CN104910324A - Method for producing lincomycin molecularly imprinted polymer - Google Patents
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Abstract
The invention discloses a method for producing a lincomycin molecularly imprinted polymer. The method comprises producing a styrene monomer to obtain a polystyrene microsphere; uniformly dispersing the polystyrene microsphere and sodium dodecyl sulfate into ultrapure water; adding azodiisobutyronitrile, dibutyl phthalate and methylbenzene to be stirred and swelled for 20 to 24 hours; adding lincomycin, methylacrylic acid, ethyldiol methacrylate, sodium dodecyl sulfate, polyvinyl alcohol, octyl alcohol and chloroform into an obtained system after low temperature mixing to be stirred and swelled for 20 to 24 hours; adding a polyvinyl alcohol aqueous solution for temperature rise and a reaction and performing centrifugal separation, washing and drying to obtain a semi-finished molecularly imprinted polymer; cleaning the semi-finished molecularly imprinted polymer for 20 to 24 hours through a mixed solvent of methyl alcohol and acetic acid and performing centrifugation, washing and drying to obtain the lincomycin molecularly imprinted polymer. According to the method for producing the lincomycin molecularly imprinted polymer, the produced lincomycin molecularly imprinted polymer is a novel adsorbent with the specificity identification capability, the specificity is achieved in the adsorption process, the pertinency is high, and target molecules can be identified from a complex mixed system.
Description
Technical field
The present invention relates to functional high molecule material preparing technical field, relate to a kind of method preparing lincomycin molecularly imprinted polymer.
Background technology
Lincomycin is as a kind of microbiotic of high-efficiency broad spectrum, have that antibacterial ability is strong, the advantage such as convenient drug administration (as can oral, intravenous drip or intramuscular injection), application in medical treatment is comparatively general, can be used for treating the infection caused by gram-positive microorganism, inflammation or septicemia etc.In addition, lincomycin also has very strong restraining effect for livestock, poultry pathogenic microorganism, is thus also used in feed as veterinary drug.Because it is applied widely, Application comparison is general, therefore prepare a kind of sorbent material lincomycin to selective adsorption capacity, for the Separation & Purification of lincomycin in industrial production, and environment, in food inspection the enrichment of lincomycin have very important meaning with analyzing.
Common material collection, the method for separation have extraction process, absorption method, membrane sepn etc., wherein adsorption method of separation is comparatively easy, economical, but it is poor that traditional sorbent material has selectivity, do not possess the weak points such as specificity adsorptive power, the sorbing material therefore preparing highly selective has problem to be solved in adsorption separation technology.In this case, molecularly imprinted polymer obtains and pays close attention to widely.Molecularly imprinted polymer is a kind of novel polymer adsorbing material, compared with traditional sorbent material, it contains the hole that a lot of shape and size and material upon adsorption match, have again in these holes and can interact into the binding site of key with the particular functional group of material upon adsorption, therefore it has certain memory and recognition capability for target molecule upon adsorption, can realize the high-selectivity adsorption to this target molecule.The method preparing molecularly imprinted polymer has multiple, such as mass polymerization, in-situ polymerization, suspension polymerization, letex polymerization, precipitation polymerization, swollen-state polymerization etc., wherein swollen-state polymerization method can obtain regular shape, presents the molecularly imprinted polymer of uniform-spherical, such molecularly imprinted polymer specific surface area is large, high adsorption capacity, loading capacity is high, and size is moderate, higher resistance to flow can not be produced, compare the separation and consentration being applicable to lincomycin in actual production.
Summary of the invention
The invention reside in and provide a kind of swelling method of two steps to prepare lincomycin molecularly imprinted polymer.Have the new adsorbent of specific recognition capability, adsorption process has specificity, with strong points, can identify target molecule from the mixed system of complexity.This sorbent material is applied to fractionation by adsorption operation, compared with conventional adsorbent, has obvious selectivity and better adsorptive power.
