CN103342692A - Method for extracting blueberry anthocyanin - Google Patents
Method for extracting blueberry anthocyanin Download PDFInfo
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- CN103342692A CN103342692A CN2013103121126A CN201310312112A CN103342692A CN 103342692 A CN103342692 A CN 103342692A CN 2013103121126 A CN2013103121126 A CN 2013103121126A CN 201310312112 A CN201310312112 A CN 201310312112A CN 103342692 A CN103342692 A CN 103342692A
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Abstract
The invention discloses a method for extracting blueberry anthocyanin. The method comprising the following steps of: (1) pretreating raw materials; (2) extracting blueberry anthocyanin to obtain a blueberry anthocyanin crude extraction solution; and (3) refining the blueberry anthocyanin, and performing vacuum concentration on the blueberry anthocyanin until the content of the blueberry anthocyanin is 50% to obtain a finished product of a blueberry anthocyanin concentrated solution. According to the method for extracting the blueberry anthocyanin, the problems of low concentration of a blueberry anthocyanin extract and higher loss of the blueberry anthocyanin during extraction can be solved, and the defects of large solvent usage amount, long extraction time and high production cost of the existing extraction method can be overcome, so that the method disclosed by the invention is beneficial for environmental protection, energy conservation and development of cyclic economy, and has very significant economic and social benefits.
Description
Technical field
The present invention relates to a kind of extracting method of vaccinium oxycoccus pigment, especially anthocyanidin content is the extracting method of 50% vaccinium oxycoccus pigment, belongs to natural active matter extractive technique field.
Background technology
Blueberry is shrub, every clump has branch 25-30 bar as a result, yielded positive results in the 2nd year, but output is less, optimum yield was arranged on the 3rd year, entered high yield period on the 5th year, 50 years its life-spans, average single plant yield 3-6 kilogram, mean fruit weight 2 grams, about general every mu of field planting 300 strains, mean yield 1500-2000 kilogram.Anthocyanidin is the antidotal nutritious supplementary of pure natural, studies have shown that it is that mankind nowadays is found good antioxidant, and its antioxidant property exceeds 50 times than vitamin-E, exceeds 200 times than vitamins C.It is 100% to the biological effectiveness of human body, takes the back and just can detect in blood in 20 minutes.Anthocyanidin is called as " oral skin cosmetics " in Europe, vaccinium oxycoccus pigment especially, and skin nutrition strengthens skin immunization power, tackles various allergic conditions, is the most effective antioxidant of present nature.It not only can prevent generating ahead of time of wrinkle of skin, can keep also that normal cell links, blood vessel stable, strengthen the fine vascular circulation, improve flowing of capillary blood vessel and vein, and then reach the rapid healing of unusual skin.Anthocyanidin is natural sunlight overcover, can prevent ultraviolet ray infringement skin, and skin belongs to reticular tissue, and wherein contained collagen protein and rigid albumen play an important role to the entire structure of skin.It is appropriately crosslinked that anthocyanidin can promote that collagen protein forms, it is as a kind of effective free-radical scavengers, can prevent the generation of skin Du " excessively crosslinked " this unusual physiological situation, thereby also just stoped the appearance of wrinkle of skin and vesica, anthocyanidin can also stop the generation of rigid proteolytic enzyme and suppress its active free radical or rigid albumen of elastin enzyme liberating of stoping, and obviously improves the healthy state of skin internally.
The content of anthocyanidin is higher than other all fruit and vegetables in the blue berry, ranks the first, and therefore, blue berry is the raw material of the good natural anthocyanidin of extraction.Vaccinium oxycoccus pigment is soluble in acidic medium, solubleness in alcoholic solution is high and water-soluble lower, domestic and international market sale at present and the product of using mostly are to adopt the solvent lixiviate in conjunction with the method preparation of column chromatographic isolation and purification, and the extraction solvent of application mostly is the mixed solution of methyl alcohol, ethanol and water.But this method exists the defective that the organic solvent usage quantity is big, technological process is many, extraction time is long, the products production cost is high.The method that present people have invented a lot of extraction anthocyanidin, but products therefrom concentration is lower, and loss is bigger, causes the significant wastage of resource.
