CN102617534A - Method for extracting and purifying flavone pigments in rose dregs - Google Patents

Method for extracting and purifying flavone pigments in rose dregs Download PDF

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Publication number
CN102617534A
CN102617534A CN2012100699110A CN201210069911A CN102617534A CN 102617534 A CN102617534 A CN 102617534A CN 2012100699110 A CN2012100699110 A CN 2012100699110A CN 201210069911 A CN201210069911 A CN 201210069911A CN 102617534 A CN102617534 A CN 102617534A
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China
Prior art keywords
rose
membrane
pigment
slag
flavones
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Pending
Application number
CN2012100699110A
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Chinese (zh)
Inventor
董丽娟
马桂宝
袁绍宸
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LANZHOU SHENGTANG AGRO-ECOLOGY TECHNOLOGY Co Ltd
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LANZHOU SHENGTANG AGRO-ECOLOGY TECHNOLOGY Co Ltd
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Priority to CN2012100699110A priority Critical patent/CN102617534A/en
Publication of CN102617534A publication Critical patent/CN102617534A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a method for extracting and purifying flavone pigments in rose dregs. The method comprises the following steps of: 1, adding the rose dregs into alkaline water in a ratio of 1:10, and heating to obtain a mixed solution; filtering the mixed solution and removing impurities to obtain a filtrate and flower dregs, adding the flower dregs into the alkaline water in a ratio of 1:10, repeating the step, and mixing the filtrate; 2, separating the filtrate for 15 minutes at a speed of 3,600 revolutions/minute, and collecting a supernate to obtain a rose flavone pigment treatment fluid; and 3, performing membrane separation on the rose flavone pigment treatment fluid to obtain a rose flavone pigment concentrated solution, and concentrating under vacuum to obtain rose flavone pigment wet powder. According to the method, energy consumption is low in the membrane separation process, the separation efficiency is high, and the color, aroma and taste and nutritional ingredients of products can be kept; a technical process is easy, short in period and low in production cost, so the method is suitable for large-scale continuous production.

