CN104059163A - Novel method for preparing Qinghai Qaidam lycium barbarum polysaccharide in extraction and separation manner - Google Patents
Novel method for preparing Qinghai Qaidam lycium barbarum polysaccharide in extraction and separation manner Download PDFInfo
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Abstract
The invention relates to a novel method for preparing a Qinghai Qaidam lycium barbarum polysaccharide in an extraction and separation manner. The method comprises the following steps: (1) washing fresh Qinghai Qaidam lycium barbarum fruits taken as raw materials with pure water for multiple times and then removing impurities so as to obtain treated lycium barbarum; (2) soaking the treated lycium barbarum in the pure water at a normal temperature and carrying out smashing so as to obtain the smashed lycium barbarum; (3) carrying out ultrasonic extraction by adding the pure water into the smashed lycium barbarum so as to obtain an extraction liquid; (4) filtering the extraction liquid with a filter cloth so as to respectively obtain a filtrate and filter residues; (5) centrifuging the filtrate so as to respectively obtain a supernate and residues; (6) feeding the supernate to pass through a nonpolar macroporous resin and then cleaning a resin column with the pure water so as to obtain a polysaccharide eluent; (7) removing granular impurities from the polysaccharide eluent via a ceramic membrane so as to obtain a transparent liquid; (8) intercepting the transparent liquid with an organic ultrafiltration membrane so as to obtain an intercepting liquid, carrying out freeze drying on the intercepting liquid to reach a constant weight so as to obtain a brown yellow Qaidam lycium barbarum polysaccharide powder product. The method is simple, convenient, rapid and low in cost.
Description
Technical field
The present invention relates to a kind of preparation method of lycium barbarum polysaccharide, relate in particular to Qaidam, Qinghai lycium barbarum polysaccharide and extract separated novel preparation method.
Background technology
Qaidam matrimony vine, mainly produces the Caidamu Basin on Qinghai-Tibet Platean.The unique geography and climate in Qinghai-Tibet Platean has been brought up the good quality of Qaidam matrimony vine, has the advantages that particle is large, look red, meat is thick, sugar degree is high, taste is sweet, is pure natural, free of contamination senior tonic.Modern scientific research proves: matrimony vine has and regulates immunologic function, hypoglycemic, reducing blood-fat, the effect such as anti-ageing, antitumor, and its pharmacological action and its bioactive ingredients lycium barbarum polysaccharide LBP are closely related.Therefore, using it as functional factor, develop Medicines and Health Product and there is vast potential for future development.
The separated main water extraction and alcohol precipitation method that adopts of extraction of traditional lycium barbarum polysaccharide,, there is the shortcomings such as consuming time, yield is low, purity is low, product colour is dark in the leaching process of the long-time high heat of many tools.Supersound extraction is to utilize hyperacoustic cavitation effect, mechanical effect and heat effect, can effectively increase extraction yield, shorten extraction time, and leaching process does not need high temperature, can not change structure and the biological activity of extracting composition.Membrane separation process is, according to microbial film, the penetrating principle of matter selective is carried out to separated method, owing to having separation, concentrated, purifying and refining function concurrently, have again efficient, energy-saving and environmental protection, molecular level filters and filtration procedure is simple, be easy to the features such as control, the fields such as food, medicine, biology, environmental protection, chemical industry, metallurgy, the energy, oil, water treatment have been widely used in, produce huge economic benefit and social benefit, become one of most important means in current separation science.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of Qaidam, Qinghai lycium barbarum polysaccharide easy, quick, with low cost and extracts separated novel preparation method.