For achieving the above object, adopt technical scheme as follows:
Prepare the method for lincomycin molecularly imprinted polymer, comprise the following steps:
1) styrene monomer is prepared polystyrene microsphere;
2) polystyrene microsphere and sodium lauryl sulphate evenly spread in ultrapure water; Add Diisopropyl azodicarboxylate, dibutyl phthalate and toluene again and stir swelling 20 ~ 24h;
3) step 2 is added after getting template molecule lincomycin, methacrylic acid, Ethylene glycol dimethacrylate, sodium lauryl sulphate, polyvinyl alcohol, octanol and chloroform low-temperature mixed) stir swelling 20 ~ 24h in gained system;
4) add polyvinyl alcohol water solution be warming up to 60 ~ 70 DEG C again and react 20 ~ 24h, centrifugation, washing drying obtain work in-process molecularly imprinted polymer;
5) work in-process molecularly imprinted polymer is cleaned 20 ~ 24h with the mixed solvent of methyl alcohol and acetic acid, centrifugal, washing, dry, obtain final finished product molecularly imprinted polymer.
By such scheme, step 1) in polystyrene microsphere preparation process as follows:
Styrene monomer is mixed with dehydrated alcohol, and add polyvinylpyrrolidone and Diisopropyl azodicarboxylate, the volume ratio wherein controlling vinylbenzene and ethanol is 1:(1 ~ 1.4), the mass ratio of Diisopropyl azodicarboxylate and polyvinylpyrrolidone is 1:(5 ~ 7.5); Mixed solution is 60 ~ 70 DEG C of stirring reaction 20 ~ 24h under the condition of isolated air, and separation, drying obtain finished product polystyrene microsphere.
By such scheme, step 2) in the mass ratio of polystyrene microsphere and sodium lauryl sulphate be (4 ~ 5): 1; The mass ratio of Diisopropyl azodicarboxylate, dibutyl phthalate, toluene is 1:(5.2 ~ 6.3): (8.7 ~ 9.6).
By such scheme, step 3) in lincomycin, methacrylic acid, Ethylene glycol dimethacrylate amount of substance ratio be 1:(4 ~ 6): (20 ~ 25); Polyvinyl alcohol, sodium lauryl sulphate mass ratio are 1:(4 ~ 5); Octanol and chloroform volume ratio are (5 ~ 7): (9 ~ 10).
The preparation of molecularly imprinted polymer of the present invention adopts Two-step seed swelling method, and the polymer specific surface area that this method obtains is high, and regular shape, is comparatively applicable to industrial production.First general polymer is prepared as swelling necessary kind of ball, the molecularly imprinted polymer that obtained particle diameter is larger again on this basis.
With the monomer of vinylbenzene as polyreaction, in etoh solvent, carry out thermal-initiated polymerization by Diisopropyl azodicarboxylate; Wherein polyvinylpyrrolidone is as dispersion agent, polystyrene dispersion can be formed single bead, can not accumulate to and form large bulk polymer together.
Polystyrene microsphere carries out swelling under the effect of swelling agent dibutyl phthalate, and particle diameter expands, and forms cell texture by the effect with pore-creating agent toluene; Now, template molecule lincomycin, function monomer, linking agent Ethylene glycol dimethacrylate are under the effect of polyethylene of dispersing agent alcohol, evenly be attached to the surface, hole of vesicular polystyrene microsphere, again by the effect of initiator Diisopropyl azodicarboxylate, polymerization forms high-crosslinking-degree polymkeric substance, and be distributed in microballoon hole, form space opening structure lincomycin to specific recognition performance, after wash-out removing lincomycin, this molecularly imprinted polymer just can identify and adsorb lincomycin molecule from the mixed system of complexity.
The invention has the beneficial effects as follows:
Obtained molecularly imprinted polymer is a kind of new adsorbent with specific recognition capability, and adsorption process has specificity, with strong points, can identify target molecule from the mixed system of complexity.
The present invention prepares molecularly imprinted polymer and is applied to fractionation by adsorption operation as sorbent material, compared with conventional adsorbent, has obvious selectivity and better adsorptive power.
Accompanying drawing explanation
Fig. 1: lincomycin molecularly imprinted polymer scanning electron microscope (SEM) photograph prepared by embodiment 1;
Fig. 2: lincomycin molecularly imprinted polymer infrared spectrogram prepared by embodiment 1;
Fig. 3: molecularly imprinted polymer loading capacity obtained in embodiment 1,2,3 is with the change of concentration;
Fig. 4: molecularly imprinted polymer loading capacity obtained in embodiment 1,2,3 over time;
Embodiment
Following examples explain technical scheme of the present invention further, but not as limiting the scope of the invention.