Description

A kind of method with the flavones pigment in the membrane technique extraction and purification rose slag
Technical field
The present invention relates to membrane separation technique is used for the technical field of plant extract, particularly adopt the ultra-filtration membrane of specific molecular weight cut-off and a kind of method that nf membrane organically combines with the flavones pigment in the membrane technique extraction and purification rose slag.
Background technology
Current research shows, contains a large amount of flavones pigment compounds in the rose slag, has very high using value.Just because of this, rose flavones pigment is just causing food expert's attention as a kind of health care nutrient.Traditional technology mainly adopts evaporation concentration, big, the filtration difficulty of energy consumption in the technological process, and also the temperature height can make flavones decompose, and influences extraction yield, and product colour is darker, and the flavones pigment content is not high.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that exists to prior art, provides that a kind of technological process energy consumption is low, separation efficiency is high, can keep the color, smell and taste of product and a kind of method with the flavones pigment in the membrane technique extraction and purification rose slag of nutritive ingredient.
Technical problem of the present invention adopts following technical proposals to solve:
A kind of method with the flavones pigment in the membrane technique extraction and purification rose slag; May further comprise the steps: 1. adopt the rose slag of carrying oil as raw materials for production; With the ratio adding alkaline water of rose slag in 1:10, be heated to 65 ℃-90 ℃, obtain mixed solution after 1 to 2 hours; Mixed solution is obtained filtrating and flower slag after with the filtered through gauze decon, and the flower slag adds alkaline water by 1:10 again, repeats above-mentioned steps, merging filtrate.
2. adopt whizzer filtrating to be separated 15min above-mentioned merging filtrate, obtain supernatant and filter residue, discard filter residue, collect supernatant, promptly get rose flavones pigment treatment solution with the speed of 3600r/min.
3. rose flavones pigment treatment solution is carried out membrane sepn, adopt the ultra-filtration membrane of molecular weight cut-off 1500dalton to separate earlier, hold back and remove soluble proteins in the solution, larger molecular organics matter, collect and see through liquid; Adopt the nanofiltration membrane separation of molecular weight cut-off 200dalton again, the small molecules inorganics in the filtering solution, the part of filtering simultaneously moisture, concentrated mother liquor, working pressure: 0.05~0.20MPa, 25 ℃~60 ℃ of temperature obtain rose flavones pigment concentrate.Through vacuum concentration, vacuum tightness is 0.03~0.07MPa again, and temperature is 20 ℃~65 ℃, obtains rose flavones pigment wet-milling.
Said step 3.-3.-nf membrane of b is with the PA membrane of molecular weight cut-off 200dalton the ultra-filtration membrane of a adopts the PS membrane of molecular weight cut-off 1500dalton.
The present invention possesses following beneficial effect:
1, the membrane sepn process is carried out at normal temperatures, does not undergo phase transition, and does not add any chemical reagent, and energy consumption is low, and separation efficiency is high, can keep the color, smell and taste and the nutritive ingredient of product.
2, membrane sepn of the present invention adopts sepn process efficiently, utilizes common simple device, the technological process processing ease.
3, process cycle is short, and production cost is low, is easy to serialization scale operation.
Embodiment
Embodiment 1
1, will carry 10 ㎏ flower slag+100 ㎏ alkaline waters of oil, be heated to 65 ℃, obtain mixed solution in 2 hours, mixed solution will be obtained filtrating and colored slag after with the filtered through gauze decon; The flower slag adds 100 ㎏ alkaline waters again, and reheat to 90 ℃ obtained mixed solution in 1 hour, and mixed solution is obtained filtrating and colored slag after with the filtered through gauze decon; Twice filtrating is merged.
2, with merging filtrate adopt whizzer with the centrifugal speed of 3600r/min to filtrating spinning 15min, obtain supernatant and filter residue, discard filter residue, collect supernatant, promptly get rose flavones pigment treatment solution.
3, the above-mentioned rose flavones pigment treatment solution that obtains is carried out membrane sepn, adopts the ultra-filtration membrane of molecular weight cut-off 1500dalton earlier---the PS membrane circulation separates; Hold back and remove soluble proteins in the solution, larger molecular organics matter; Collect and see through liquid, remove various larger molecular organicses, the working pressure of ultra-filtration membrane: 0.1MPa; 50 ℃ of temperature, must see through liquid is 62.5 ㎏.
4, adopting the nf membrane of molecular weight cut-off 200dalton again---PA membrane separates, the small molecules inorganics in the filtering solution, but the part of filtering simultaneously moisture; Concentrated mother liquor, working pressure: 0.5MPa, 60 ℃ of temperature; Obtain rose flavones liquid concentrator 16.8 ㎏, again through vacuum concentration, vacuum tightness is 0.03MPa; Temperature is 20 ℃, obtains rose flavones pigment wet-milling 5.6 ㎏.
5, it is dry rose flavones pigment wet-milling to be put into baking oven, and temperature is controlled at 75 ℃, and the time is 6 hours, gets flavones pigment Vandyke brown dry powder 0.3 ㎏.
Embodiment 2
1, will carry 10 ㎏ flower slag+100 ㎏ alkaline waters of oil, be heated to 90 ℃, obtain mixed solution in 1 hour, mixed solution will be obtained filtrating and colored slag after with the filtered through gauze decon; The flower slag adds 100 ㎏ alkaline waters again, and reheat to 65 ℃ obtained mixed solution in 2 hours, and mixed solution is obtained filtrating and colored slag after with the filtered through gauze decon; Twice filtrating is merged.
2, with merging filtrate adopt whizzer with the centrifugal speed of 3600r/min to filtrating spinning 15min, obtain supernatant and filter residue, discard filter residue, collect supernatant, promptly get rose flavones pigment treatment solution.
3, the above-mentioned rose flavones pigment treatment solution that obtains is carried out membrane sepn, adopts the ultra-filtration membrane of molecular weight cut-off 1500dalton earlier---the PS membrane circulation separates; Hold back and remove soluble proteins in the solution, larger molecular organics matter; Collect and see through liquid, remove various larger molecular organicses, the working pressure of ultra-filtration membrane: 0.6MPa; 25 ℃ of temperature, seeing through the liquid yield is 62.5 ㎏.
4, adopting the nf membrane of molecular weight cut-off 200dalton again---PA membrane separates, the small molecules inorganics in the filtering solution, but the part of filtering simultaneously moisture; Concentrated mother liquor, working pressure: 2.0MPa, 25 ℃ of temperature; Obtain rose flavones liquid concentrator 16.8 ㎏, again through vacuum concentration, vacuum tightness is 0.07MPa; Temperature is 65 ℃, obtains rose flavones pigment wet-milling 5.6 ㎏.
5, it is dry rose flavones pigment wet-milling to be put into baking oven, and temperature is controlled at 80 ℃ of 5 hours times, gets flavones pigment Vandyke brown dry powder 0.3 ㎏.