For addressing the above problem, Qaidam, Qinghai of the present invention lycium barbarum polysaccharide extracts separated novel preparation method, comprises the following steps:
(1) Qaidam, the Qinghai medlar fresh fruit of take is raw material, adopts pure water washing repeatedly to remove afterwards impurity, the matrimony vine after being processed;
By the matrimony vine after described processing in the ratio soak at room temperature of 1g:3 ~ 5mL in pure water, after 8 ~ 12h, the matrimony vine after soaking is injected to pulverizer together with soak solution and carries out fragmentation, obtain broken matrimony vine;
(3) in the matrimony vine of described fragmentation, in the ratio of 1g:10 ~ 20mL, add pure water, in temperature, be that 20 ~ 40 ℃, ultrasonic power are that 600 ~ 1000 W, mixing speed are to carry out circulating supersound extraction under the condition of 600 ~ 1000 rpm, extraction time is 2 times, each extraction time is 40 ~ 60 min, merges and obtains extracting solution;
(4) 200 order filter-cloth filterings for described extracting solution, obtain respectively filtrate and filter residue;
(5) described filtrate, after tubular-bowl centrifuge is centrifugal, obtains respectively supernatant liquor and residue;
(6) described supernatant liquor is crossed non-polar macroporous resin D900 with the flow velocity of 100 ~ 300 mL/min, and iterative cycles, until elutriant does not change at the light absorption value of 450 nm; Then use the pure water of 3 ~ 5 times of column volumes to clean resin column, to replace the polysaccharide extraction liquid in resin column, obtain polysaccharide elutriant;
(7) the ceramic membrane that is 50 ~ 200 nm by described polysaccharide elutriant via hole diameter is removed particulate contamination, obtains seeing through liquid;
(8) the described first ultrafiltration organic membrane that is 100000 through molecular weight cut-off of liquid that sees through is held back, the ultrafiltration organic membrane that is 1000 ~ 10000 through molecular weight cut-off is again held back, when per-meate side no longer includes while flowing out through liquid, add 50 ~ 200 L pure water circulation is continued, obtain trapped fluid; This trapped fluid to constant weight, obtains the pulverous Qaidam of brown color lycium barbarum polysaccharide product through lyophilize.
The described step (7) condition of middle ceramic membrane removal of impurities refers to that pressure is that 0.5 ~ 3 MPa, flow velocity are 100 ~ 500 mL/min.
The described step (8) condition of middle ultrafiltration organic membrane refers to that pressure is that 5 ~ 20 Kg, flow velocity are 50 ~ 300 mL/min.
Described step (8) in cryodesiccated condition refer to that sample pre-freeze temperature is that-30 ~-50 ℃, sample temperature of heating plate are that 0 ~ 30 ℃, condenser temperature are that-50 ~-78 ℃, vacuum tightness are 0.1 ~ 100 Pa.
The present invention compared with prior art has the following advantages:
1, the present invention adopts supersound extraction Qaidam lycium barbarum polysaccharide, and extraction efficiency is high, and leaching process do not need high temperature, can effectively avoid high temperature to lycium barbarum polysaccharide structure and bioactive destruction.
2. the present invention adopts D900 macroporous resin to carry out the decolouring of polysaccharide extraction liquid, and cost is low, efficiency is high, is easy to realize industrialization.
3. the present invention adopts ceramic membrane and the organic membrane-bound membrane separation technique of ultrafiltration, have that technical process is short, simple to operate, efficiency is high, low power consumption and other advantages, effectively reduced production cost, while resulting Qaidam lycium barbarum polysaccharide product property stable homogeneous, purity high (60% ~ 78%), there is certain anti-oxidant activity, can develop the Medicines and Health Product with antioxygenation.
4. the present invention adopts the Freeze Drying Technique of carrying out under low temperature, low pressure, can effectively avoid the impact of high temperature on quality product in conventional drying technology.
Embodiment
embodiment 1qaidam, Qinghai lycium barbarum polysaccharide extracts separated novel preparation method, comprises the following steps:
(1) 10 Qaidam, the Kg Qinghai medlar fresh fruits of take are raw material, adopt pure water washing repeatedly to remove afterwards impurity, the matrimony vine after being processed.
By the matrimony vine after processing in the ratio soak at room temperature of 1g:3mL in pure water, after 8h, the matrimony vine after immersion is injected to pulverizer together with soak solution and carries out fragmentation, obtain broken matrimony vine.
(3) in broken matrimony vine, in the ratio of 1g:10mL, add pure water, in temperature, be that 20 ℃, ultrasonic power are that 600 W, mixing speed are to carry out circulating supersound extraction under the condition of 600 rpm, extraction time is 2 times, and each extraction time is 40 min, merges and obtains extracting solution.
(4) 200 order filter-cloth filterings for extracting solution, obtain respectively filtrate and filter residue.
(5) filtrate, after tubular-bowl centrifuge is centrifugal with the rotating speed of 20000 rpm, obtains respectively supernatant liquor and residue.
