CN101974169B - Corn bran active polysaccharide and preparation method thereof - Google Patents
Corn bran active polysaccharide and preparation method thereof Download PDFInfo
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- CN101974169B CN101974169B CN2010105088294A CN201010508829A CN101974169B CN 101974169 B CN101974169 B CN 101974169B CN 2010105088294 A CN2010105088294 A CN 2010105088294A CN 201010508829 A CN201010508829 A CN 201010508829A CN 101974169 B CN101974169 B CN 101974169B
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Abstract
The invention relates to a method for extracting polysaccharides by comprehensively utilizing a corn non-starch component, i.e., corn bran, which belongs to the technical field of deep processing of agricultural byproducts and comprehensive utilization of by-products thereof. The invention discloses a corn bran active polysaccharide component and a preparation method thereof. The preparation method comprises the following steps of: taking the corn bran as materials to prepare the corn bran active polysaccharide component through the processes of microwave pretreatment, ultrasonic extraction, protein removing, bleaching, Sephadex G-75 column chromatography, concentration, and the like, wherein the extraction rate of a corn bran polysaccharide compound reaches as much as 8.16%, the protein removing rate reaches 80.42%, the sugar retention rate is 89.93 %, and the inhibition rate on S180 cells reaches as much as 59.12% which is 1.431 times as the value-added inhibition rate of 0. 05mg/mlcyclophosphamide. Therefore, a polysaccharides function factor component with antitumor activity developed by the invention not only can greatly improve the technical level of research and development on the corn non-starch component and the economic efficiency of corn processing enterprises, but also can provide an effective way for the development and the industrial transformation of corn bran active polysaccharide products.
Description
Technical field
The present invention relates to the non-starch fraction of corn---a kind of method of active polysaccharide is extracted in the maize peel comprehensive utilization, belongs to the technical field that agricultural byproducts intensive processing and byproduct comprehensive thereof utilize.
Background technology
Corn is the second largest grain variety of China, and corn processed enterprise all can produce a large amount of by products---maize peel every year, and is most directly as feed; Be underutilized, added value is very low, causes the major product cost high; The market competitiveness is poor, and economic benefit is low.And the vegetable polysaccharides compounds causes like antitumor, anti-infective, radioprotective, lowering blood glucose blood fat etc. that because of its different physiological roles people's the degree of depth is paid attention to.If can further utilize the exploitation of corn deep processing by product maize peel to have the polyose functional factor of anti-tumor activity; Both can improve the corn processed economic benefit of enterprises greatly, also be simultaneously to obtain the product development of maize peel active polysaccharide an effective way is provided.
At present, the contriver at home in academic journal " food research and development " volume the 2nd phase the 35th～38 page of " maize peel active polysaccharide extractive technique " of being delivered in February in 2009 the 30th through comparative analysis and L
9(3
4) research method such as orthogonal experimental design, its research contents only is centered around the influence to the maize peel polysaccharide extract rate of the different extraction times of high spot reviews, extraction temperature, lixiviate solid-to-liquid ratio.Paper studies result shows that the primary and secondary relation that influences maize peel polysaccharide extract rate factor is temperature, solid-liquid ratio, extraction time successively; The optimum extraction process condition is 100 ℃, extraction time 4h, and solid-to-liquid ratio 1: 20, polysaccharide extract rate on average can reach 4.43%.
Publish thesis is mainly reflected in following 4 main aspects with otherness of the present invention:
(1) the disclosed product of patent of the present invention is a kind of maize peel active polysaccharide component; Be to be measurement index with the S180 cell inhibitory rate; Identify and the functional performance evaluation study through extraction, separation, purifying, structure; What optimize reaches 59.12% maize peel active polysaccharide component to the S180 cell inhibitory rate, and this inhibiting rate is 1.431 times of 0.05mg/mL endoxan increment inhibiting rates; And the middle maize peel polyose crude extract that is merely the hot water lixiviate of setting forth that publishes thesis.Therefore say and publish thesis disclosed product of patent of the present invention and institute to set forth material be diverse.
(2) the disclosed technology of patent of the present invention is a kind of preparation method who prepares the maize peel active polysaccharide, and its core methed is a microwave and ultrasonic combined, and its maize peel polysaccharide compound extraction yield is up to 8.16%; And the focus of the middle set forth that publishes thesis has only been investigated three influence factors of different extraction times, extraction temperature, lixiviate solid-to-liquid ratio the influence situation big or small to the maize peel polysaccharide extract rate in the hot water leach extraction method, and research thinking and research means are all inequality;
(3) disclose analysis of maize peel polysaccharide content and yield method of calculation in publishing thesis, can directly apply in the patent extract of the present invention the analysis of maize peel polysaccharide content and yield and calculate, but be not under the jurisdiction of the claim protection domain of patent of the present invention.