Summary of the invention
At the deficiency that prior art exists, technical problem to be solved by this invention is to provide a kind of extracting method of vaccinium oxycoccus pigment, the problem that concentration is low, the leaching process loss is bigger of solution vaccinium oxycoccus pigment extract.
For solving the problems of the technologies described above, the technical solution used in the present invention is, a kind of extracting method of vaccinium oxycoccus pigment, and it comprises the following steps:
(1) pre-treatment of raw material: getting does not have the clean impurity elimination of the blue berry that rots, and adds extracting solution in 1: 1～1: 2 by the feed liquid mass ratio, and crushing and beating gets the blueberry slurries; Described extracting solution is ethanolic soln or the ethanolic soln of lactic acid acidifying or the ethanolic soln of citric acid acidifying of tartrate acidifying; The volume fraction of ethanol is 35～75% in the extracting solution, drips tartrate or lactic acid or citric acid, and making the ethanolic soln pH value of acidifying is 3.0～6.0.
(2) extraction of vaccinium oxycoccus pigment: get the blueberry slurries, press material liquid volume and added aforementioned extracting solution than 1: 4～1: 10, stirring and leaching staticly settled layering after 20～30 minutes, and 40～65 ℃ of lixiviates are 2～3 hours then, collect the upper strata vat liquor; Get vat liquor in the centrifugal 10～15min of 6000～12000r/min, obtain throw out and supernatant liquor, throw out by the lixiviate 1 time again of above-mentioned condition, and is obtained throw out and supernatant liquor with above-mentioned the same terms centrifugation; Collect, merge the centrifuged supernatant of 2 secondary clearings then; With centrifuged supernatant 55～65 ℃ of temperature, vacuum tightness-0.08～-the 1.0MPa condition under concentrating under reduced pressure, the ethyl acetate that adds 20%～30% its volume then, fully stirring and evenly mixing is removed the upper strata ethyl acetate behind the standing demix, obtains the vaccinium oxycoccus pigment crude extract;
(3) vaccinium oxycoccus pigment is refining: with the vaccinium oxycoccus pigment crude extract with the flow velocity of 1～4 times of column volume/h through being filled with the macroporous resin absorption post, vaccinium oxycoccus pigment is saturated by macroporous resin adsorption, use again 65% ethanolic soln with the flow velocity wash-out of 0.1～0.5 times of column volume/h by the vaccinium oxycoccus pigment of macroporous resin adsorption, collect elutriant; With elutriant 50～60 ℃ of temperature, vacuum tightness-0.08～-the 1.0MPa condition under concentrating under reduced pressure vaccinium oxycoccus pigment content be 50%, obtain vaccinium oxycoccus pigment concentrated solution finished product;
Described lixiviate is ultrasonic auxiliary lixiviate; Ultrasonic temperature 30-50 ℃, ultrasonic power 500-700W, dutycycle 1: 0.1-1: 0.5, ultrasonic time 5-10min.
Described macroporous resin is nonpolar macroporous adsorption resins such as D101 or AB-8.
The extracting method of vaccinium oxycoccus pigment of the present invention, the problem that the concentration that can solve the vaccinium oxycoccus pigment extract is low, the loss of leaching process anthocyanidin is bigger, and can overcome the defective that the solvent usage quantity is big, extraction time is long, production cost is high that present extracting method exists, be conducive to the development of environmental protection, energy-conservation and recycling economy, have the economic and social benefit of highly significant.
Embodiment
The present invention is described in more detail below in conjunction with embodiment.
Embodiment 1
The extracting method of the vaccinium oxycoccus pigment of present embodiment, it comprises the following steps:
(1) pre-treatment of raw material: getting does not have the clean impurity elimination of the blue berry that rots, and adds extracting solution at 1: 1 by the feed liquid mass ratio, and crushing and beating gets the blueberry slurries; Described extracting solution is the ethanolic soln of citric acid acidifying; The volume fraction of ethanol is 35% in the extracting solution, drips citric acid, makes the ethanolic soln pH value of acidifying be 3.0-4.0.