(6) supernatant liquor is crossed non-polar macroporous resin D900 with the flow velocity of 100 mL/min, and iterative cycles, until elutriant does not change at the light absorption value of 450 nm; Then with the pure water of 3 times of column volumes, clean resin column, to replace the polysaccharide extraction liquid in resin column, obtain polysaccharide elutriant.
(7) by polysaccharide elutriant via hole diameter, being the ceramic membrane of 50 nm, is that 0.5 MPa, flow velocity are to remove particulate contamination under the condition of 100 mL/min at pressure, obtains seeing through liquid.
(8) by seeing through liquid, at pressure, be that 5 Kg, flow velocity are under the condition of 50 mL/min, the ultrafiltration organic membrane that is first 100000 through molecular weight cut-off is held back, the ultrafiltration organic membrane that is 1000 through molecular weight cut-off is again held back, when per-meate side no longer includes while flowing out through liquid, add 50 L pure water circulation is continued, obtain trapped fluid; This trapped fluid pre-freeze, sample temperature of heating plate at-30 ℃ be 0 ℃, condenser temperature for-50 ℃, vacuum tightness be under the condition of 0.1 Pa through lyophilize to constant weight, obtain the 1.10 pulverous Qaidam of Kg brown color lycium barbarum polysaccharide products.
After tested, the polysaccharide content of this Qaidam lycium barbarum polysaccharide product is 62%, to the clearance rate of DPPH, can reach 62%, and in the reaction of β-carotene-linoleic acid system, inhibiting rate can reach 66%, presents good anti-oxidant activity.
embodiment 2qaidam, Qinghai lycium barbarum polysaccharide extracts separated novel preparation method, comprises the following steps:
(1) 10 Qaidam, the Kg Qinghai medlar fresh fruits of take are raw material, adopt pure water washing repeatedly to remove afterwards impurity, the matrimony vine after being processed.
By the matrimony vine after processing in the ratio soak at room temperature of 1g:4mL in pure water, after 10h, the matrimony vine after immersion is injected to pulverizer together with soak solution and carries out fragmentation, obtain broken matrimony vine.
(3) in broken matrimony vine, in the ratio of 1g:10mL, add pure water, in temperature, be that 30 ℃, ultrasonic power are that 800 W, mixing speed are to carry out circulating supersound extraction under the condition of 700 rpm, extraction time is 2 times, and each extraction time is 50 min, merges and obtains extracting solution.
(4) 200 order filter-cloth filterings for extracting solution, obtain respectively filtrate and filter residue.
(5) filtrate, after tubular-bowl centrifuge is centrifugal with the rotating speed of 20000 rpm, obtains respectively supernatant liquor and residue.
(6) supernatant liquor is crossed non-polar macroporous resin D900 with the flow velocity of 100 mL/min, and iterative cycles, until elutriant does not change at the light absorption value of 450 nm; Then with the pure water of 5 times of column volumes, clean resin column, to replace the polysaccharide extraction liquid in resin column, obtain polysaccharide elutriant.
(7) by polysaccharide elutriant via hole diameter, being the ceramic membrane of 200 nm, is that 3 MPa, flow velocity are to remove particulate contamination under the condition of 500 mL/min at pressure, obtains seeing through liquid.
(8) by seeing through liquid, at pressure, be that 5 Kg, flow velocity are under the condition of 50 mL/min, the ultrafiltration organic membrane that is first 100000 through molecular weight cut-off is held back, the ultrafiltration organic membrane that is 1000 through molecular weight cut-off is again held back, when per-meate side no longer includes while flowing out through liquid, add 50 L pure water circulation is continued, obtain trapped fluid; This trapped fluid pre-freeze, sample temperature of heating plate at-40 ℃ be 10 ℃, condenser temperature for-60 ℃, vacuum tightness be under the condition of 10 Pa through lyophilize to constant weight, obtain the 1.14 pulverous Qaidam of Kg brown color lycium barbarum polysaccharide products.
