Preparation method of soluble soybean polysaccharide

Abstract

The invention discloses a preparation method of soluble soybean polysaccharide. The method comprises the following steps: dissolving soybean phospholipid in n-hexane, adding 50-60% ethyl acetate-water solution, stirring, extracting, standing for layering, taking the lower ethyl acetate-water phase, concentrating and recovering ethyl acetate, concentrating the residual water phase through a ceramic membrane, intercepting macromolecular impurities, diluting the intercepted phase with water, continuously concentrating, and concentrating the permeate through a nanofiltration membrane to remove small molecular impurities, thereby obtaining the soybean phospholipid. And carrying out spray drying on a trapped phase of the nanofiltration membrane to obtain a product. The preparation method has the following beneficial effects: soybean lecithin is used as a raw material, so that the source of soluble soybean polysaccharide is expanded; through a specific membrane separation process, the purity of the soluble soybean polysaccharide is greater than or equal to 85%, and the net extraction rate is greater than or equal to 95%; the production process is simple, and large-scale industrial production is easy to realize.

Description

Technical Field

[0001] The invention belongs to the technical field of phospholipids, and in particular relates to a method for preparing soluble soybean polysaccharide. Background Art

[0002] Soybean polysaccharide is a complex carbohydrate, mainly composed of galactose, mannose, arabinose and galacturonic acid. Compared with traditional plant collagen, animal gelatin, etc., soybean polysaccharide has better water solubility, stability and safety. These unique properties make soybean polysaccharide have broad application prospects in food, medicine, cosmetics and other fields. In the food industry, soluble soybean polysaccharide can be used as thickener, stabilizer, emulsifier and gelling agent to improve the taste, texture and stability of food. For example, adding soybean polysaccharide to ice cream can improve its anti-melting property, so that ice cream can still maintain a good taste and texture at a higher temperature. In addition, soybean polysaccharide can also be used to make jelly, jam, beverages and other foods to improve the nutritional value and health care function of the product. In the field of medicine, soluble soybean polysaccharide is widely used in drug carriers, sustained-release preparations and biomaterials due to its good biocompatibility and low toxicity. Studies have shown that soybean polysaccharide can combine with drug molecules to form a stable drug carrier to achieve targeted delivery and sustained release of drugs. In addition, soybean polysaccharides can also be used as biomaterials in fields such as tissue engineering and regenerative medicine to promote cell growth and differentiation. In the field of cosmetics, soluble soybean polysaccharides are widely used in skin care products, makeup and hair products due to their excellent moisturizing, viscosity and film-forming properties. Soybean polysaccharides can bind to receptors on the surface of skin cells and promote hydration between cells, thereby playing a moisturizing and anti-aging role. At the same time, soybean polysaccharides can also increase the viscosity and film-forming properties of cosmetics, and improve the product's user experience and stability. With people's pursuit of healthy diet and green life, the market demand for soluble soybean polysaccharides will continue to grow. In the future, researchers and enterprises should continue to conduct in-depth research and development of soybean polysaccharide application technologies to promote their application and development in more fields. Summary of the invention

[0003] The object of the present invention is to provide a method for separating high-purity soluble soybean polysaccharides from soybean lecithin, which has simple process and is easy to industrialize.

[0004] The above-mentioned object of the present invention is achieved by the following technical means: dissolving soybean lecithin in n-hexane, adding 50-60% ethyl acetate, stirring and extracting, standing and stratifying, taking the lower ethyl acetate-water phase and concentrating to recover ethyl acetate, the remaining water phase is first concentrated by a ceramic membrane to intercept macromolecular impurities, the intercepted phase is diluted with water and further concentrated, the permeate is concentrated by a nanofiltration membrane to remove small molecular impurities, and the intercepted phase of the nanofiltration membrane is taken and spray-dried to obtain the product.

[0005] The soybean lecithin of the present invention is soluble in n-hexane, and the ratio of the soybean lecithin to n-hexane is 1:4-1:5 calculated by mass volume percentage.

[0006] The invention adds 50-60% ethyl acetate into n-hexane, and the ratio of n-hexane to 50-60% ethyl acetate is 1:1-1:1.5 calculated by volume percentage.

