel flavor. The method comprises the following steps: (1) taking sugarcane molasses and diluting it; (2) biological fermentation, inactivation, cooling, and filtering; (3) chromatography through four macroporous resin columns connected in series, gradient elution, and low-temperature concentration; and (4) alcohol precipitation, concentration, paste formation, and drying to obtain a sugarcane polyphenol composition. This method utilizes biological fermentation combined with gradient elution using four macroporous resin columns connected in series with different solvents, and utilizes the separation of active ingredients and impurities to optimize the purity of the sugarcane polyphenols. The process is simple, safe throughout, and suitable for large-scale factory production. The resulting sugarcane polyphenol composition has a polyphenol content greater than 20%, good water solubility, and a caramel flavor. The composition can be widely used in foods, health products, beverages, and the like.

Description

Technical Field

[0001] The invention relates to the technical field of natural active substance extraction, and in particular to a method for preparing sugarcane polyphenols with caramel flavor. Background Art

[0002] my country produces a huge amount of sugarcane each year and has abundant sugarcane resources. Sugarcane contains phenolic acids, flavonoids, and other phenolic compounds. Polyphenol extracts from sugarcane have certain effects in scavenging free radicals and providing antioxidant benefits. They can also be used to lower cholesterol, combat obesity, fight diabetes, provide antibacterial properties, and preserve fresh produce. Sugarcane molasses (also known as molasses in English) is the thick liquid left after the sugar industry processes the squeezed sugarcane juice through heating, neutralization, precipitation, filtration, concentration, and crystallization. Molasses is not only an energy source but also has advantages such as rapid digestion and absorption, improved palatability, reduced dust, and improved granule quality. Sugarcane molasses is rich in a large number of high-value-added products. Therefore, it is necessary to intensify research on sugarcane molasses, innovate simpler and more efficient extraction methods to extract the natural active substances in sugarcane molasses, and develop broader research and application areas for sugarcane polyphenol extracts.

[0003] Currently, most research focuses on sugarcane peel and sugarcane scum. For example, CN105816702A discloses a method for preparing a sugarcane polyphenol extract using sugarcane or bagasse as raw materials. However, research on molasses, the final product of sugar production, is limited. The present invention provides a method for producing sugarcane polyphenols from molasses. Summary of the Invention

[0004] The object of the present invention is to provide a method for preparing a sugarcane polyphenol composition with a caramel flavor by using sugarcane molasses, wherein the method separates effective ingredients from impurities and optimizes the purity of the sugarcane polyphenols.

[0005] The preparation method comprises the following steps:

[0006] (1) Take sugarcane molasses and dilute it;

[0007] (2) Biological fermentation, inactivation, cooling, and filtration;

[0008] (3) chromatography through four large-pore columns connected in series, gradient elution, and cryogenic concentration;

[0009] (4) alcohol precipitation, concentration, paste making, and drying to obtain a sugarcane polyphenol composition.

[0010] The sugarcane molasses in step (1) has a polyphenol content of 2.5% and a solid content of 70%, which is diluted with pure water to a solid content of 7-10%.

[0011] Step (2) specifically comprises adding highly active yeast, fermenting at 30-32° C. for 4-6 hours, then heating to greater than 98° C., maintaining for 5-10 minutes, cooling to 25-30° C., filtering through a 200-mesh filter cloth, and obtaining liquid 1.

[0012] The highly active yeast is Angel Yeast, and the added amount is 0.5-1wt.% of the amount of sugarcane molasses.

[0013] The model of the macroporous resin is xda-6, DM18 or LK-83S, and the manufacturer is Xi'an Lanxiao Biopharmaceutical Co., Ltd.

[0014] The mass ratio of the amount of each macroporous resin to the solid content in the sugarcane molasses is 1:1.

[0015] The chromatography through four series-connected macroporous columns in step (3) includes: the drug solution 1 first enters the first resin, and after entering, it is eluted with pure water, and the effluent 1 and the water washing liquid 1 are collected and merged into the drug solution 2; the drug solution 2 enters the second resin, and after entering, it is eluted with pure water, and the effluent 2 and the water washing liquid 2 are collected and merged into the drug solution 3; the drug solution 3 enters the third resin, and after entering, it is eluted with pure water, and the effluent 3 and the water washing liquid 3 are collected and merged into the drug solution 4; the drug solution 4 enters the fourth resin, and after entering, the four resins are eluted again with pure water in turn, until the effluent is clear and transparent; the amount of pure water used for elution after entering the first to third resins is 0.5-1 times the amount of resin, and the amount of pure water used for elution again after entering the fourth resin is 2-4 times the amount of resin.

