Comprehensive extraction method of wolfberry functional components for industrial pilot

Abstract

A comprehensive extraction method of efficacy components of industrial pilot wolfberry, comprising the following steps: wolfberry dry fruit is crushed to 100-150 mesh by air cooling crusher, first put into subcritical extraction kettle to extract wolfberry carotenoids and oil; the residue after subcritical extraction is continuously extracted with water, and the water extract is filtered by membrane to obtain wolfberry polysaccharide; the residue after water extraction is continuously extracted with ethanol to obtain crude extract of alkaloids, and the crude extract is continuously purified by macroporous resin separation column to obtain wolfberry alkaloids.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of extraction of active substances from Lycium barbarum, and particularly relates to a comprehensive extraction method of functional components of Lycium barbarum for industrial pilot test. BACKGROUND

[0002] Lycium barbarum is a traditional medicinal and edible plant resource. Modern medical research shows that Lycium barbarum has multiple active effects such as reducing blood sugar, reducing blood pressure, reducing blood lipids, antioxidant, anti-aging, anti-fatigue, anti-tumor, protecting the reproductive system, and immune regulation. Lycium barbarum is rich in Lycium barbarum polysaccharide, carotenoids, alkaloids and other unique bioactive substances. These active ingredients are important material basis for Lycium barbarum to exert efficacy.

[0003] Although the Lycium barbarum industry is booming and the industrial scale is continuously growing, there is a technical problem of low processing conversion rate. 80% of the products are circulated in the market in the form of dried fruits. The main reason is the lack of comprehensive extraction and utilization process technology of multiple characteristic active ingredients of Lycium barbarum. This status makes the Lycium barbarum processing industry lag behind the needs of its own industrial development, becoming a bottleneck restricting the high-quality development of the industry. SUMMARY

[0004] Therefore, the present application discloses a comprehensive extraction method of functional components of Lycium barbarum for industrial pilot test to solve the technical problems of low processing conversion rate and lack of comprehensive extraction and processing technology of Lycium barbarum.

[0005] A comprehensive extraction method of functional components of Lycium barbarum for industrial pilot test comprises the following steps:

[0006] The dried Lycium barbarum fruit is crushed to 100-150 meshes by a forced air cooling crusher, and then is first put into a subcritical extraction kettle to extract Lycium barbarum carotenoids and oil;

[0007] The residue after subcritical extraction is continuously extracted with water, and Lycium barbarum polysaccharide is obtained by membrane filtration of the water extract;

[0008] The residue after water extraction is continuously extracted with ethanol to obtain a crude extract of alkaloids, and the crude extract is continuously purified by a macroporous resin separation column to obtain Lycium barbarum alkaloids.

[0009] In the above-mentioned comprehensive extraction method of functional components of Lycium barbarum for industrial pilot test, the dried Lycium barbarum fruit is crushed to 100-150 meshes by a forced air cooling crusher, and then is first put into a subcritical extraction kettle to extract Lycium barbarum carotenoids and oil; the residue after subcritical extraction is continuously extracted with water, and Lycium barbarum polysaccharide is obtained by membrane filtration of the water extract; the residue after water extraction is continuously extracted with ethanol to obtain a crude extract of alkaloids, and the crude extract is continuously purified by a macroporous resin separation column to obtain Lycium barbarum alkaloids. In this way, three types of active ingredients in Lycium barbarum can be extracted and purified at the same time, which is convenient to operate, simple, safe, environmentally friendly, and realizes the high-value comprehensive utilization and industrial production of Lycium barbarum resources. Attached Figure Description

[0010] Figure 1 This is a flowchart illustrating a preferred embodiment of a method for the comprehensive extraction of active ingredients from wolfberry in industrial applications. Detailed Implementation

[0011] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below in conjunction with specific embodiments and corresponding drawings. Obviously, the described embodiments are only a part of the embodiments of this invention, and not all of them. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this invention.