(2) extraction of vaccinium oxycoccus pigment: get the blueberry slurries, press material liquid volume and added aforementioned extracting solution than 1: 4, stirring and leaching staticly settled layering after 20～30 minutes, and 40～65 ℃ of lixiviates are 3 hours then, collect the upper strata vat liquor; Described lixiviate is ultrasonic auxiliary lixiviate; Ultrasonic temperature 30-50 ℃, ultrasonic power 500-700W, dutycycle 1: 0.1-1: 0.5, ultrasonic time 5-10min.Get vat liquor in the centrifugal 10min of 6000～12000r/min, obtain throw out and supernatant liquor, throw out by the lixiviate 1 time again of above-mentioned condition, and is obtained throw out and supernatant liquor with above-mentioned the same terms centrifugation; Collect, merge the centrifuged supernatant of 2 secondary clearings then; With centrifuged supernatant 55～65 ℃ of temperature, vacuum tightness-0.08～-the 1.0MPa condition under concentrating under reduced pressure, the ethyl acetate that adds 20%～30% its volume then, fully stirring and evenly mixing is removed the upper strata ethyl acetate behind the standing demix, obtains the vaccinium oxycoccus pigment crude extract;
(3) vaccinium oxycoccus pigment is refining: with the vaccinium oxycoccus pigment crude extract with the flow velocity of 4 times of column volume/h through being filled with the macroporous resin absorption post, described macroporous resin is nonpolar macroporous adsorption resins such as D101 or AB-8.Vaccinium oxycoccus pigment is saturated by macroporous resin adsorption, use again 65% ethanolic soln with the flow velocity wash-out of 0.5 times of column volume/h by the vaccinium oxycoccus pigment of macroporous resin adsorption, collect elutriant; With elutriant 50～60 ℃ of temperature, vacuum tightness-0.08～-the 1.0MPa condition under concentrating under reduced pressure vaccinium oxycoccus pigment content be 50%, obtain vaccinium oxycoccus pigment concentrated solution finished product.
Embodiment 2
The extracting method of the vaccinium oxycoccus pigment of present embodiment, it comprises the following steps:
(1) pre-treatment of raw material: getting does not have the clean impurity elimination of the blue berry that rots, and adds extracting solution at 1: 2 by the feed liquid mass ratio, and crushing and beating gets the blueberry slurries; Described extracting solution is the ethanolic soln of tartrate acidifying; The volume fraction of ethanol is 75% in the extracting solution, drips tartrate, makes the ethanolic soln pH value of acidifying be 5.0-6.0.
(2) extraction of vaccinium oxycoccus pigment: get the blueberry slurries, press material liquid volume and added aforementioned extracting solution than 1: 10, stirring and leaching staticly settled layering after 20～30 minutes, and 40～65 ℃ of lixiviates are 2 hours then, collect the upper strata vat liquor; Described lixiviate is ultrasonic auxiliary lixiviate; Ultrasonic temperature 30-50 ℃, ultrasonic power 500-700W, dutycycle 1: 0.1-1: 0.5, ultrasonic time 5-10min.Get vat liquor in the centrifugal 15min of 6000～12000r/min, obtain throw out and supernatant liquor, throw out by the lixiviate 1 time again of above-mentioned condition, and is obtained throw out and supernatant liquor with above-mentioned the same terms centrifugation; Collect, merge the centrifuged supernatant of 2 secondary clearings then; With centrifuged supernatant 55～65 ℃ of temperature, vacuum tightness-0.08～-the 1.0MPa condition under concentrating under reduced pressure, the ethyl acetate that adds 20%～30% its volume then, fully stirring and evenly mixing is removed the upper strata ethyl acetate behind the standing demix, obtains the vaccinium oxycoccus pigment crude extract;
(3) vaccinium oxycoccus pigment is refining: with the vaccinium oxycoccus pigment crude extract with the flow velocity of 1 times of column volume/h through being filled with the macroporous resin absorption post, described macroporous resin is nonpolar macroporous adsorption resins such as D101 or AB～8.Vaccinium oxycoccus pigment is saturated by macroporous resin adsorption, use again 65% ethanolic soln with the flow velocity wash-out of 0.1 times of column volume/h by the vaccinium oxycoccus pigment of macroporous resin adsorption, collect elutriant; With elutriant 50～60 ℃ of temperature, vacuum tightness-0.08～-the 1.0MPa condition under concentrating under reduced pressure vaccinium oxycoccus pigment content be 50%, obtain vaccinium oxycoccus pigment concentrated solution finished product.
