CN103554329A - Molecularly imprinted polymer based aloe-emodin removal technology - Google Patents
Molecularly imprinted polymer based aloe-emodin removal technology Download PDFInfo
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- CN103554329A CN103554329A CN201310498676.3A CN201310498676A CN103554329A CN 103554329 A CN103554329 A CN 103554329A CN 201310498676 A CN201310498676 A CN 201310498676A CN 103554329 A CN103554329 A CN 103554329A
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- rhabarberone
- imprinted polymer
- molecularly imprinted
- emodin
- aloe
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Abstract
The invention belongs to the technical field of aloe-emodin removal and discloses a molecularly imprinted polymer based aloe-emodin removal technology. The technology comprises the following steps: dissolving an aloe-emodin standard product with a purity being more than 98% into acetone the weight of which is 60 times as large as the weight of the aloe-emodin standard product; then mixing with a methacrylic acid or acrylamide functional monomer, an ethylene glycol dimethacrylate crosslinking agent and an azodiisobutyronitrile initiator; carrying out ultrasonic treatment, blowing nitrogen, sealing, carrying out 60 DEG C water-bath polymerization reaction for 24h; crushing, sieving by using a 100-mesh sieve, and drying; carrying out repeated eluting and suction filter by using methanol acetic acid eluent (volume ratio: 8:2) the weight of which is 50 times as large as the weight of aloe-emodin under ultrasonic conditions under an ultrasonic condition until the eluent has no absorption through detection under 429nm condition; and drying again; and mixing with an aloe-emodin gel solution, and centrifuging, wherein liquid supernatant is a gel solution with aloe-emodin removed. By using the aloe-emodin removal technology, the aloe-emodin removal rate can reach 99.50%.
Description
Technical field
The technical field that removes that the invention belongs to Schuttgelb in new food raw material aloe, has particularly related to a kind of rhabarberone of molecularly imprinted polymer that utilizes and has removed technological method.
Technical background
Rhabarberone is the material of a kind of orange needle crystal or khaki color crystalline powder, belongs to Anthraquinones, is present in aloe.In the processing process of aloe food, may have part rhabarberone and remain in aloe food, the rhabarberone of lower concentration will work the mischief to HUMAN HEALTH, and has catharsis effect and sensitization.Therefore,, in the course of processing of actual food product system, remove or the content that reduces rhabarberone is very important.
Present stage, the mode that removes of rhabarberone was mainly liquid-liquid extraction, but this method length consuming time, complex steps, need to consume a large amount of solvents, and removal effect is general.Therefore, the present invention is directed to rhabarberone and prepared molecularly imprinted polymer, this molecularly imprinted polymer has specific adsorption effect to rhabarberone, the rhabarberone in can effective elimination food.
Summary of the invention
The object of the invention be to provide a kind of fast, the technology that removes of the rhabarberone that efficient, selectivity is good, decreasing ratio is high.Technical scheme of the present invention is as follows:
(1) preparation of rhabarberone molecularly imprinted polymer: taking purity is more than 98% rhabarberone standard substance, be dissolved in the acetone of 60 times of rhabarberone weight, with methacrylic acid or acrylamide function monomer (1:4), ethylene glycol dimethacrylate linking agent (1:20), Diisopropyl azodicarboxylate initiator (1:6) mixes, mixed solution supersound process 10min, nitrogen blows 15min, sealing, be placed in 60 ℃ of water-bath polyreaction 24h, pulverize, cross 100 mesh sieves, dry, be placed in beaker, elutriant (the methyl alcohol: acetic acid that adds 50 times of rhabarberone weight, volume ratio 8:2), ultrasonic wash-out 30min, suction filtration, get filter residue and repeat said process, until elutriant detects without absorbing under 429nm wavelength, filter residue after wash-out is placed in to baking oven, dry, obtain rhabarberone molecularly imprinted polymer,
(2) removing of rhabarberone molecularly imprinted polymer: get the gelating soln that contains rhabarberone, add above-mentioned molecularly imprinted polymer, concussion 5h, centrifugal, remove precipitation, supernatant liquor is the gelating soln that has removed rhabarberone.
Advantage of the present invention is: adopt rhabarberone removal methods of the present invention, easy and simple to handle, consuming time short, decreasing ratio is high.
Accompanying drawing explanation
The adsorptive capacity curve of Fig. 1 molecular imprinting polymer to different concns rhabarberone solution, i.e. concentration gradient adsorption curve.
Embodiment
Below in conjunction with example, the present invention is described in further details, but the present invention is not limited only to following examples.
Embodiment 1
Get 63mg rhabarberone standard substance, use 20ml acetone solution, add methacrylic acid function monomer 110mg, place 12h and carry out prepolymerization, then add ethylene glycol dimethacrylate linking agent 1.2g, Diisopropyl azodicarboxylate initiator 18mg, supersound process 10min, is transferred to test tube by solution and carries out nitrogen and blow 15min, sealing, 60 ℃ of water-bath 24h, obtain bar-shaped polymkeric substance.Polymkeric substance was pulverized to 100 mesh sieves, dried, added methyl alcohol: acetic acid (volume ratio 8:2) elutriant is ultrasonic wash-out, suction filtration repeatedly, until elutriant detects without absorbing under 429nm wavelength, filter residue after wash-out is placed in to baking oven, dries, obtain rhabarberone molecularly imprinted polymer.