[0012] like Figure 1 As shown, the present invention provides a comprehensive extraction method for the active ingredients of wolfberry used in industrial trials, comprising the following steps:

[0013] Dried wolfberries were pulverized to 100-150 mesh using an air-cooled pulverizer and then extracted in a subcritical extraction vessel to obtain wolfberry carotenoids and oils.

[0014] The residue after subcritical extraction was further extracted with water, and the aqueous extract was filtered through a membrane to obtain wolfberry polysaccharide.

[0015] The residue after water extraction was further extracted with ethanol to obtain a crude extract of alkaloids. The crude extract was then purified using a macroporous resin column to obtain wolfberry alkaloids.

[0016] The specific steps of "pulverizing dried goji berries to 100-150 mesh using an air-cooled pulverizer and then extracting them into a subcritical extraction vessel to obtain goji berry carotenoids and oils" are as follows: pulverizing dried goji berries to 100-150 mesh using an air-cooled pulverizer, loading the goji berry powder into the extraction vessel, closing the feeder, and extracting most of the air from the extractor.

[0017] Inject liquefied butane, set the temperature to 50~60℃, the pressure to 0.4~0.5 MPa, the feed-to-liquid ratio to 1:2~1:3, and the extraction time to 1~2 h;

[0018] After extraction, the valve is opened to pressurize the extract from the extraction tank to the separation tank. The wolfberry residue in the extraction tank and the extract in the separation tank are desolvated and vaporized to complete the desolvation process.

[0019] After desolventizing, the wolfberry residue can be removed from the extractor, and wolfberry carotenoids and unsaturated oils can be released from the separation tank.

[0020] The step of "continuing to extract the residue after subcritical extraction with water, and filtering the water extract with a membrane to obtain wolfberry polysaccharide" is specifically as follows: the first wolfberry residue after subcritical extraction is put into an extraction tank, water is injected at a solid-liquid ratio of 1:10-1:20, and stirring extraction is carried out at 50-60°C for 1-2 hours to obtain a wolfberry residue mixture;

[0021] The wolfberry residue mixture is filtered in sequence through a flat plate centrifuge and a high-speed tubular centrifuge, and then filtered through a filter membrane with a molecular weight of 1000-5000 Da to obtain a wolfberry polysaccharide solution.

[0022] After the wolfberry polysaccharide solution is concentrated at 50-60°C under reduced pressure, spray drying is directly carried out without any excipients to obtain a wolfberry polysaccharide powder. The spray drying conditions are as follows: inlet air temperature 150-170°C, outlet air temperature 100°C, air sweeping temperature 42°C, and dehumidified inlet air temperature 32°C.

[0023] Further, the comprehensive extraction method of wolfberry functional components in industrial pilot production also includes a preparation step of wolfberry beverage, specifically: the small molecule waste liquid filtered in the step of "continuing to extract the residue after subcritical extraction with water, and filtering the water extract with a membrane to obtain wolfberry polysaccharide" is added with 5-10% of wolfberry original pulp, 1-2% of sweetener, and 0.05-0.1% of sour agent, and then homogenized, canned, and sterilized to produce wolfberry beverage. The produced beverage has the unique aroma of fresh wolfberry and dried wolfberry, and has uniform texture and is not prone to stratification.

[0024] The step of "continuing to extract the residue after water extraction with ethanol to obtain a crude alkaloid extract, and purifying the crude extract with a macroporous resin column to obtain wolfberry alkaloids" is specifically as follows: the secondary wolfberry residue obtained by filtering the wolfberry residue mixture in sequence through a flat plate centrifuge and a high-speed tubular centrifuge is put into an extraction tank, 75% ethanol solution is injected at a solid-liquid ratio of 1:10-1:20, and stirring extraction is carried out at 50-60°C for 1-2 hours to obtain a secondary wolfberry residue mixture.

[0025] The secondary wolfberry residue mixture is filtered in sequence through a flat plate centrifuge and a high-speed tubular centrifuge to obtain an extract, which is concentrated under reduced pressure at 50-60°C to obtain a wolfberry alkaloid crude extract concentrate. The remaining wolfberry residue can be used as feed or fertilizer.