[0007] The soybean lecithin of the present invention is mixed with normal hexane and 50-60% ethyl acetate for extraction for 60-90 minutes at a temperature of 30-35°C.

[0008] The soybean lecithin of the present invention is mixed with normal hexane and 50-60% ethyl acetate and then left to stand for 2-3 hours.

[0009] The present invention recovers ethyl acetate from the lower ethyl acetate-water phase after static stratification. The recovery end point is that the ethyl acetate content in the water phase is ≤1.0% calculated by volume percentage.

[0010] The residual water phase of the present invention is concentrated by a ceramic membrane, and the pore size of the ceramic membrane is 500nm.

[0011] The water phase intercepted by the ceramic membrane of the present invention is diluted with water and further concentrated. Calculated by volume percentage, the ratio of the dilution water to the original solution is 8:1 to 9:1.

[0012] The permeate passing through the 500nm ceramic membrane of the present invention is concentrated by a nanofiltration membrane, the molecular weight of the nanofiltration membrane is 5000Da, and the concentration ratio is 9:1-10:1 calculated by volume percentage.

[0013] The interception phase of the present invention is spray-dried through a 5000Da nanofiltration membrane, and the spray-drying conditions are: an inlet air temperature of 140°C, an outlet air temperature of 95°C, and a feed rate of 5L / h.

[0014] The present invention uses soybean lecithin as a raw material, expands the source of soluble soybean polysaccharides, and the soluble soybean polysaccharide content in soybean lecithin is higher than that in soybean meal; the present invention adopts a specific membrane separation technology, combines ceramic membranes and nanofiltration membranes with different pore sizes to achieve separation of soybean polysaccharides and impurities, and purification of soybean polysaccharides; the specific membrane separation technology can achieve separation of impurities and retention of soybean polysaccharide components according to the molecular weight and the oil-water affinity of the material, and can separate high-purity soluble soybean polysaccharides from soybean lecithin.

[0015] The present invention uses only organic solvents and membrane separation in the soybean polysaccharide extraction process, and the process does not involve chemical reactions and high-temperature treatment, which has a beneficial effect on the maximum retention of soybean polysaccharides. The product purity and net extraction rate of the separated soluble soybean polysaccharides are high, and soybean lecithin is used as a raw material. The soluble soybean polysaccharides in the soybean lecithin are higher, and the yield of the extracted soluble soybean polysaccharides is higher, the product purity is ≥85%, and the product net extraction rate is ≥95%. In addition, by setting the extraction time, extraction temperature, ceramic membrane pore size, and nanofiltration membrane molecular weight, the separation effect of separating residual lecithin in soybean polysaccharides and other impurities with different oil and water properties is optimal under the set parameter conditions. DETAILED DESCRIPTION

[0016] The following examples are only used to illustrate the present invention, and the protection scope of the present invention is not limited to the following examples. A person skilled in the art can achieve the purpose of the present invention according to the above disclosure of the present invention and the range of each parameter.

[0017] Example 1

[0018] Weigh 500g soybean lecithin (wherein the soluble soybean polysaccharide content is 10.5%), dissolve in 2000ml n-hexane, add 2000ml 50% ethyl acetate-water solution, extract at 35℃ for 60min, let stand for stratification for 2h, separate and obtain 1950ml of lower ethyl acetate-water phase, concentrate and recover ethyl acetate, concentrate until the ethyl acetate content in the water phase is ≤1.0%, obtain 980ml of water phase, concentrate the water phase through a 500nm ceramic membrane, add 8820ml of water to continue concentrating when the concentration is almost over, collect and obtain 7800ml of water phase permeated through the ceramic membrane, pass the permeated water phase through a 5000Da nanofiltration membrane, stop concentrating when 7000ml of water phase is concentrated, and spray dry the nanofiltration membrane intercepted phase. The conditions of spray drying are: inlet air temperature 140℃, outlet air temperature 95℃, feed rate 5L / h, and obtain 58.0g product with a product purity of 87.6%.