The process that the present invention prepares lincomycin molecularly imprinted polymer is as follows:
1) styrene monomer is mixed with dehydrated alcohol, and add polyvinylpyrrolidone and Diisopropyl azodicarboxylate, the volume ratio wherein controlling vinylbenzene and ethanol is 1:(1 ~ 1.4), the mass ratio of Diisopropyl azodicarboxylate and polyvinylpyrrolidone is 1:(5 ~ 7.5); 60 ~ 70 DEG C of stirring reaction 20 ~ 24h under the condition of isolated air, separation, drying obtain finished product polystyrene microsphere;
2) step 1 is got) polystyrene microsphere and sodium lauryl sulphate evenly spread in ultrapure water, and stir swelling, wherein the mass ratio of polystyrene microsphere and sodium lauryl sulphate is (4 ~ 5): 1; Add Diisopropyl azodicarboxylate, dibutyl phthalate and toluene again and stir swelling 20 ~ 24h, wherein the mass ratio of Diisopropyl azodicarboxylate, dibutyl phthalate, toluene is 1:(5.2 ~ 6.3): (8.7 ~ 9.6);
3) get template molecule lincomycin, methacrylic acid, Ethylene glycol dimethacrylate, sodium lauryl sulphate, polyvinyl alcohol, octanol and chloroform low-temperature mixed evenly after add in said apparatus, proceed stirring 20 ~ 24h, wherein Control architecture molecule, function monomer, the ratio of linking agent three amount of substance is 1:(4 ~ 6): (20 ~ 25), the mass ratio of dispersion agent and emulsifying agent is 1:(4 ~ 5), pore-creating agent volume ratio is (5 ~ 7): (9 ~ 10).
4) lincomycin molecularly imprinted polymer is prepared in thermal-initiated polymerization
Getting polyethylene of dispersing agent alcohol is dissolved in ultrapure water, and wherein controlling polyvinyl alcohol water solution concentration is 8 ~ 10g/l.This system adds in above-mentioned reaction unit, then is warming up to 60 ~ 70 DEG C and reacts 20 ~ 24h, obtains molecularly imprinted polymer;
5) removal of template molecule
By obtained imprinted polymer centrifugation, after washing drying, it is cleaned 20 ~ 24h with the mixed solvent of methyl alcohol and acetic acid, then with pure methyl alcohol and ultrapure water centrifuge washing, drying repeatedly, obtains final finished product molecularly imprinted polymer.
Embodiment 1
Mixed with dehydrated alcohol by styrene monomer, and add polyethylene of dispersing agent pyrrolidone and draw Diisopropyl azodicarboxylate, the consumption wherein controlling vinylbenzene and ethanol is respectively 70ml, and polyvinylpyrrolidone consumption is 1.5g, and the consumption of Diisopropyl azodicarboxylate is 0.3g.Add in reaction unit after above each material is mixed in low temperature environment, under the condition of isolated air, be heated to 70 DEG C of stirring reaction 20h, after the polymkeric substance separation drying of acquisition, obtain finished product polystyrene microsphere.
Get finished product polystyrene microsphere and sodium lauryl sulphate joins in ultrapure water, the consumption wherein controlling polystyrene microsphere is 1.0g, and the consumption of sodium lauryl sulphate is 0.2g, and ultrapure water consumption is 30ml.Add in reaction unit after this system is fully mixed and stir, get Diisopropyl azodicarboxylate simultaneously, dibutyl phthalate and toluene join in ultrapure water, the consumption wherein controlling dibutyl phthalate is 0.52g, the consumption of toluene is 0.87g, the consumption of Diisopropyl azodicarboxylate is 0.1g, and ultrapure water consumption is 25ml.Add in said apparatus after these materials are mixed under low temperature environment, the swelling 20h of Keep agitation.
Get template molecule lincomycin, function monomer methacrylic acid, linking agent Ethylene glycol dimethacrylate, dispersion agent sodium lauryl sulphate, polyvinyl alcohol, solvents octanol and chloroform, join in ultrapure water, wherein controlling lincomycin consumption is 1mmol, methacrylic acid consumption 6mmol, the consumption of Ethylene glycol dimethacrylate is 25mmol, and the consumption of sodium lauryl sulphate is 0.1g, polyvinyl alcohol consumption is 0.4g, octanol consumption is 5ml, and chloroform consumption is 10ml, and ultrapure water consumption is 40ml.Add in step 2 device after these materials are mixed under low temperature environment, proceed to stir 20h;
Getting polyvinyl alcohol is dissolved in ultrapure water, and wherein controlling polyvinyl alcohol consumption is 0.2g, and ultrapure water consumption is 20ml.By in the device that adds after this system Homogeneous phase mixing in step 2, under the condition of isolated air, be heated to 70 DEG C of polyreaction 20h, obtain molecularly imprinted polymer;
By obtained imprinted polymer centrifugation, 3 times are washed respectively with methyl alcohol and ultrapure water, after vacuum-drying, be placed on again in apparatus,Soxhlet's, 24h is cleaned with the mixed solvent of methyl alcohol and acetic acid, again with pure washed with methanol 5h, subsequently with ultrapure water centrifuge washing 3 times repeatedly, obtain final finished product molecularly imprinted polymer.