[0026] Further, the comprehensive extraction method of the functional components of wolfberry for industrial pilot test further comprises a wolfberry alkaloid purification step, specifically: injecting the concentrated wolfberry alkaloid crude extract into a macroporous resin separation column, performing gradient elution with ethanol with a concentration of 0% to 95%, 2 to 3 BV for each gradient elution, collecting the eluate, reducing and concentrating the eluate, and freeze-drying to obtain wolfberry alkaloids. The macroporous resin is D101 or AB-8 type, the diameter-height ratio of the macroporous resin separation column is 1:10 to 1:13, the loading flow rate is 0.5 to 1 BV / h, and the elution flow rate is 1 to 2 BV / h.

[0027] The comprehensive extraction method of the functional components of wolfberry for industrial pilot test has the following effects:

[0028] (1) The present application comprehensively considers the extraction yield of three types of active components in wolfberry, the content of effective components, and the cost of production process, and obtains an extraction and purification process with better indicators. The polysaccharide yield is 8.9%, of which the wolfberry polysaccharide content is 58%; the yield of wolfberry carotenoids and oil is 4.1%, of which the total carotenoid content is 3.3%; the total alkaloid yield is 0.7%; the yield of each part is much higher than that of the prior art.

[0029] (2) The present application can simultaneously extract and purify three types of active components in wolfberry, has high extraction efficiency, low total energy consumption, convenient operation, simple, safe, and environmentally friendly process, realizes high-value comprehensive utilization of wolfberry resources, and is easy to realize industrialized production.

[0030] (3) The present application fully utilizes the small molecule sugar extract liquid, which is usually treated as waste during the extraction of wolfberry polysaccharide, to obtain wolfberry beverage, reduces environmental pollution, and improves the utilization rate of wolfberry fruit resources.

Claims

1. A comprehensive extraction method of functional components of Lycium barbarum in industrial pilot, characterized in that, It comprises the following steps: The dry fruit of wolfberry is crushed to 100-150 mesh by a wind-cooled pulverizer, and is first put into a subcritical extraction kettle to extract wolfberry carotenoids and oil; the subcritical extraction kettle extraction comprises injecting liquefied butane, setting the temperature to 50-60℃, the pressure to 0.4-0.5 Mpa, the solid-liquid ratio to 1:2-1:3, and the extraction time to 1-2 h; The residue after subcritical extraction is continuously extracted with water, and the water extract is filtered by a membrane to obtain wolfberry polysaccharide; the extraction comprises injecting water at a solid-liquid ratio of 1:10-1:20, and stirring extraction at 50-60℃ for 1-2 h; The residue after water extraction is continuously extracted with ethanol to obtain a crude extract of alkaloids, and the crude extract is further purified by a macroporous resin separation column to obtain wolfberry alkaloids; the ethanol extraction comprises injecting 75% ethanol solution at a solid-liquid ratio of 1:10-1:20, stirring extraction at 50-60℃ for 1-2 h, and obtaining a secondary wolfberry residue mixture; the secondary wolfberry residue mixture is filtered to obtain an extract, and the extract is concentrated under reduced pressure at 50-60℃ to obtain a wolfberry alkaloid crude extract concentrate.

2. The comprehensive extraction method of the functional components of Lycium barbarum in industrial pilot according to claim 1, characterized in that: The step of "the dry fruit of wolfberry is crushed to 100-150 mesh by a wind-cooled pulverizer, and is first put into a subcritical extraction kettle to extract wolfberry carotenoids and oil" specifically comprises: the dry fruit of wolfberry is crushed to 100-150 mesh by a wind-cooled pulverizer, the wolfberry powder is loaded into the extraction kettle, the feeder is closed, and most of the air in the extraction kettle is pumped out; liquefied butane is injected, the temperature is set to 50-60℃, the pressure is set to 0.4-0.5 Mpa, the solid-liquid ratio is set to 1:2-1:3, and the extraction time is set to 1-2 h; after the extraction is completed, the valve is opened to press the extract from the extraction kettle to the separation tank, and the wolfberry residue in the extraction kettle and the extract in the separation tank are subjected to a desolventization process by reduced pressure vaporization; after desolventization, the wolfberry residue is taken out of the extraction kettle, and wolfberry carotenoids and oil are discharged from the separation tank.