[0019] Example 2

[0020] Weigh 500g soybean lecithin (wherein the soluble soybean polysaccharide content is 11.3%), dissolve in 2500ml n-hexane, add 2500ml 50% ethyl acetate-water solution, extract at 35℃ for 30min, let stand for stratification for 3h, separate and obtain 2450ml of lower ethyl acetate-water phase, concentrate and recover ethyl acetate, concentrate until the ethyl acetate content in the water phase is ≤1.0%, obtain 1200ml of water phase, concentrate the water phase through a 500nm ceramic membrane, add 9600ml of water to continue concentrating when the concentration is almost over, collect and obtain 10600ml of water phase permeated through the ceramic membrane, pass the permeated water phase through a 5000Da nanofiltration membrane, stop concentrating when 9500ml of water phase is concentrated, and spray dry the nanofiltration membrane intercepted phase. The conditions for spray drying are: inlet air temperature 140℃, outlet air temperature 95℃, feed rate 5L / h, and obtain 63.3g product with a product purity of 86.5%.

[0021] Example 3

[0022] Weigh 500g soybean lecithin (wherein the soluble soybean polysaccharide content is 9.6%), dissolve in 2000ml n-hexane, add 2500ml 60% ethyl acetate-water solution, extract at 30℃ for 60min, let stand for stratification for 3h, separate and obtain 2450ml of lower ethyl acetate-water phase, concentrate and recover ethyl acetate, concentrate until the ethyl acetate content in the water phase is ≤1.0%, obtain 1200ml of water phase, concentrate the water phase through a 500nm ceramic membrane, add 10800ml of water to continue concentrating when the concentration is almost over, collect and obtain 11800ml of water phase permeated through the ceramic membrane, pass the permeated water phase through a 5000Da nanofiltration membrane, stop concentrating when 10500ml of water phase is concentrated, and spray dry the nanofiltration membrane intercepted phase. The conditions for spray drying are: inlet air temperature 140℃, outlet air temperature 95℃, feed rate 5L / h, and obtain 52.8g product with a product purity of 88.3%.

[0023] Example 4

[0024] Weigh 500g soybean lecithin (wherein the soluble soybean polysaccharide content is 10.5%), dissolve in 2500ml n-hexane, add 3750ml 50% ethyl acetate-water solution, extract at 30℃ for 60min, let stand for stratification for 3h, separate and obtain 3700ml of lower ethyl acetate-water phase, concentrate and recover ethyl acetate, concentrate until the ethyl acetate content in the water phase is ≤1.0%, obtain 1750ml of water phase, concentrate the water phase through a 500nm ceramic membrane, add 14000ml of water to continue concentrating when the concentration is almost over, collect and obtain 11800ml of water phase permeated through the ceramic membrane, pass the permeated water phase through a 5000Da nanofiltration membrane, stop concentrating when 14000ml of water phase is concentrated, and spray dry the nanofiltration membrane intercepted phase. The conditions for spray drying are: inlet air temperature 140℃, outlet air temperature 95℃, feed rate 5L / h, and obtain 56.5g product with a product purity of 89.4%.

[0025] Example 5

[0026] Weigh 500g soybean lecithin (wherein the soluble soybean polysaccharide content is 12.3%), dissolve in 2000ml n-hexane, add 3000ml 60% ethyl acetate-water solution, extract at 35℃ for 30min, let stand for stratification for 2h, separate and obtain 2950ml of lower ethyl acetate-water phase, concentrate and recover ethyl acetate, concentrate until the ethyl acetate content in the water phase is ≤1.0%, obtain 1400ml of water phase, concentrate the water phase through a 500nm ceramic membrane, add 11200ml of water to continue concentrating when the concentration is almost over, collect and obtain 12400ml of water phase permeated through the ceramic membrane, pass the permeated water phase through a 5000Da nanofiltration membrane, stop concentrating when 11050ml of water phase is concentrated, and spray dry the nanofiltration membrane intercepted phase. The conditions of spray drying are: inlet air temperature 140℃, outlet air temperature 95℃, feed rate 5L / h, and obtain 67.5g product with a product purity of 87.3%.