Embodiment 3
The extracting method of the vaccinium oxycoccus pigment of present embodiment, it comprises the following steps:
(1) pre-treatment of raw material: getting does not have the clean impurity elimination of the blue berry that rots, and adds extracting solution at 1: 1.5 by the feed liquid mass ratio, and crushing and beating gets the blueberry slurries; Described extracting solution is the ethanolic soln of lactic acid acidifying; The volume fraction of ethanol is 50% in the extracting solution, drips lactic acid, and making the ethanolic soln pH value of acidifying is 5.0.
(2) extraction of vaccinium oxycoccus pigment: get the blueberry slurries, press material liquid volume and added aforementioned extracting solution than 1: 7, stirring and leaching staticly settled layering after 20～30 minutes, and 40～65 ℃ of lixiviates are 2.5 hours then, collect the upper strata vat liquor; Described lixiviate is ultrasonic auxiliary lixiviate; Ultrasonic temperature 30-50 ℃, ultrasonic power 500-700W, dutycycle 1: 0.1-1: 0.5, ultrasonic time 5-10min.Get vat liquor in the centrifugal 13min of 6000～12000r/min, obtain throw out and supernatant liquor, throw out by the lixiviate 1 time again of above-mentioned condition, and is obtained throw out and supernatant liquor with above-mentioned the same terms centrifugation; Collect, merge the centrifuged supernatant of 2 secondary clearings then; With centrifuged supernatant 55～65 ℃ of temperature, vacuum tightness-0.08～-the 1.0MPa condition under concentrating under reduced pressure, the ethyl acetate that adds 20%～30% its volume then, fully stirring and evenly mixing is removed the upper strata ethyl acetate behind the standing demix, obtains the vaccinium oxycoccus pigment crude extract;
(3) vaccinium oxycoccus pigment is refining: with the vaccinium oxycoccus pigment crude extract with the flow velocity of 2 times of column volume/h through being filled with the macroporous resin absorption post, described macroporous resin is nonpolar macroporous adsorption resins such as D101 or AB-8.Vaccinium oxycoccus pigment is saturated by macroporous resin adsorption, use again 65% ethanolic soln with the flow velocity wash-out of 0.3 times of column volume/h by the vaccinium oxycoccus pigment of macroporous resin adsorption, collect elutriant; With elutriant 50～60 ℃ of temperature, vacuum tightness-0.08～-the 1.0MPa condition under concentrating under reduced pressure vaccinium oxycoccus pigment content be 50%, obtain vaccinium oxycoccus pigment concentrated solution finished product.
The extracting method of vaccinium oxycoccus pigment of the present invention adopts the combination organic solvent method to carry out lixiviate to fruit juice, to improve the extraction yield of pigment.For the original character that guarantees pigment constant, in extracting whole process, adopt low temperature control acid system to keep the stability of pigment, the problem that the concentration that can solve the vaccinium oxycoccus pigment extract is low, the loss of leaching process anthocyanidin is bigger, and can overcome the defective that the solvent usage quantity is big, extraction time is long, production cost is high that present extracting method exists, be conducive to the development of environmental protection, energy-conservation and recycling economy, have the economic and social benefit of highly significant.
Claims (3)
1. the extracting method of a vaccinium oxycoccus pigment, it comprises the following steps:
(1) pre-treatment of raw material: getting does not have the clean impurity elimination of the blue berry that rots, and adds extracting solution in 1: 1～1: 2 by the feed liquid mass ratio, and crushing and beating gets the blueberry slurries; Described extracting solution is ethanolic soln or the ethanolic soln of lactic acid acidifying or the ethanolic soln of citric acid acidifying of tartrate acidifying; The volume fraction of ethanol is 35～75% in the extracting solution, drips tartrate or lactic acid or citric acid, and making the ethanolic soln pH value of acidifying is 3.0～6.0.