Embodiment 2
The rhabarberone solution of preparation different concns (is respectively 100ppm, 300ppm, 500ppm, 700ppm, 900ppm, 1000ppm), respectively get 3ml, add molecularly imprinted polymer 150mg to adsorb, centrifuging and taking supernatant liquor after 5h, at 429nm place, measure its absorbancy, compare in the absorbancy at 429nm place with original solution.Both differences are the rhabarberone being adsorbed.
Adsorptive capacity calculation formula:
Q=(C
0-C)×V／W
Q: adsorptive capacity (μ mol/g)
C0: the starting point concentration of rhabarberone solution (μ mol/ml)
C: the rhabarberone strength of solution (μ mol/ml) after molecularly imprinted polymer absorption
V: the volume of solution (ml)
W: sorbent material dry weight (g)
According to formula, calculate the adsorptive capacity of molecularly imprinted polymer to rhabarberone, this molecularly imprinted polymer to the adsorptive capacity of the rhabarberone solution of 6 kinds of different concns as shown in Figure 1.
The adsorption effect of table 1 molecularly imprinted polymer to different concns Schuttgelb
Embodiment 3
Get aloe leaf or Aloe gel or beverage beverage homogenate 5g, be placed in 50ml centrifuge tube, add methyl alcohol 30ml, sonic oscillation 30min, centrifugal 10min at 20 ℃, rotating speed 3000r/min, suction filtration.Above-mentioned experimental procedure repeats 3 times, collects filtrate.Get respectively 3 parts of 5ml filtrates, add molecularly imprinted polymer in 10ml centrifuge tube, vibration 5h.Method by embodiment 1 is measured, and the results are shown in Table 2.
Decreasing ratio (%)=rhabarberone adsorptive capacity (μ mol)/rhabarberone actual content (μ mol)
The decreasing ratio of rhabarberone in table 2 actual sample
Above preferred embodiment is only for illustrating content of the present invention; in addition; the present invention also has other embodiments; in every case those skilled in the art are because of technology enlightenment involved in the present invention, and adopt to be equal to, replace or technical scheme that equivalent deformation mode forms all drops in protection scope of the present invention.
Claims (7)
1. the rhabarberone based on molecularly imprinted polymer removes a technology, it is characterized in that: comprise the steps:
(1) preparation of rhabarberone molecularly imprinted polymer: the rhabarberone standard substance that take a certain amount of higher degree, be dissolved in the acetone of 60 times of rhabarberone weight, with function monomer (1:4), linking agent (1:20), initiator (1:6) mixes, mixed solution supersound process 10min, nitrogen blows 15min, sealing, be placed in 60 ℃ of water-bath polyreaction 24h, pulverize, cross 100 mesh sieves, dry, be placed in beaker, the elutriant that adds 50 times of rhabarberone weight, ultrasonic extraction 30min, suction filtration, get filter residue and repeat said process, until detect under 429nm wavelength in elutriant without absorbing, filter residue after wash-out is placed in to baking oven, dry, obtain rhabarberone molecularly imprinted polymer,
(2) removing of rhabarberone molecularly imprinted polymer: get the gelating soln that contains rhabarberone, add above-mentioned molecularly imprinted polymer, concussion 5h, centrifugal, remove precipitation, supernatant liquor is the gelating soln that has removed rhabarberone.
2. a kind of rhabarberone based on molecularly imprinted polymer according to claim 1 removes technology, it is characterized in that: the purity of the rhabarberone standard substance of selecting in described step (1) is more than 98%.
3. a kind of rhabarberone based on molecularly imprinted polymer according to claim 1 removes technology, it is characterized in that: in described step (1), function monomer is selected methacrylic acid or acrylamide.
4. a kind of rhabarberone based on molecularly imprinted polymer according to claim 1 removes technology, it is characterized in that: in described step (1), linking agent is selected ethylene glycol dimethacrylate.
5. a kind of rhabarberone based on molecularly imprinted polymer according to claim 1 removes technology, it is characterized in that: in described step (1), initiator is selected Diisopropyl azodicarboxylate.
6. a kind of rhabarberone based on molecularly imprinted polymer according to claim 1 removes technology, it is characterized in that: the elutriant of selecting in described step (1) is methyl alcohol: acetic acid (8:2, volume ratio) solution.
7. a kind of rhabarberone based on molecularly imprinted polymer according to claim 1 removes technology, it is characterized in that: the technical process described in employing step 1, the decreasing ratio of rhabarberone is 99.50%.
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| CN201310498676.3A CN103554329A (en) | 2013-10-17 | 2013-10-17 | Molecularly imprinted polymer based aloe-emodin removal technology |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565483A (en) * | 2009-06-03 | 2009-10-28 | 江南大学 | Preparation method of bensulfuron methyl molecularly imprinted polymer and application thereof |
| CN101712731A (en) * | 2009-03-13 | 2010-05-26 | 河北理工大学 | Preparation and application of emodin molecular imprinted polymer |
| CN102485758A (en) * | 2010-12-03 | 2012-06-06 | 江南大学 | Glutathione molecular imprinting polymer, preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101712731A (en) * | 2009-03-13 | 2010-05-26 | 河北理工大学 | Preparation and application of emodin molecular imprinted polymer |
| CN101565483A (en) * | 2009-06-03 | 2009-10-28 | 江南大学 | Preparation method of bensulfuron methyl molecularly imprinted polymer and application thereof |
| CN102485758A (en) * | 2010-12-03 | 2012-06-06 | 江南大学 | Glutathione molecular imprinting polymer, preparation method and application thereof |
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Application publication date: 20140205 |