[0027] Example 6

[0028] Weigh 500g soybean lecithin (wherein the soluble soybean polysaccharide content is 11.6%), dissolve in 2000ml n-hexane, add 2000ml 60% ethyl acetate-water solution, extract at 30℃ for 30min, let stand for stratification for 3h, separate and obtain 1950ml of lower ethyl acetate-water phase, concentrate and recover ethyl acetate, concentrate until the ethyl acetate content in the water phase is ≤1.0%, obtain 980ml of water phase, concentrate the water phase through a 500nm ceramic membrane, add 7840ml of water to continue concentrating when the concentration is almost over, collect and obtain 8570ml of water phase permeated through the ceramic membrane, pass the permeated water phase through a 5000Da nanofiltration membrane, stop concentrating when 7670ml of water phase is concentrated, and spray dry the nanofiltration membrane intercepted phase. The conditions of spray drying are: inlet air temperature 140℃, outlet air temperature 95℃, feed rate 5L / h, and obtain 62.8g product with a product purity of 89.8%.

[0029] Example 7

[0030] Weigh 500g soybean lecithin (wherein the soluble soybean polysaccharide content is 10.5%), dissolve in 2000ml n-hexane, add 2000ml 50% ethyl acetate-water solution, extract at 35℃ for 30min, let stand for stratification for 2h, separate and obtain 1950ml of lower ethyl acetate-water phase, concentrate and recover ethyl acetate, concentrate until the ethyl acetate content in the water phase is ≤1.0%, obtain 950ml of water phase, concentrate the water phase through a 500nm ceramic membrane, add 8850ml of water to continue concentrating when the concentration is almost over, collect and obtain 9550ml of water phase permeated through the ceramic membrane, pass the permeated water phase through a 5000Da nanofiltration membrane, stop concentrating when 8500ml of water phase is concentrated, and spray dry the nanofiltration membrane intercepted phase. The conditions for spray drying are: inlet air temperature 140℃, outlet air temperature 95℃, feed rate 5L / h, and obtain 57.9g product with a product purity of 87.5%.

[0031] Example 8

[0032] Weigh 500g soybean lecithin (wherein the soluble soybean polysaccharide content is 9.7%), dissolve in 2500ml n-hexane, add 2500ml 55% ethyl acetate-water solution, extract at 35℃ for 60min, let stand for stratification for 2h, separate and obtain 2450ml of lower ethyl acetate-water phase, concentrate and recover ethyl acetate, concentrate until the ethyl acetate content in the water phase is ≤1.0%, obtain 1200ml of water phase, concentrate the water phase through a 500nm ceramic membrane, add 9600ml of water to continue concentrating when the concentration is almost over, collect and obtain 10500ml of water phase permeated through the ceramic membrane, pass the permeated water phase through a 5000Da nanofiltration membrane, stop concentrating when 9400ml of water phase is concentrated, and spray dry the nanofiltration membrane intercepted phase. The conditions of spray drying are: inlet air temperature 140℃, outlet air temperature 95℃, feed rate 5L / h, and obtain 52.6g product with a product purity of 89.4%.

[0033] Example 9

[0034] Weigh 500g soybean lecithin (wherein the soluble soybean polysaccharide content is 9.3%), dissolve in 2000ml n-hexane, add 3000ml 50% ethyl acetate-water solution, extract at 30℃ for 60min, let stand for stratification for 3h, separate and obtain 2950ml of lower ethyl acetate-water phase, concentrate and recover ethyl acetate, concentrate until the ethyl acetate content in the water phase is ≤1.0%, obtain 1450ml of water phase, concentrate the water phase through a 500nm ceramic membrane, add 13050ml of water to continue concentrating when the concentration is almost over, collect and obtain 14250ml of water phase permeated through the ceramic membrane, pass the permeated water phase through a 5000Da nanofiltration membrane, stop concentrating when 12750ml of water phase is concentrated, and spray dry the nanofiltration membrane intercepted phase. The conditions for spray drying are: inlet air temperature 140℃, outlet air temperature 95℃, feed rate 5L / h, and obtain 51.1g product with a product purity of 88.3%.