After tested, the polysaccharide content of this Qaidam lycium barbarum polysaccharide product is 60%, to the clearance rate of DPPH, can reach 60%, and in the reaction of β-carotene-linoleic acid system, inhibiting rate can reach 65%, presents good anti-oxidant activity.
embodiment 3qaidam, Qinghai lycium barbarum polysaccharide extracts separated novel preparation method, comprises the following steps:
(1) 10 Qaidam, the Kg Qinghai medlar fresh fruits of take are raw material, adopt pure water washing repeatedly to remove afterwards impurity, the matrimony vine after being processed.
By the matrimony vine after processing in the ratio soak at room temperature of 1g:4mL in pure water, after 10h, the matrimony vine after immersion is injected to pulverizer together with soak solution and carries out fragmentation, obtain broken matrimony vine.
(3) in broken matrimony vine, in the ratio of 1g:10mL, add pure water, in temperature, be that 30 ℃, ultrasonic power are that 800 W, mixing speed are to carry out circulating supersound extraction under the condition of 800 rpm, extraction time is 2 times, and each extraction time is 50 min, merges and obtains extracting solution.
(4) 200 order filter-cloth filterings for extracting solution, obtain respectively filtrate and filter residue.
(5) filtrate, after tubular-bowl centrifuge is centrifugal with the rotating speed of 20000 rpm, obtains respectively supernatant liquor and residue.
(6) supernatant liquor is crossed non-polar macroporous resin D900 with the flow velocity of 200 mL/min, and iterative cycles, until elutriant does not change at the light absorption value of 450 nm; Then with the pure water of 4 times of column volumes, clean resin column, to replace the polysaccharide extraction liquid in resin column, obtain polysaccharide elutriant.
(7) by polysaccharide elutriant via hole diameter, being the ceramic membrane of 100 nm, is that 2 MPa, flow velocity are to remove particulate contamination under the condition of 350 mL/min at pressure, obtains seeing through liquid.
(8) by seeing through liquid, at pressure, be that 10 Kg, flow velocity are under the condition of 150 mL/min, the ultrafiltration organic membrane that is first 100000 through molecular weight cut-off is held back, the ultrafiltration organic membrane that is 1000 through molecular weight cut-off is again held back, when per-meate side no longer includes while flowing out through liquid, add 100 L pure water circulation is continued, obtain trapped fluid; This trapped fluid pre-freeze, sample temperature of heating plate at-35 ℃ be 20 ℃, condenser temperature for-70 ℃, vacuum tightness be under the condition of 40 Pa through lyophilize to constant weight, obtain the 1.08 pulverous Qaidam of Kg brown color lycium barbarum polysaccharide products.
After tested, the polysaccharide content of this Qaidam lycium barbarum polysaccharide product is 64%, to the clearance rate of DPPH, can reach 63%, and in the reaction of β-carotene-linoleic acid system, inhibiting rate can reach 69%, presents good anti-oxidant activity.
embodiment 4qaidam, Qinghai lycium barbarum polysaccharide extracts separated novel preparation method, comprises the following steps:
(1) 5 Qaidam, the Kg Qinghai medlar fresh fruits of take are raw material, adopt pure water washing repeatedly to remove afterwards impurity, the matrimony vine after being processed.
By the matrimony vine after processing in the ratio soak at room temperature of 1g:5mL in pure water, after 12h, the matrimony vine after immersion is injected to pulverizer together with soak solution and carries out fragmentation, obtain broken matrimony vine.
(3) in broken matrimony vine, in the ratio of 1g:20mL, add pure water, in temperature, be that 40 ℃, ultrasonic power are that 1000 W, mixing speed are to carry out circulating supersound extraction under the condition of 1000 rpm, extraction time is 2 times, and each extraction time is 60 min, merges and obtains extracting solution.
(4) 200 order filter-cloth filterings for extracting solution, obtain respectively filtrate and filter residue.
(5) filtrate, after tubular-bowl centrifuge is centrifugal with the rotating speed of 20000 rpm, obtains respectively supernatant liquor and residue.
(6) supernatant liquor is crossed non-polar macroporous resin D900 with the flow velocity of 300 mL/min, and iterative cycles, until elutriant does not change at the light absorption value of 450 nm; Then with the pure water of 5 times of column volumes, clean resin column, to replace the polysaccharide extraction liquid in resin column, obtain polysaccharide elutriant.