(4) technological line and key points for operation (as follows) are disclosed in publishing thesis; Though all belong to raw material part gatherer process from maize peel → fine screen → clean → dry → pulverize; But this part content is not under the jurisdiction of the claim protection domain of patent of the present invention, and other parts are different fully with the disclosed technical scheme of patent of the present invention.
The patented technology route: maize peel → fine screen → clean → dry → pulverize → Microwave Pretreatment → ultrasonic extraction → except that albumen → decolouring → Sephadex G-75 column chromatography → concentrated → maize peel active polysaccharide component
Paper technological line: maize peel → fine screen → clean → dry → pulverize → hot water lixiviate → filter → filtrate in 4 ℃ of refrigerators and leave standstill 12h → filtration → filtrating concentrating → alcohol precipitation → filtration → filter residue and drying → Crude polysaccharides;
Summary of the invention
The technical problem that institute of the present invention quasi-solution is determined is: disclose a kind of maize peel active polysaccharide component; The method that openly prepares maize peel active polysaccharide component; Being to utilize the non-starch fraction of corn---maize peel is a main raw material; Adopt microwave and UW new technology, prepare and to reach 59.12% maize peel active polysaccharide component to the S180 cell inhibitory rate.
Technical scheme of the present invention is:
A kind of maize peel active polysaccharide component, component mainly contains uronic acid, neutral sugar; It is characterized in that each component and content thereof does, glucuronic acid content is 5%～15%, and neutral sugar content is 95%～85%;
Maize peel active polysaccharide component among the present invention, can reach 59.12% maize peel active polysaccharide concentration of component to the S180 cell inhibitory rate be 0.5mg/mL～3.5mg/mL.
A kind of method for preparing maize peel active polysaccharide component is characterized in that, through Microwave Pretreatment, ultrasonic extraction, remove albumen, decolouring, Sephadex G-75 column chromatography, technological process such as concentrate;
1) described Microwave Pretreatment process: be with through fine screen, (weight and volume ratio are v) carried out batch mixing at 1: 20 according to the solid-liquid ratio of maize peel and water to clean, dry, be crushed to 60 purpose corn bran raw materials; After treating that mixing of materials evenly; Place microwave heating appts; The controlled microwave processing power is that 200W～500W, microwave treatment time are after taking out behind 3min～15min, to place ultrasonic unit rapidly;
2) described ultrasonic extraction treating processes: be that material after the microwave treatment is carried out ultrasonic extraction; The control ultrasonic power is after 100W～800W, ultrasonic time are 5min～35min; Adopt whizzer to carry out solid-liquid separation (rotating speed 4000r/min～10000r/min; Centrifugation time 5min～30min), abandon throw out keeps supernatant and is maize peel polysaccharide compound crude extract;
3) the described protein process that removes: be to adopt the Sevage method; With the Sevage reagent (chloroform: propyl carbinol=4: 1) that adds 1/8～1/2 volume in the maize peel polysaccharide compound crude extract; Behind jolting 10～50min, leave standstill 30min～120min, centrifugal then disgorging matter (rotating speed 4000r/min～10000r/min; Behind the centrifugation time 5min～30min), it is subsequent use to keep supernatant;
4) described decolorization: be gac (powder, cylindrical, particle) with 0.5%～5.0%; The processing of decolouring under the condition of 40 ℃～100 ℃ of bleaching temperatures, bleaching time 10min～180min; Centrifugal then disgorging matter (rotating speed 4000r/min～10000r/min; Behind the centrifugation time 5min～30min), it is subsequent use to keep supernatant;
5) described Sephadex G-75 column chromatography process: be that the destainer applied sample amount is controlled at 5mL～10mL, deionized water eluent flow velocity is 0.2mL/min～1.0mL/min;
6) described concentration process: be destainer to be carried out vacuum concentration handle; Vacuum tightness is 0.065Mpa～0.095Mpa; Temperature can be 40 ℃～85 ℃, and making maize peel active polysaccharide concentration of component is 0.5mg/mL～3.5mg/mL (wherein glucuronic acid content is 5%～15%, neutral sugar content is 95%～85%).
Technique effect of the present invention is following:
(1) the present invention be a kind of be raw material with the maize peel; Through Microwave Pretreatment, ultrasonic extraction, remove albumen, decolouring, Sephadex G-75 column chromatography, technological process such as concentrate; Can prepare maize peel polysaccharide compound extraction yield up to 8.16%, the protein decreasing ratio reaches 80.42%, sugared retention rate is 89.93%, S180 cell inhibiting rate is reached 59.12%, is 1.431 times maize peel active polysaccharide component of the increment inhibiting rate of 0.05mg/ml endoxan.