[0035] Example 10

[0036] Weigh 500g soybean lecithin (wherein the soluble soybean polysaccharide content is 10.6%), dissolve in 2500ml n-hexane, add 2500ml 60% ethyl acetate-water solution, extract at 30℃ for 30min, let stand for stratification for 2h, separate and obtain 2450ml of lower ethyl acetate-water phase, concentrate and recover ethyl acetate, concentrate until the ethyl acetate content in the water phase is ≤1.0%, obtain 1200ml of water phase, concentrate the water phase through a 500nm ceramic membrane, add 10800ml of water to continue concentrating when the concentration is almost over, collect and obtain 11750ml of water phase permeated through the ceramic membrane, pass the permeated water phase through a 5000Da nanofiltration membrane, stop concentrating when 10450ml of water phase is concentrated, and spray dry the nanofiltration membrane intercepted phase. The conditions for spray drying are: inlet air temperature 140℃, outlet air temperature 95℃, feed rate 5L / h, and obtain 56.9g product with a product purity of 89.4%.

[0037] The test data of Examples 1 to 10 are summarized in Table 1 below:

[0038] Table 1 Test data of Example 1 to Example 10

[0039]

[0040]

[0041] Note 1: Net extraction rate = (product weight * product purity * 100%) / (raw material purity * feed amount)

[0042] As can be seen from Table 1, the purity of the soluble soybean polysaccharide products produced by the 10 embodiments is about 86.5-89.8%, all greater than 85.0%, and the net extraction rate of the soluble soybean polysaccharide is about 95.93-97.18%, all greater than 95.0%. The preparation method of the present invention can separate high-purity soluble soybean polysaccharides from soybean lecithin, and the product has high purity, high net extraction rate, and is easy to produce.

Claims

1. A method for preparing soluble soybean polysaccharide, characterized in that: Soybean lecithin is dissolved in n-hexane, and then 50-60% ethyl acetate-water solution ethyl acetate is added, stirred and extracted, and allowed to stand for stratification. The lower ethyl acetate-water phase is taken and concentrated to recover the ethyl acetate. The remaining water phase is first concentrated by a ceramic membrane to retain large molecular impurities, and the retained phase is diluted with water and further concentrated. The permeate is concentrated by a nanofiltration membrane to remove small molecular impurities, and the retained phase of the nanofiltration membrane is taken and spray-dried to obtain the product.

2. The method for preparing soluble soybean polysaccharide according to claim 1, characterized in that: Calculated by mass volume percentage, the ratio of the soybean lecithin to n-hexane is 1:4 to 1:

5.

3. The method for preparing soluble soybean polysaccharide according to claim 1, characterized in that: Calculated by volume percentage, the ratio of n-hexane to 50-60% ethyl acetate is 1:1 to 1:1.

5.

4. The method for preparing soluble soybean polysaccharide according to claim 1, characterized in that: The extraction time of the mixture of n-hexane and 50-60% ethyl acetate is 60-90 minutes, and the extraction temperature is 30-35°C.

5. The method for preparing soluble soybean polysaccharide according to claim 1, characterized in that: After mixing n-hexane and 50-60% ethyl acetate, the mixture is allowed to stand for 2-3 hours.

6. The method for preparing soluble soybean polysaccharide according to claim 1, characterized in that: Calculated by volume percentage, the end point of recovering ethyl acetate in the lower ethyl acetate-water phase is: the ethyl acetate content in the water phase is ≤1.0%.

7. The method for preparing soluble soybean polysaccharide according to claim 1, characterized in that: After the ethyl acetate is recovered, the remaining aqueous phase is concentrated using a ceramic membrane with a pore size of 500 nm.

8. The method for preparing soluble soybean polysaccharide according to claim 1, characterized in that: The water phase intercepted by the ceramic membrane is diluted with water to continue concentration. Calculated by volume percentage, the ratio of dilution water to original solution is 8:1 to 9:

1.

9. The method for preparing soluble soybean polysaccharide according to claim 7, characterized in that: The permeate passing through the 500nm ceramic membrane is concentrated by a nanofiltration membrane with a molecular weight of 5000Da. Calculated by volume percentage, the concentration ratio is 9:1 to 10:

1.

10. The method for preparing soluble soybean polysaccharide according to claim 9, characterized in that: The intercept phase was spray dried through a 5000Da nanofiltration membrane, and the spray drying conditions were: inlet air temperature 140°C, outlet air temperature 95°C, and feed rate 5L / h.

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