(2) extraction of vaccinium oxycoccus pigment: get the blueberry slurries, press material liquid volume and added aforementioned extracting solution than 1: 4～1: 10, stirring and leaching staticly settled layering after 20～30 minutes, and 40～65 ℃ of lixiviates are 2～3 hours then, collect the upper strata vat liquor; Get vat liquor in the centrifugal 10～15min of 6000～12000r/min, obtain throw out and supernatant liquor, throw out by the lixiviate 1 time again of above-mentioned condition, and is obtained throw out and supernatant liquor with above-mentioned the same terms centrifugation; Collect, merge the centrifuged supernatant of 2 secondary clearings then; With centrifuged supernatant 55～65 ℃ of temperature, vacuum tightness-0.08～-the 1.0MPa condition under concentrating under reduced pressure, the ethyl acetate that adds 20%～30% its volume then, fully stirring and evenly mixing is removed the upper strata ethyl acetate behind the standing demix, obtains the vaccinium oxycoccus pigment crude extract;
(3) vaccinium oxycoccus pigment is refining: with the vaccinium oxycoccus pigment crude extract with the flow velocity of 1～4 times of column volume/h through being filled with the macroporous resin absorption post, vaccinium oxycoccus pigment is saturated by macroporous resin adsorption, use again 65% ethanolic soln with the flow velocity wash-out of 0.1～0.5 times of column volume/h by the vaccinium oxycoccus pigment of macroporous resin adsorption, collect elutriant; With elutriant 50～60 ℃ of temperature, vacuum tightness-0.08～-the 1.0MPa condition under concentrating under reduced pressure vaccinium oxycoccus pigment content be 50%, obtain vaccinium oxycoccus pigment concentrated solution finished product.
2. the extracting method of vaccinium oxycoccus pigment according to claim 1 is characterized in that, described lixiviate is ultrasonic auxiliary lixiviate; Ultrasonic temperature 30-50 ℃, ultrasonic power 500-700W, dutycycle 1: 0.1-1: 0.5, ultrasonic time 5-10min.
3. the extracting method of vaccinium oxycoccus pigment according to claim 2 is characterized in that, described macroporous resin is nonpolar macroporous adsorption resins such as D101 or AB-8.
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| CN103626733A (en) * | 2013-11-08 | 2014-03-12 | 天津大学 | Separation method of blueberry anthocyanin |
| CN104447666A (en) * | 2014-11-27 | 2015-03-25 | 沈阳农业大学 | Method for extracting black chokeberry anthocyanin |
| CN104725341A (en) * | 2015-02-12 | 2015-06-24 | 贵州省生物研究所 | Efficient extraction method for blueberry anthocyanin |
| CN105130942A (en) * | 2015-09-03 | 2015-12-09 | 广东融和生态农业有限公司 | Method for extracting anthocyanin from blueberries |
| CN105176938A (en) * | 2015-09-03 | 2015-12-23 | 广东融和生态农业有限公司 | Method for simultaneously separating anthocyanin, SOD and nicotinic acid from blueberry cloudy juice |
| CN105254609A (en) * | 2015-11-27 | 2016-01-20 | 江苏万村爱农农业科技有限公司 | Blueberry anthocyanin extracting method |
| CN105558255A (en) * | 2015-12-29 | 2016-05-11 | 陕西省植物蛋白食品工程技术研究中心有限公司 | Blueberry-leaf peptide nutrient and preparation method thereof |
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| CN105961636A (en) * | 2016-06-06 | 2016-09-28 | 张大伟 | Linseed oil rich in blueberry anthocyanin and production method of linseed oil |
| CN106074280A (en) * | 2016-07-12 | 2016-11-09 | 广州丹奇日用化工厂有限公司 | The preparation method and applications of purple Chinese cabbage anthocyanidin |