(7) by polysaccharide elutriant via hole diameter, being the ceramic membrane of 200 nm, is that 3 MPa, flow velocity are to remove particulate contamination under the condition of 500 mL/min at pressure, obtains seeing through liquid.
(8) by seeing through liquid, at pressure, be that 20 Kg, flow velocity are under the condition of 300 mL/min, the ultrafiltration organic membrane that is first 100000 through molecular weight cut-off is held back, the ultrafiltration organic membrane that is 10000 through molecular weight cut-off is again held back, when per-meate side no longer includes while flowing out through liquid, add 200 L pure water circulation is continued, obtain trapped fluid; This trapped fluid pre-freeze, sample temperature of heating plate at-50 ℃ be 30 ℃, condenser temperature for-78 ℃, vacuum tightness be under the condition of 100 Pa through lyophilize to constant weight, obtain the 0.092 pulverous Qaidam of Kg brown color lycium barbarum polysaccharide product.
After tested, the polysaccharide content of this Qaidam lycium barbarum polysaccharide product is 76%, to the clearance rate of DPPH, can reach 72%, and in the reaction of β-carotene-linoleic acid system, inhibiting rate can reach 77%, presents good anti-oxidant activity.
embodiment 5qaidam, Qinghai lycium barbarum polysaccharide extracts separated novel preparation method, comprises the following steps:
(1) 5 Qaidam, the Kg Qinghai medlar fresh fruits of take are raw material, adopt pure water washing repeatedly to remove afterwards impurity, the matrimony vine after being processed.
By the matrimony vine after processing in the ratio soak at room temperature of 1g:5mL in pure water, after 9h, the matrimony vine after immersion is injected to pulverizer together with soak solution and carries out fragmentation, obtain broken matrimony vine.
(3) in broken matrimony vine, in the ratio of 1g:20mL, add pure water, in temperature, be that 30 ℃, ultrasonic power are that 800 W, mixing speed are to carry out circulating supersound extraction under the condition of 900 rpm, extraction time is 2 times, and each extraction time is 50 min, merges and obtains extracting solution.
(4) 200 order filter-cloth filterings for extracting solution, obtain respectively filtrate and filter residue.
(5) filtrate, after tubular-bowl centrifuge is centrifugal with the rotating speed of 20000 rpm, obtains respectively supernatant liquor and residue.
(6) supernatant liquor is crossed non-polar macroporous resin D900 with the flow velocity of 300 mL/min, and iterative cycles, until elutriant does not change at the light absorption value of 450 nm; Then with the pure water of 3 times of column volumes, clean resin column, to replace the polysaccharide extraction liquid in resin column, obtain polysaccharide elutriant.
(7) by polysaccharide elutriant via hole diameter, being the ceramic membrane of 50 nm, is that 0.5 MPa, flow velocity are to remove particulate contamination under the condition of 100 mL/min at pressure, obtains seeing through liquid.
(8) by seeing through liquid, at pressure, be that 20 Kg, flow velocity are under the condition of 300 mL/min, the ultrafiltration organic membrane that is first 100000 through molecular weight cut-off is held back, the ultrafiltration organic membrane that is 10000 through molecular weight cut-off is again held back, when per-meate side no longer includes while flowing out through liquid, add 200 L pure water circulation is continued, obtain trapped fluid; This trapped fluid pre-freeze, sample temperature of heating plate at-45 ℃ be 15 ℃, condenser temperature for-65 ℃, vacuum tightness be under the condition of 70 Pa through lyophilize to constant weight, obtain the pulverous Qaidam of .085 Kg brown color lycium barbarum polysaccharide product.
After tested, the polysaccharide content of this Qaidam lycium barbarum polysaccharide product is 78%, to the clearance rate of DPPH, can reach 75%, and in the reaction of β-carotene-linoleic acid system, inhibiting rate can reach 80%, presents good anti-oxidant activity.
embodiment 6qaidam, Qinghai lycium barbarum polysaccharide extracts separated novel preparation method, comprises the following steps:
(1) 5 Qaidam, the Kg Qinghai medlar fresh fruits of take are raw material, adopt pure water washing repeatedly to remove afterwards impurity, the matrimony vine after being processed.
By the matrimony vine after processing in the ratio soak at room temperature of 1g:4mL in pure water, after 11h, the matrimony vine after immersion is injected to pulverizer together with soak solution and carries out fragmentation, obtain broken matrimony vine.