[0016] The gradient elution described in step (3) includes: eluting four resins simultaneously, first eluting with 10% ethanol to wash away impurities, and then eluting with 50-60% ethanol. After the effluent is dried and the polyphenol content is detected to be greater than 0.8%, the ethanol eluate is collected and the eluates of the second and third resins are combined.

[0017] The concentration in step (3) is to concentrate the combined eluate using a low-temperature concentrator at a temperature < 60° C. until it is alcohol-free and the concentration is 48-52 BRIX.

[0018] Furthermore, the elution volume of the 10% ethanol elution is 2-5 times the amount of resin, and the elution flow rate is 1-1.5 BV / h; the elution volume of the 50-60% ethanol elution is 2-4 times the amount, and the elution flow rate is 0.8-2 BV / h.

[0019] Step (4) specifically comprises adding 3-4 times the volume of pure methanol or anhydrous ethanol of the concentrate, sealing well, keeping stirring constantly, keeping at 4-6° C. for 1-2 hours, centrifuging, taking the supernatant and concentrating it to be alcohol-free, making a paste to a Brix of 35-40 BRIX, spray drying, and obtaining a sugarcane polyphenol composition.

[0020] The sugarcane polyphenol composition contains 20-25% of polyphenols, 1-20% of flavonoids and 0.1-2% of polysaccharides.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] (1) Biofermentation combined with gradient elution of four macroporous resins in series with different solvents was used to separate the active ingredients from the impurities to optimize the purity of sugarcane polyphenols, and the polyphenol content was later obtained to be greater than 20%.

[0023] (2) Low temperature stirring and alcohol precipitation further increase the content of polyphenols and active ingredients, while also taking into account the decolorization effect. At the same time, water is added for concentration to remove ethanol residues and spray to ensure that the product has no solvent residues and meets the needs of the development of big health.

[0024] (3) The preparation method is simple, safe, and environmentally friendly throughout the process, and is suitable for large-scale factory production. The obtained sugarcane polyphenol composition has good water solubility and a burnt aroma, and can be widely used in food, health products, beverages, etc. DETAILED DESCRIPTION

[0025] The following examples further illustrate the specific implementation of the present invention, but the implementation and protection of the present invention are not limited thereto. It should be noted that if there are any processes not specifically described below, they can be implemented or understood by those skilled in the art with reference to the existing technology.

[0026] Example 1

[0027] Take 428.6 g of sugarcane molasses (polyphenol content of 2.5%, solid content of 70%) and dilute it with purified water until the solid content reaches 7%.

[0028] Add 3g of highly active yeast (Angel Yeast), ferment at 32℃ for 5 hours, heat to 99℃, keep for 10 minutes to inactivate, cool the solution, wait for the solution to cool to 28℃, and filter the solution through a 200-mesh filter cloth.

[0029] The drug solution was chromatographed over four macroporous resins (DM18, Xi'an Lanxiao Biotechnology Co., Ltd.) connected in series, with each resin using 300 g. The drug solution was first introduced into the first resin (column flow rate was 1 BV / h), and after the introduction, it was eluted with 300 mL of pure water, and the effluent and the washing liquid were collected and combined together; the drug solution was introduced into the second resin, and after the second resin had completely introduced the drug solution, it was eluted with 300 mL of pure water, and the effluent and the washing liquid were collected and combined together; the drug solution was introduced into the third resin, and after the third resin had completely introduced the drug solution, it was eluted with 300 mL of pure water, and the effluent and the washing liquid were collected and combined together; the drug solution was introduced into the fourth resin, and after the fourth resin had completely introduced the drug solution, the four resins were eluted again with pure water in sequence until the effluent was clear and transparent (the dosage was 1200 mL of pure water). Gradient elution: Elution of all four resins simultaneously begins with 10% ethanol at a volume of 600 mL and a flow rate of 1.5 BV / h to remove impurities. Then, elution is performed with 50% ethanol at a volume of 900 mL and a flow rate of 1.5 BV / h. After the collected effluent is dried and tested for polyphenol content exceeding 0.8%, the 50% ethanol eluate is collected and combined with the eluates from the second and third resins. Concentrate to an alcohol-free state using a cryogenic concentrator (temperature <60°C) and to 48 BRIX. Add an equal volume of anhydrous ethanol, seal tightly, and maintain constant stirring. After incubating at 6°C for 1 hour, centrifuge and concentrate the supernatant to an alcohol-free state, making a paste to 35 BRIX.