It is specifically intended that, non-molecularly imprinted polymer used in contrast, except not adding template molecule lincomycin, and do not exist beyond elution action, other making method is identical for the method for lincomycin molecularly imprinted polymer with above-mentioned two step swollen-state polymerization legal systems.
Fig. 1 is the lincomycin molecularly imprinted polymer scanning electron microscope (SEM) photograph of preparation in embodiment 1, comprises the appearance structure of single polymer microballoon and the concrete form of microsphere surface.As can be seen from the figure, molecularly imprinted polymer presents uniform-spherical, its diameter is 17 ~ 18 μm, a large amount of hole being of a size of submicron order is there is at polymer surfaces, the sizes and shape in these holes can match each other with lincomycin molecule, realizes the high-selectivity adsorption to lincomycin.
Fig. 2 is the infrared spectrogram of embodiment 1, comprises the infrared spectrogram of function monomer methacrylic acid a, linking agent Ethylene glycol dimethacrylate b and lincomycin molecularly imprinted polymer c.1637cm is shown in methacrylic acid spectrogram
-1the peak at place is carbon-carbon double bond stretching vibration peak, 1718cm
-1the peak that place occurs is the stretching vibration peak of carbonyl; 1637cm is shown in Ethylene glycol dimethacrylate spectrogram
-1the peak at place is the stretching vibration peak of carbon-carbon double bond, 1720cm
-1place is the stretching vibration peak of carbonyl, 1150cm
-1the peak at place is the stretching vibration peak of carbon-oxygen bond; And in polymer spectra figure, 1637cm
-1the carbon-carbon double bond stretching vibration peak at place obviously reduces, and shows that function monomer and linking agent have carried out abundant polymerization.3400cm
-1place occurs that wider peak is the stretching vibration peak of hydroxyl, 1720cm
-1the peak that place occurs is the stretching vibration peak of carbonyl, and what these two peaks represented is can with the hydroxyl of template molecularity and carbonyl group in molecularly imprinted polymer.
Embodiment 2
Styrene monomer is mixed with dehydrated alcohol, and add polyethylene of dispersing agent pyrrolidone and initiator Diisopropyl azodicarboxylate, the consumption wherein controlling vinylbenzene and ethanol is respectively 60ml, 70ml, and polyvinylpyrrolidone consumption is 1.2g, and the consumption of Diisopropyl azodicarboxylate is 0.2g.Add in reaction unit after above each material is mixed in low temperature environment, under the condition of isolated air, be heated to 60 DEG C of stirring reaction 24h, after the polymkeric substance separation drying of acquisition, obtain finished product polystyrene microsphere.
Get finished product polystyrene microsphere and sodium lauryl sulphate joins in ultrapure water, the consumption wherein controlling polystyrene microsphere is 0.8g, and the consumption of sodium lauryl sulphate is 0.2g, and ultrapure water consumption is 30ml.Add in reaction unit after this system is fully mixed and stir, get Diisopropyl azodicarboxylate simultaneously, dibutyl phthalate and toluene join in ultrapure water, the consumption wherein controlling dibutyl phthalate is 0.52g, the consumption of toluene is 0.96g, the consumption of Diisopropyl azodicarboxylate is 0.1g, and ultrapure water consumption is 23ml.Add in said apparatus after these materials are mixed under low temperature environment, the swelling 24h of Keep agitation.