(3) in broken matrimony vine, in the ratio of 1g:20mL, add pure water, in temperature, be that 30 ℃, ultrasonic power are that 800 W, mixing speed are to carry out circulating supersound extraction under the condition of 800 rpm, extraction time is 2 times, and each extraction time is 50 min, merges and obtains extracting solution.
(4) 200 order filter-cloth filterings for extracting solution, obtain respectively filtrate and filter residue.
(5) filtrate, after tubular-bowl centrifuge is centrifugal with the rotating speed of 20000 rpm, obtains respectively supernatant liquor and residue.
(6) supernatant liquor is crossed non-polar macroporous resin D900 with the flow velocity of 200 mL/min, and iterative cycles, until elutriant does not change at the light absorption value of 450 nm; Then with the pure water of 4 times of column volumes, clean resin column, to replace the polysaccharide extraction liquid in resin column, obtain polysaccharide elutriant.
(7) by polysaccharide elutriant via hole diameter, being the ceramic membrane of 100 nm, is that 2 MPa, flow velocity are to remove particulate contamination under the condition of 350 mL/min at pressure, obtains seeing through liquid.
(8) by seeing through liquid, at pressure, be that 10 Kg, flow velocity are under the condition of 250 mL/min, the ultrafiltration organic membrane that is first 100000 through molecular weight cut-off is held back, the ultrafiltration organic membrane that is 10000 through molecular weight cut-off is again held back, when per-meate side no longer includes while flowing out through liquid, add 100 L pure water circulation is continued, obtain trapped fluid; This trapped fluid pre-freeze, sample temperature of heating plate at-40 ℃ be 25 ℃, condenser temperature for-75 ℃, vacuum tightness be under the condition of 80 Pa through lyophilize to constant weight, obtain the 0.09 pulverous Qaidam of Kg brown color lycium barbarum polysaccharide product.
After tested, the polysaccharide content of this Qaidam lycium barbarum polysaccharide product is 75%, to the clearance rate of DPPH, can reach 71%, and in the reaction of β-carotene-linoleic acid system, inhibiting rate can reach 75%, presents good anti-oxidant activity.
embodiment 7qaidam, Qinghai lycium barbarum polysaccharide extracts separated novel preparation method, comprises the following steps:
(1) 7 Qaidam, the Kg Qinghai medlar fresh fruits of take are raw material, adopt pure water washing repeatedly to remove afterwards impurity, the matrimony vine after being processed.
By the matrimony vine after processing in the ratio soak at room temperature of 1g:4mL in pure water, after 11h, the matrimony vine after immersion is injected to pulverizer together with soak solution and carries out fragmentation, obtain broken matrimony vine.
(3) in broken matrimony vine, in the ratio of 1g:15mL, add pure water, in temperature, be that 30 ℃, ultrasonic power are that 800 W, mixing speed are to carry out circulating supersound extraction under the condition of 900 rpm, extraction time is 2 times, and each extraction time is 50 min, merges and obtains extracting solution.
(4) 200 order filter-cloth filterings for extracting solution, obtain respectively filtrate and filter residue.
(5) filtrate, after tubular-bowl centrifuge is centrifugal with the rotating speed of 20000 rpm, obtains respectively supernatant liquor and residue.
(6) supernatant liquor is crossed non-polar macroporous resin D900 with the flow velocity of 100mL/min, and iterative cycles, until elutriant does not change at the light absorption value of 450 nm; Then with the pure water of 5 times of column volumes, clean resin column, to replace the polysaccharide extraction liquid in resin column, obtain polysaccharide elutriant.
(7) by polysaccharide elutriant via hole diameter, being the ceramic membrane of 50 nm, is that 3 MPa, flow velocity are to remove particulate contamination under the condition of 400 mL/min at pressure, obtains seeing through liquid.
(8) by seeing through liquid, at pressure, be that 20 Kg, flow velocity are under the condition of 250 mL/min, the ultrafiltration organic membrane that is first 100000 through molecular weight cut-off is held back, the ultrafiltration organic membrane that is 5000 through molecular weight cut-off is again held back, when per-meate side no longer includes while flowing out through liquid, add 200 L pure water circulation is continued, obtain trapped fluid; This trapped fluid pre-freeze, sample temperature of heating plate at-35 ℃ be 25 ℃, condenser temperature under-55 ℃, the vacuum tightness condition that is 30Pa through lyophilize to constant weight, obtain the 0.18 pulverous Qaidam of Kg brown color lycium barbarum polysaccharide product.