| CN106243075A (en) * | 2016-08-03 | 2016-12-21 | 安徽徽王农业有限公司 | The separation method of vaccinium oxycoccus pigment |
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| CN109553599A (en) * | 2019-01-17 | 2019-04-02 | 江苏省农业科学院 | A kind of blueberry anthocyanin and its preparation method and application |
| WO2020233101A1 (en) * | 2019-05-21 | 2020-11-26 | 江南大学 | Colorful-jelly 4d printing method utilizing spontaneous color change of blueberry anthocyanins |
| CN112094256A (en) * | 2020-07-31 | 2020-12-18 | 浙江理工大学绍兴生物医药研究院有限公司 | Method for extracting purple acanthopanax anthocyanin |
| CN115466240A (en) * | 2022-10-20 | 2022-12-13 | 吉林化工学院 | Method for extracting anthocyanin from blueberries |
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| CN103626733B (en) * | 2013-11-08 | 2015-07-29 | 天津大学 | Separation method of blueberry anthocyanin |
| CN103626733A (en) * | 2013-11-08 | 2014-03-12 | 天津大学 | Separation method of blueberry anthocyanin |
| CN104447666A (en) * | 2014-11-27 | 2015-03-25 | 沈阳农业大学 | Method for extracting black chokeberry anthocyanin |
| CN104725341A (en) * | 2015-02-12 | 2015-06-24 | 贵州省生物研究所 | Efficient extraction method for blueberry anthocyanin |
| CN105130942A (en) * | 2015-09-03 | 2015-12-09 | 广东融和生态农业有限公司 | Method for extracting anthocyanin from blueberries |
| CN105176938A (en) * | 2015-09-03 | 2015-12-23 | 广东融和生态农业有限公司 | Method for simultaneously separating anthocyanin, SOD and nicotinic acid from blueberry cloudy juice |
| CN105254609A (en) * | 2015-11-27 | 2016-01-20 | 江苏万村爱农农业科技有限公司 | Blueberry anthocyanin extracting method |
| CN105558255B (en) * | 2015-12-29 | 2019-10-01 | 陕西省植物蛋白食品工程技术研究中心有限公司 | Blueberry leaf peptide nutrient food and preparation method thereof |
| CN105558255A (en) * | 2015-12-29 | 2016-05-11 | 陕西省植物蛋白食品工程技术研究中心有限公司 | Blueberry-leaf peptide nutrient and preparation method thereof |
| CN105961636A (en) * | 2016-06-06 | 2016-09-28 | 张大伟 | Linseed oil rich in blueberry anthocyanin and production method of linseed oil |
| CN105949164A (en) * | 2016-06-08 | 2016-09-21 | 句容市东方紫酒业有限公司 | Mulberry anthocyanin extracting method |
| CN106074280A (en) * | 2016-07-12 | 2016-11-09 | 广州丹奇日用化工厂有限公司 | The preparation method and applications of purple Chinese cabbage anthocyanidin |
| CN106243075A (en) * | 2016-08-03 | 2016-12-21 | 安徽徽王农业有限公司 | The separation method of vaccinium oxycoccus pigment |
| CN107173463A (en) * | 2017-06-15 | 2017-09-19 | 德阳市华盛植物油有限公司 | A kind of vegetable oil with the function that reduces blood pressure |
| CN107183217A (en) * | 2017-06-15 | 2017-09-22 | 德阳市华盛植物油有限公司 | Can reduce blood pressure blood fat edible vegetable oil preparation method |
| CN107232461A (en) * | 2017-06-15 | 2017-10-10 | 西南大学 | A kind of processing method of purple potato blueberry composite beverage |
| CN107736542A (en) * | 2017-10-10 | 2018-02-27 | 广西南宁桂尔创环保科技有限公司 | A kind of compound lozenge of blueberry and preparation method thereof |
| CN109553599A (en) * | 2019-01-17 | 2019-04-02 | 江苏省农业科学院 | A kind of blueberry anthocyanin and its preparation method and application |
| WO2020233101A1 (en) * | 2019-05-21 | 2020-11-26 | 江南大学 | Colorful-jelly 4d printing method utilizing spontaneous color change of blueberry anthocyanins |
| CN112094256A (en) * | 2020-07-31 | 2020-12-18 | 浙江理工大学绍兴生物医药研究院有限公司 | Method for extracting purple acanthopanax anthocyanin |
| CN115466240A (en) * | 2022-10-20 | 2022-12-13 | 吉林化工学院 | Method for extracting anthocyanin from blueberries |
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Application publication date: 20131009 |