Get template molecule lincomycin, function monomer methacrylic acid, linking agent Ethylene glycol dimethacrylate, dispersion agent sodium lauryl sulphate, polyvinyl alcohol, solvents octanol and chloroform, join in ultrapure water, wherein controlling lincomycin consumption is 1mmol, methacrylic acid consumption 4mmol, the consumption of Ethylene glycol dimethacrylate is 20mmol, and the consumption of sodium lauryl sulphate is 0.1g, polyvinyl alcohol consumption is 0.5g, octanol consumption is 7ml, and chloroform consumption is 10ml, and ultrapure water consumption is 37ml.Add in step 2 device after these materials are mixed under low temperature environment, proceed to stir 24h;
Getting polyvinyl alcohol is dissolved in ultrapure water, and wherein controlling polyvinyl alcohol consumption is 0.2g, and ultrapure water consumption is 20ml.By in the device that adds after this system Homogeneous phase mixing in step 2, under the condition of isolated air, be heated to 60 DEG C of polyreaction 24h, obtain molecularly imprinted polymer;
By obtained imprinted polymer centrifugation, 3 times are washed respectively with methyl alcohol and ultrapure water, after vacuum-drying, be placed on again in apparatus,Soxhlet's, 23h is cleaned with the mixed solvent of methyl alcohol and acetic acid, again with pure washed with methanol 4h, subsequently with ultrapure water centrifuge washing 3 times repeatedly, obtain final finished product molecularly imprinted polymer.
It is specifically intended that, non-molecularly imprinted polymer used in contrast, except not adding template molecule lincomycin, and do not exist beyond elution action, other making method is identical for the method for lincomycin molecularly imprinted polymer with above-mentioned two step swollen-state polymerization legal systems.Binding performance of molecular imprinted polymers the results are shown in Figure 3, Fig. 4.
Embodiment 3
Styrene monomer is mixed with dehydrated alcohol, and add polyethylene of dispersing agent pyrrolidone and initiator Diisopropyl azodicarboxylate, the consumption wherein controlling vinylbenzene and ethanol is respectively 50ml, 70ml, and polyvinylpyrrolidone consumption is 1.5g, and the consumption of Diisopropyl azodicarboxylate is 0.2g.Add in reaction unit after above each material is mixed in low temperature environment, under the condition of isolated air, be heated to 60 DEG C of stirring reaction 22h, after the polymkeric substance separation drying of acquisition, obtain finished product polystyrene microsphere.
Get finished product polystyrene microsphere and sodium lauryl sulphate joins in ultrapure water, the consumption wherein controlling polystyrene microsphere is 0.9g, and the consumption of sodium lauryl sulphate is 0.2g, and ultrapure water consumption is 30ml.Add in reaction unit after this system is fully mixed and stir, get Diisopropyl azodicarboxylate simultaneously, dibutyl phthalate and toluene join in ultrapure water, the consumption wherein controlling dibutyl phthalate is 0.63g, the consumption of toluene is 0.87g, the consumption of Diisopropyl azodicarboxylate is 0.1g, and ultrapure water consumption is 24ml.Add in said apparatus after these materials are mixed under low temperature environment, the swelling 22h of Keep agitation.
Get template molecule lincomycin, function monomer methacrylic acid, linking agent Ethylene glycol dimethacrylate, dispersion agent sodium lauryl sulphate, polyvinyl alcohol, solvents octanol and chloroform, join in ultrapure water, wherein controlling lincomycin consumption is 1mmol, methacrylic acid consumption 5mmol, the consumption of Ethylene glycol dimethacrylate is 22mmol, and the consumption of sodium lauryl sulphate is 0.1g, polyvinyl alcohol consumption is 0.4g, octanol consumption is 5ml, and chloroform consumption is 9ml, and ultrapure water consumption is 39ml.Add in step 2 device after these materials are mixed under low temperature environment, proceed to stir 22h;
Getting polyvinyl alcohol is dissolved in ultrapure water, and wherein controlling polyvinyl alcohol consumption is 0.2g, and ultrapure water consumption is 20ml.By in the device that adds after this system Homogeneous phase mixing in step 2, under the condition of isolated air, be heated to 70 DEG C of polyreaction 22h, obtain molecularly imprinted polymer;
By obtained imprinted polymer centrifugation, 3 times are washed respectively with methyl alcohol and ultrapure water, after vacuum-drying, be placed on again in apparatus,Soxhlet's, 20h is cleaned with the mixed solvent of methyl alcohol and acetic acid, again with pure washed with methanol 3h, subsequently with ultrapure water centrifuge washing 3 times repeatedly, obtain final finished product molecularly imprinted polymer.
It is specifically intended that, non-molecularly imprinted polymer used in contrast, except not adding template molecule lincomycin, and do not exist beyond elution action, other making method is identical for the method for lincomycin molecularly imprinted polymer with above-mentioned two step swollen-state polymerization legal systems.Binding performance of molecular imprinted polymers the results are shown in Figure 3, Fig. 4.