[0030] The sugarcane polyphenol composition was obtained by spray drying. Testing showed that the composition contained 22% polyphenols, 20% flavonoids and 2% polysaccharides.

[0031] Example 2

[0032] Take 428.6 g of sugarcane molasses (polyphenol content of 2.5%, solid content of 70%) and dilute it with pure water until the solid content is 8%.

[0033] Add 1.5g of highly active yeast (Angel Yeast), ferment at 30℃ for 4 hours, heat to 100℃, keep for 10 minutes to inactivate, cool the solution, wait for the solution to cool to 25℃, and filter the solution through a 200-mesh filter cloth.

[0034] The drug solution was chromatographed over four macroporous resins (Xi'an Lanxiao Biotechnology Co., Ltd., xda-6) connected in series, with each resin using 300 g of the drug solution. The drug solution was first introduced into the first resin (column flow rate was 1.5 BV / h), and after the introduction, it was eluted with 150 mL of pure water, and the effluent and the washing liquid were collected and merged together; the drug solution was introduced into the second resin, and after the second resin had completely introduced the drug solution, it was eluted with 150 mL of pure water, and the effluent and the washing liquid were collected and merged together; the drug solution was introduced into the third resin, and after the third resin had completely introduced the drug solution, it was eluted with 150 mL of pure water, and the effluent and the washing liquid were collected and merged together; the drug solution was introduced into the fourth resin, and after the fourth resin had completely introduced the drug solution, the four resins were eluted again with pure water in sequence until the effluent was clear and transparent (the dosage was 900 mL of pure water). Gradient elution: Four resins are eluted simultaneously. First, use 10% ethanol with an elution volume of 900 mL and an elution flow rate of 1 BV / h to remove impurities. Then use 60% ethanol with an elution volume of 900 mL and an elution flow rate of 0.8 BV / h. After the collected effluent is dried and the polyphenol content is greater than 0.8%, start collecting the 60% ethanol eluate and combine the eluates from the second and third resins. Use a low-temperature concentrator (temperature <60°C) to concentrate to alcohol-free and to 52 BRIX. Add 4 times the volume of pure methanol, seal tightly, keep stirring continuously, keep at 4°C for 2 hours, centrifuge, and take the supernatant and concentrate to alcohol-free, making a paste to 40 BRIX.

[0035] The sugarcane polyphenol composition was obtained by spray drying. Testing showed that the composition contained 20% polyphenols, 15% flavonoids and 1% polysaccharides.

[0036] Example 3

[0037] Take 428.6 g of sugarcane molasses (polyphenol content of 2.5%, solid content of 70%) and dilute it with pure water until the solid content is 10%.

[0038] Add 1.5g of highly active yeast (Angel Yeast), ferment at 31°C for 6 hours, heat to 99°C, keep for 8 minutes to inactivate, cool the solution, wait for the solution to cool to 28°C, and filter through a 200-mesh filter cloth.

[0039] The drug solution was chromatographed over four macroporous resins (LK-83S, Xi'an Lanxiao Biotechnology Co., Ltd.) in series, with each resin using 300 g of the drug solution. The drug solution was first introduced into the first resin (with a column flow rate of 1.5 BV / h). After the introduction, it was eluted with 300 mL of pure water, and the effluent and the washing liquid were collected and merged together; the drug solution was introduced into the second resin, and after the second resin had completely introduced the drug solution, it was eluted with 300 mL of pure water, and the effluent and the washing liquid were collected and merged together; the drug solution was introduced into the third resin, and after the third resin had completely introduced the drug solution, it was eluted with 300 mL of pure water, and the effluent and the washing liquid were collected and merged together; the drug solution was introduced into the fourth resin, and after the fourth resin had completely introduced the drug solution, the four resins were eluted again with pure water in sequence until the effluent was clear and transparent (using 600 mL of pure water). Gradient elution: Elution of four resins simultaneously: first, elution with 10% ethanol, elution volume of 1500mL, elution flow rate of 1BV / h to remove impurities; then elution with 55% ethanol, elution volume of 900mL, elution flow rate of 2BV / h; after the collected effluent is dried and the polyphenol content is greater than 0.8%, start collecting the 55% ethanol eluate and combine the eluates of the second and third resins. Use a low-temperature concentrator (temperature <60°C) to concentrate to alcohol-free and concentrate to 50BRIX. Add 4 times the volume of pure methanol, seal well, keep stirring continuously, keep at 5°C for 1.5 hours, centrifuge, take the supernatant and concentrate to alcohol-free, and make a paste to 38BRIX.