(2) operational path of the present invention's design is simple and direct, less equipment investment, the feasible effective ways of industrialization promotion.
(3) can process product types such as oral liquid, electuary or capsule in component of the present invention.
Embodiment
Embodiment 1:
Will be through fine screen, (weight and volume ratio are v) carried out batch mixing after evenly at 1: 20 according to the solid-liquid ratio of maize peel and water to clean, dry, be crushed to 60 purpose corn bran raw materials; Being placed on microwave heating appts and controlled microwave processing power is that 200W, microwave treatment time are 15min; Then place ultrasonic unit more rapidly; The control ultrasonic power is after 800W, ultrasonic time are 5min, carries out solid-liquid separation (rotating speed 4000r/min, centrifugation time 5min); Abandon throw out, keep supernatant and be maize peel polysaccharide compound phase extract; Adopt the Sevage method to remove albumen, with the Sevage reagent of adding 1/8 volume in the maize peel polysaccharide compound crude extract (chloroform: propyl carbinol=4: 1), behind the jolting 50min; Leave standstill 100min, after the centrifugal then disgorging matter (rotating speed 10000r/min, centrifugation time 5min); Select the processing of decolouring under the condition of 5.0% 80 ℃ of gac (powder), bleaching temperatures, bleaching time 110min for use; After the centrifugal then disgorging matter (rotating speed 6000r/min, centrifugation time 15min), supernatant carries out Sephadex G-75 column chromatography; Make the destainer applied sample amount be controlled at 6.5mL, deionized water eluent flow velocity is 0.2mL/min; Destainer is carried out vacuum concentration handle, vacuum tightness is 0.065Mpa, and temperature can be 55 ℃, and making maize peel active polysaccharide concentration of component is that 1.5mg/mL (wherein glucuronic acid content is 5%, neutral sugar content is 95%) gets final product.
Embodiment 2:
Will be through fine screen, (weight and volume ratio are v) carried out batch mixing after evenly at 1: 20 according to the solid-liquid ratio of maize peel and water to clean, dry, be crushed to 60 purpose corn bran raw materials; Being placed on microwave heating appts and controlled microwave processing power is that 500W, microwave treatment time are 3min; Then place ultrasonic unit more rapidly; The control ultrasonic power is after 200W, ultrasonic time are 5min, carries out solid-liquid separation (rotating speed 4000r/min, centrifugation time 30min); Abandon throw out, keep supernatant and be maize peel polysaccharide compound crude extract; Adopt the Sevage method to remove albumen, with the Sevage reagent of adding 1/5 volume in the maize peel polysaccharide compound crude extract (chloroform: propyl carbinol=4: 1), behind the jolting 10min; Leave standstill 120min, after the centrifugal then disgorging matter (rotating speed 4000r/min, centrifugation time 30min); Select the processing of decolouring under the condition of 3.5% 40 ℃ of gac (cylindrical), bleaching temperatures, bleaching time 90min for use; After the centrifugal then disgorging matter (rotating speed 8000r/min, centrifugation time 5min), supernatant carries out Sephadex G-75 column chromatography; Make the destainer applied sample amount be controlled at 10mL, deionized water eluent flow velocity is 1.0mL/min; Destainer is carried out vacuum concentration handle, vacuum tightness is 0.095Mpa, and temperature can be 85 ℃, and making maize peel active polysaccharide concentration of component is that 3.4mg/mL (wherein glucuronic acid content is 15%, neutral sugar content is 85%) gets final product.
Embodiment 3:
Will be through fine screen, (weight and volume ratio are v) carried out batch mixing after evenly at 1: 20 according to the solid-liquid ratio of maize peel and water to clean, dry, be crushed to 60 purpose corn bran raw materials; Being placed on microwave heating appts and controlled microwave processing power is that 350W, microwave treatment time are 5min; Then place ultrasonic unit more rapidly; The control ultrasonic power is after 100W, ultrasonic time are 35min, carries out solid-liquid separation (rotating speed 10000r/min, centrifugation time 5min); Abandon throw out, keep supernatant and be maize peel polysaccharide compound crude extract; Adopt the Sevage method to remove albumen, with the Sevage reagent of adding 1/2 volume in the maize peel polysaccharide compound crude extract (chloroform: propyl carbinol=4: 1), behind the jolting 20min; Leave standstill 30min, after the centrifugal then disgorging matter (rotating speed 8000r/min, centrifugation time 15min); Select the processing of decolouring under the condition of 0.5% 100 ℃ of gac (particle), bleaching temperatures, bleaching time 10min for use; After the centrifugal then disgorging matter (rotating speed 10000r/min, centrifugation time 5min), supernatant carries out Sephadex G-75 column chromatography; Make the destainer applied sample amount be controlled at 5mL, deionized water eluent flow velocity is 0.85mL/min; Destainer is carried out vacuum concentration handle, vacuum tightness is 0.065Mpa, and temperature can be 40 ℃, and making maize peel active polysaccharide concentration of component is that 0.55mg/mL (wherein glucuronic acid content is 10%, neutral sugar content is 90%) gets final product.