3. The comprehensive extraction method of the functional components of Lycium barbarum in industrial pilot according to claim 1, characterized in that: The step of "the residue after subcritical extraction is continuously extracted with water, and the water extract is filtered by a membrane to obtain wolfberry polysaccharide" specifically comprises: the first wolfberry residue after subcritical extraction is put into an extraction tank, water is injected at a solid-liquid ratio of 1:10-1:20, stirring extraction is carried out at 50-60℃ for 1-2 h, and a wolfberry residue mixture is obtained; the wolfberry residue mixture is sequentially filtered by a flat plate centrifuge and a high-speed tubular centrifuge, and then filtered by a filter membrane with a molecular weight of 1000 Da-5000 Da to obtain a wolfberry polysaccharide solution; the wolfberry polysaccharide solution is concentrated under reduced pressure at 50-60℃, and then directly subjected to spray drying without any auxiliary materials to obtain wolfberry polysaccharide powder; the spray drying conditions are: inlet air temperature 150-170℃, outlet air temperature 100℃, air sweeping temperature 42℃, and dehumidification inlet air temperature 32℃.

4. The comprehensive extraction method of the functional components of Lycium barbarum in industrial pilot according to claim 3, characterized in that: It also comprises a preparation step of wolfberry beverage, specifically: the small molecule waste liquid filtered by a membrane in the step of "the residue after subcritical extraction is continuously extracted with water, and the water extract is filtered by a membrane to obtain wolfberry polysaccharide" is added with 5-10% wolfberry original pulp, 1-2% sweetener, and 0.05-0.1% acidifier, and then subjected to homogenization, canning, and sterilization to prepare wolfberry beverage.

5. The comprehensive extraction method of the functional components of Lycium barbarum in industrial pilot according to claim 3, characterized in that: The residue after water extraction is continuously extracted with ethanol to obtain a crude extract of alkaloids, and the crude extract is continuously purified with a macroporous resin separation column to obtain the wolfberry alkaloids. The step is specifically as follows: the secondary wolfberry residue obtained after the secondary wolfberry residue is filtered with a flat plate centrifuge and a high-speed tube centrifuge in sequence is poured into an extraction tank, 75% ethanol solution is injected into the extraction tank at a solid-liquid ratio of 1:10-1:20, and the mixture is stirred and extracted at 50-60 ℃ for 1-2 h to obtain a secondary wolfberry residue mixture; The secondary wolfberry residue mixture is filtered with a flat plate centrifuge and a high-speed tube centrifuge in sequence to obtain an extract, and the extract is concentrated under reduced pressure at 50-60 ℃ to obtain a wolfberry alkaloid crude extract concentrate.

6. The comprehensive extraction method of the functional components of Lycium barbarum in industrial pilot according to claim 5, characterized in that: The wolfberry alkaloid purification step further includes the following steps: the wolfberry alkaloid crude extract concentrate is injected into a macroporous resin separation column, ethanol with a concentration of 0%-95% is used for gradient elution, each gradient elution is performed for 2-3 BV, eluate is collected respectively, the eluate is concentrated under reduced pressure, and freeze-drying is performed to obtain wolfberry alkaloids.

7. The comprehensive extraction method of the functional components of Lycium barbarum in industrial pilot according to claim 6, characterized in that: The macroporous resin is D101 or AB-8, and the diameter-height ratio of the macroporous resin separation column is 1:10-1:13, the loading flow rate is 0.5-1 BV / h, and the elution flow rate is 1-2 BV / h.

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