After tested, the polysaccharide content of this Qaidam lycium barbarum polysaccharide product is 70%, to the clearance rate of DPPH, can reach 66%, and in the reaction of β-carotene-linoleic acid system, inhibiting rate can reach 72%, presents good anti-oxidant activity.
embodiment 8qaidam, Qinghai lycium barbarum polysaccharide extracts separated novel preparation method, comprises the following steps:
(1) 7 Qaidam, the Kg Qinghai medlar fresh fruits of take are raw material, adopt pure water washing repeatedly to remove afterwards impurity, the matrimony vine after being processed.
By the matrimony vine after processing in the ratio soak at room temperature of 1g:4mL in pure water, after 11h, the matrimony vine after immersion is injected to pulverizer together with soak solution and carries out fragmentation, obtain broken matrimony vine.
(3) in broken matrimony vine, in the ratio of 1g:15mL, add pure water, in temperature, be that 30 ℃, ultrasonic power are that 800 W, mixing speed are to carry out circulating supersound extraction under the condition of 700 rpm, extraction time is 2 times, and each extraction time is 50 min, merges and obtains extracting solution.
(4) 200 order filter-cloth filterings for extracting solution, obtain respectively filtrate and filter residue.
(5) filtrate, after tubular-bowl centrifuge is centrifugal with the rotating speed of 20000 rpm, obtains respectively supernatant liquor and residue.
(6) supernatant liquor is crossed non-polar macroporous resin D900 with the flow velocity of 200 mL/min, and iterative cycles, until elutriant does not change at the light absorption value of 450 nm; Then with the pure water of 4 times of column volumes, clean resin column, to replace the polysaccharide extraction liquid in resin column, obtain polysaccharide elutriant.
(7) by polysaccharide elutriant via hole diameter, being the ceramic membrane of 100 nm, is that 2 MPa, flow velocity are to remove particulate contamination under the condition of 350 mL/min at pressure, obtains seeing through liquid.
(8) by seeing through liquid, at pressure, be that 10 Kg, flow velocity are under the condition of 200 mL/min, the ultrafiltration organic membrane that is first 100000 through molecular weight cut-off is held back, the ultrafiltration organic membrane that is 5000 through molecular weight cut-off is again held back, when per-meate side no longer includes while flowing out through liquid, add 100 L pure water circulation is continued, obtain trapped fluid; This trapped fluid pre-freeze, sample temperature of heating plate at-50 ℃ be 15 ℃, condenser temperature for-65 ℃, vacuum tightness be under the condition of 60 Pa through lyophilize to constant weight, obtain the 0.2 pulverous Qaidam of Kg brown color lycium barbarum polysaccharide product.
After tested, the polysaccharide content of this Qaidam lycium barbarum polysaccharide product is 68%, to the clearance rate of DPPH, can reach 64%, and in the reaction of β-carotene-linoleic acid system, inhibiting rate can reach 69%, presents good anti-oxidant activity.
Above-mentioned
embodiment 1 ~ 8in, step (4) the filter residue of gained and step (5) the residue of gained can be used as supercritical CO
2or the raw material of subcritical fluid extraction β-carotene.