Claims (3)
1. the preparation method of a maize peel active polysaccharide component is characterized in that, through Microwave Pretreatment, ultrasonic extraction, remove albumen, decolouring, Sephadex G-75 column chromatography, spissated technological process; Described maize peel active polysaccharide component, each component and content thereof do, glucuronic acid content is 5%～15%, and neutral sugar content is 95%～85%;
1) described Microwave Pretreatment process: be with through fine screen, clean, dry, be crushed to 60 purpose corn bran raw materials and carry out batch mixing at 1: 20 according to the feed liquid weight and the volume ratio of maize peel and water; After treating that mixing of materials evenly; Place microwave heating appts; The controlled microwave processing power is that 200W～500W, microwave treatment time are after taking out behind 3min～15min, to place ultrasonic unit rapidly;
2) described ultrasonic extraction treating processes: be that material after the microwave treatment is carried out ultrasonic extraction; The control ultrasonic power is after 100W～800W, ultrasonic time are 5min～35min; Adopt whizzer to carry out solid-liquid separation, centrifugal rotational speed 4000r/min～10000r/min, centrifugation time 5min～30min; Abandon throw out, keep supernatant and be maize peel polysaccharide compound crude extract;
3) the described protein process that removes: be to adopt the Sevage method; With the chloroform that adds 1/8～1/2 volume in the maize peel polysaccharide compound crude extract: the Sevage reagent of propyl carbinol=4: 1, behind jolting 10～50min, leave standstill 30min～120min; Centrifugal then disgorging matter; Centrifugal rotational speed 4000r/min～10000r/min, behind centrifugation time 5min～30min, it is subsequent use to keep supernatant;
4) described decolorization: be gac with 0.5%～5.0%; The processing of decolouring under the condition of 40 ℃～100 ℃ of bleaching temperatures, bleaching time 10min～180min; Centrifugal then disgorging matter; Centrifugal rotational speed 4000r/min～10000r/min, behind centrifugation time 5min～30min, it is subsequent use to keep supernatant;
5) described Sephadex G-75 column chromatography process: be that the destainer applied sample amount is controlled at 5mL～10mL, deionized water eluent flow velocity is 0.2mL/min～1.0mL/min;
6) described concentration process: be destainer to be carried out vacuum concentration handle; Vacuum tightness is 0.065Mpa～0.095Mpa; Temperature is 40 ℃～85 ℃; Making maize peel active polysaccharide concentration of component is 0.5mg/mL～3.5mg/mL, and wherein glucuronic acid content is 5%～15%, neutral sugar content is 95%～85%.
2. the maize peel active polysaccharide component of the preparation method of claim 1 maize peel active polysaccharide component preparation.
3. according to the described maize peel active polysaccharide of claim 2 component, it is characterized in that, described maize peel active polysaccharide component, can reach 59.12% maize peel active polysaccharide concentration of component to the S180 cell inhibitory rate be 0.5mg/mL～3.5mg/mL.
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| CN102702377A (en) * | 2012-06-21 | 2012-10-03 | 四川农业大学 | Termitomyces albuminosus polysaccharide separation and purification method and injection thereof |
| CN103340390B (en) * | 2013-06-26 | 2015-05-20 | 广州中医药大学 | Internal heat reducing and inflammation diminishing chili sauce |
| CN103923220B (en) * | 2014-04-17 | 2016-05-18 | 吉林大学 | A kind of method that improves maize peel coarse polysaccharide extractive rate by fast neutron irradiated technology |
| CN110511295A (en) * | 2019-09-23 | 2019-11-29 | 哈尔滨市第二医院 | A method of polysaccharide is prepared using corn stigma |
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| CN1640892A (en) * | 2004-12-16 | 2005-07-20 | 吉林农业大学 | Method for producing maize active polysaccharide |
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| CN1640892A (en) * | 2004-12-16 | 2005-07-20 | 吉林农业大学 | Method for producing maize active polysaccharide |
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| Title |
|---|
| JP特开2008-162944A 2008.07.17 |
| 林松毅等.玉米皮活性多糖提取技术.《食品研究与开发》.2009,第30卷(第2期),35-38. * |
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