[0040] The sugarcane polyphenol composition was obtained by spray drying. Testing showed that the composition contained 22% polyphenols, 18% flavonoids and 0.5% polysaccharides.

[0041] The above embodiments are only preferred implementation modes of the present invention and are only used to explain the present invention rather than to limit the present invention. Any changes, substitutions, modifications, etc. made by those skilled in the art without departing from the spirit of the present invention should fall within the scope of protection of the present invention.

Claims

1. A method for preparing sugarcane polyphenols with caramel flavor, characterized in that: The preparation method comprises the following steps: (1) Take sugarcane molasses and dilute it; (2) Biological fermentation, inactivation, cooling, and filtration; (3) chromatography through four macroporous resin columns connected in series, gradient elution, and cryogenic concentration; (4) alcohol precipitation, concentration, paste making, and drying to obtain a sugarcane polyphenol composition; The step (2) specifically comprises adding highly active yeast, fermenting at 30-32° C. for 4-6 hours, then heating to greater than 98° C., maintaining for 5-10 minutes, cooling to 25-30° C., and filtering through a 200-mesh filter cloth to obtain a first liquid; the highly active yeast is Angel Yeast, and the amount added is 0.5-1 wt.% of the amount of sugarcane molasses; The chromatography through four series-connected macroporous resin columns in step (3) includes: the first liquid is first introduced into the first macroporous resin column, and after the liquid is introduced, it is eluted with pure water, and the first effluent and the first water washing liquid are collected and merged into the second liquid; the second liquid is introduced into the second macroporous resin column, and after the liquid is introduced, it is eluted with pure water, and the second effluent and the second water washing liquid are collected and merged into the third liquid; the third liquid is introduced into the third macroporous resin column, and after the liquid is introduced, it is eluted with pure water, and the third effluent and the third water washing liquid are collected and merged into the fourth liquid; the fourth liquid is introduced into the fourth macroporous resin column, and after the liquid is introduced, the four macroporous resin columns are eluted with pure water again in sequence until the effluent is clear and transparent; the amount of pure water used for elution after the liquid is introduced into the first to third macroporous resin columns is 0.5-1 times the amount of resin, and the amount of pure water used for elution after the liquid is introduced into the fourth macroporous resin column is 2-4 times the amount of resin; The gradient elution described in step (3) includes: eluting with four macroporous resin columns at the same time, first eluting with 10% ethanol to wash away impurities, and then eluting with 50-55% ethanol. After the effluent is dried and the polyphenol content is detected to be greater than 0.8%, the ethanol eluate is collected and the eluates from the second and third macroporous resin columns are combined; the elution volume of the 10% ethanol elution is 2-5 times the amount of resin, and the elution flow rate is 1-1.5 BV / h; the elution volume of the 50-55% ethanol elution is 2-4 times the amount, and the elution flow rate is 0.8-2 BV / h; Step (4) specifically comprises adding 3-4 times the volume of pure methanol or anhydrous ethanol of the concentrate, sealing well, keeping stirring constantly, keeping at 4-6° C. for 1-2 hours, centrifuging, taking the supernatant and concentrating it to be alcohol-free, making a paste to a Brix of 35-40 BRIX, spray drying, and obtaining a sugarcane polyphenol composition.

2. The preparation method according to claim 1, characterized in that The sugarcane molasses in step (1) has a polyphenol content of 2.5% and a solid content of 70%, which is diluted with pure water to a solid content of 7-10%.

3. The preparation method according to claim 1, characterized in that The mass ratio of the resin dosage of each macroporous resin column to the solid content in the sugarcane molasses is 1:1, and the model of the macroporous resin is xda-6, DM18 or LK-83S.

4. The preparation method according to claim 1, characterized in that The low-temperature concentration in step (3) is to concentrate the combined eluate using a low-temperature concentrator at a temperature < 60° C. until it is alcohol-free and the concentration is 48-52 BRIX.

5. The preparation method according to claim 1, characterized in that The sugarcane polyphenol composition contains 20-25% of polyphenols, 1-20% of flavonoids and 0.1-2% of polysaccharides.