Claims (4)
1. Qaidam, Qinghai lycium barbarum polysaccharide extracts separated novel preparation method, comprises the following steps:
(1) Qaidam, the Qinghai medlar fresh fruit of take is raw material, adopts pure water washing repeatedly to remove afterwards impurity, the matrimony vine after being processed;
By the matrimony vine after described processing in the ratio soak at room temperature of 1g:3 ~ 5mL in pure water, after 8 ~ 12h, the matrimony vine after soaking is injected to pulverizer together with soak solution and carries out fragmentation, obtain broken matrimony vine;
(3) in the matrimony vine of described fragmentation, in the ratio of 1g:10 ~ 20mL, add pure water, in temperature, be that 20 ~ 40 ℃, ultrasonic power are that 600 ~ 1000 W, mixing speed are to carry out circulating supersound extraction under the condition of 600 ~ 1000 rpm, extraction time is 2 times, each extraction time is 40 ~ 60 min, merges and obtains extracting solution;
(4) 200 order filter-cloth filterings for described extracting solution, obtain respectively filtrate and filter residue;
(5) described filtrate, after tubular-bowl centrifuge is centrifugal, obtains respectively supernatant liquor and residue;
(6) described supernatant liquor is crossed non-polar macroporous resin D900 with the flow velocity of 100 ~ 300 mL/min, and iterative cycles, until elutriant does not change at the light absorption value of 450 nm; Then use the pure water of 3 ~ 5 times of column volumes to clean resin column, to replace the polysaccharide extraction liquid in resin column, obtain polysaccharide elutriant;
(7) the ceramic membrane that is 50 ~ 200 nm by described polysaccharide elutriant via hole diameter is removed particulate contamination, obtains seeing through liquid;
(8) the described first ultrafiltration organic membrane that is 100000 through molecular weight cut-off of liquid that sees through is held back, the ultrafiltration organic membrane that is 1000 ~ 10000 through molecular weight cut-off is again held back, when per-meate side no longer includes while flowing out through liquid, add 50 ~ 200 L pure water circulation is continued, obtain trapped fluid; This trapped fluid to constant weight, obtains the pulverous Qaidam of brown color lycium barbarum polysaccharide product through lyophilize.
2. Qaidam, Qinghai as claimed in claim 1 lycium barbarum polysaccharide extracts separated novel preparation method, it is characterized in that: the described step (7) condition of middle ceramic membrane removal of impurities refers to that pressure is that 0.5 ~ 3 MPa, flow velocity are 100 ~ 500 mL/min.
3. Qaidam, Qinghai as claimed in claim 1 lycium barbarum polysaccharide extracts separated novel preparation method, it is characterized in that: the described step (8) condition of middle ultrafiltration organic membrane refers to that pressure is that 5 ~ 20 Kg, flow velocity are 50 ~ 300 mL/min.
4. Qaidam, Qinghai as claimed in claim 1 lycium barbarum polysaccharide extracts separated novel preparation method, it is characterized in that: described step (8) in cryodesiccated condition refer to that sample pre-freeze temperature is that-30 ~-50 ℃, sample temperature of heating plate are that 0 ~ 30 ℃, condenser temperature are that-50 ~-78 ℃, vacuum tightness are 0.1 ~ 100 Pa.
Priority Applications (1)
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| CN105685989A (en) * | 2016-03-08 | 2016-06-22 | 东北农业大学 | Anti-fatigue oral solution containing lepista sordida as well as preparation method and application of anti-fatigue oral solution |
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| CN106008733A (en) * | 2016-06-20 | 2016-10-12 | 威海百合生物技术股份有限公司 | Lycium barbarum polysaccharide extraction method |
| CN108524668A (en) * | 2018-05-28 | 2018-09-14 | 中国科学院兰州化学物理研究所 | A kind of preparation method to wolfberry fruit extract of the drug induced hepatic injury with reparation and therapeutic effect |
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| CN104987427A (en) * | 2015-07-23 | 2015-10-21 | 中国科学院西北高原生物研究所 | Complex enzyme microwave extraction method for optimizing lycium ruthenicum polysaccharide by utilizing response surface method |
| CN105685989A (en) * | 2016-03-08 | 2016-06-22 | 东北农业大学 | Anti-fatigue oral solution containing lepista sordida as well as preparation method and application of anti-fatigue oral solution |
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| CN112457426A (en) * | 2020-12-10 | 2021-03-09 | 中国科学院兰州化学物理研究所 | Method for simultaneously extracting different lycium barbarum polysaccharide components |
| CN112457426B (en) * | 2020-12-10 | 2022-01-28 | 中国科学院兰州化学物理研究所 | Method for simultaneously extracting different lycium barbarum polysaccharide components |
| CN114376939A (en) * | 2021-12-27 | 2022-04-22 | 广州丸美生物科技有限公司 | Polysaccharide composition and preparation method and application thereof |
| CN114376939B (en) * | 2021-12-27 | 2023-08-25 | 广州丸美生物科技有限公司 | Polysaccharide composition and preparation method and application thereof |
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