Claims (3)

1. method with the flavones pigment in the membrane technique extraction and purification rose slag is characterized in that may further comprise the steps:
1. adopt the rose slag of carrying oil as raw materials for production,, be heated to 65 ℃-90 ℃, obtain mixed solution after 1 to 2 hours the ratio adding alkaline water of rose slag in 1:10; Mixed solution is obtained filtrating and flower slag after with the filtered through gauze decon, and the flower slag adds alkaline water by 1:10 again, repeats above-mentioned steps, merging filtrate;
2. adopt whizzer filtrating to be separated 15min above-mentioned merging filtrate, obtain supernatant and filter residue, discard filter residue, collect supernatant, promptly get rose flavones pigment treatment solution with the speed of 3600r/min;
3. rose flavones pigment treatment solution is carried out membrane sepn,
3.-and a adopts earlier the hyperfiltration membrane assembly of the molecular weight cut-off 1500dalton separating treatment that circulates, working pressure: 0.1MPa-0.6MPa, and 25 ℃-50 ℃ of temperature are removed soluble proteins in the treatment solution, larger molecular organics matter, collect ultrafiltration membrane permeate liquid;
3.-and nanofiltration membrane component that b adopts molecular weight cut-off 200dalton again carries out separating treatment to seeing through liquid, and filtering sees through the small molecules inorganics in the liquid, removes part moisture simultaneously; Collect concentrated mother liquor, working pressure: 0.5-2.0MPa, 25 ℃-60 ℃ of temperature; Obtain rose flavones liquid concentrator
3.-and c is through vacuum concentration, and vacuum tightness is 0.03-0.07MPa, and temperature is 20 ℃-65 ℃, obtains rose flavones pigment wet-milling.
2. a kind of method with the flavones pigment in the membrane technique extraction and purification rose slag as claimed in claim 1 is characterized in that said step lixiviate number of times 1. is twice.
3. a kind of method as claimed in claim 1 with the flavones pigment in the membrane technique extraction and purification rose slag; It is characterized in that said step 3.-ultra-filtration membrane of a adopts the PS membrane of molecular weight cut-off 1500dalton, nf membrane adopts the PA membrane of molecular weight cut-off 200dalton.
CN2012100699110A 2012-03-16 2012-03-16 Method for extracting and purifying flavone pigments in rose dregs Pending CN102617534A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN107467712A (en) * 2017-07-28 2017-12-15 云南中烟工业有限责任公司 It is a kind of with the tobacco sauce additive of antibacterial activity and its application

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CN101125962A (en) * 2006-08-16 2008-02-20 王仕尧 Technique for extracting roselle calyx red pigment
JP2008074920A (en) * 2006-09-20 2008-04-03 Yoshino Senka Kenkyusho:Kk Method for extracting natural pigment and/or perfume
CN101473932A (en) * 2008-12-02 2009-07-08 庆阳市康惠玫瑰发展有限责任公司 Method for extracting natural rose color pigment from fresh rose
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107467712A (en) * 2017-07-28 2017-12-15 云南中烟工业有限责任公司 It is a kind of with the tobacco sauce additive of antibacterial activity and its application
CN107467712B (en) * 2017-07-28 2019-05-21 云南中烟工业有限责任公司 A kind of tobacco sauce additive and its application with antibacterial activity

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Application publication date: 20120801