Shown in the measuring method of absorption property is specific as follows:
1. the mensuration of loading capacity
Get certain density lincomycin solution 10ml, add the molecularly imprinted polymer of 50mg, sealing be placed in 25 DEG C of constant temperature oscillation casees, after abundant vibration absorption 5h, get 1ml solution 0.45 μm of mocromembrane filter and dry, after methanol constant volume, measure the content of wherein lincomycin with high performance liquid chromatograph, and adopt following formula to calculate loading capacity Q according to result
e:
In formula, C
0with C
erepresent the concentration of lincomycin in solution before and after absorption respectively, V represents the volume of solution used, and m represents the quality of added molecularly imprinted polymer.
2. the mensuration of adsorption rate
Getting concentration is respectively 2mmol/L lincomycin solution 10ml, be divided into some groups and add the molecularly imprinted polymer of 50mg, sealing be placed in 25 DEG C of constant temperature oscillation casees, vibration absorption, in order every 20min, gets the solution 1mL in single Erlenmeyer flask, filter with 0.45 μm of mocromembrane and dry, after methanol constant volume, measure the content of wherein lincomycin with high performance liquid chromatograph, and adopt following formula to calculate not adsorptive capacity Q in the same time according to result
t:
In formula, C
0with C
trepresent the concentration with lincomycin in each time point solution before adsorbing respectively, V represents the volume of solution used, and m represents the quality of added molecularly imprinted polymer.
A in Fig. 3, b, c curve to represent in embodiment 1,2,3 the obtained molecularly imprinted polymer loading capacity situation with change in concentration respectively, d, e, f curve to represent in embodiment 1,2,3 the obtained non-molecularly imprinted polymer loading capacity situation with change in concentration respectively.As can be seen from the figure, compare non-imprinted polymer, molecularly imprinted polymer is to the adsorptive capacity of lincomycin apparently higher than non-imprinted polymer, and gap is between the two more remarkable in higher concentrations.
In Fig. 4, a, b, c curve represents molecularly imprinted polymer adsorptive capacity trend over time obtained in embodiment 1,2,3 respectively.As can be seen from the figure, the absorption starting stage, the adsorptive capacity of polymkeric substance is a process increased fast, in conjunction with speed, and reaches adsorption equilibrium after 90min.
Claims (4)
1. prepare the method for lincomycin molecularly imprinted polymer, comprise the following steps:
1) styrene monomer is prepared polystyrene microsphere;
2) polystyrene microsphere and sodium lauryl sulphate evenly spread in ultrapure water; Add Diisopropyl azodicarboxylate, dibutyl phthalate and toluene again and stir swelling 20 ~ 24h;
3) step 2 is added after getting template molecule lincomycin, methacrylic acid, Ethylene glycol dimethacrylate, sodium lauryl sulphate, polyvinyl alcohol, octanol and chloroform low-temperature mixed) stir swelling 20 ~ 24h in gained system;
4) add polyvinyl alcohol water solution be warming up to 60 ~ 70 DEG C again and react 20 ~ 24h, centrifugation, washing drying obtain work in-process molecularly imprinted polymer;
5) work in-process molecularly imprinted polymer is cleaned 20 ~ 24h with the mixed solvent of methyl alcohol and acetic acid, centrifugal, washing, dry, obtain final finished product molecularly imprinted polymer.
2. prepare the method for lincomycin molecularly imprinted polymer as claimed in claim 1, it is characterized in that step 1) in polystyrene microsphere preparation process as follows:
Styrene monomer is mixed with dehydrated alcohol, and add polyvinylpyrrolidone and Diisopropyl azodicarboxylate, the volume ratio wherein controlling vinylbenzene and ethanol is 1:(1 ~ 1.4), the mass ratio of Diisopropyl azodicarboxylate and polyvinylpyrrolidone is 1:(5 ~ 7.5); Mixed solution is 60 ~ 70 DEG C of stirring reaction 20 ~ 24h under the condition of isolated air, and separation, drying obtain finished product polystyrene microsphere.
3. prepare the method for lincomycin molecularly imprinted polymer as claimed in claim 1, it is characterized in that step 2) in the mass ratio of polystyrene microsphere and sodium lauryl sulphate be (4 ~ 5): 1; The mass ratio of Diisopropyl azodicarboxylate, dibutyl phthalate, toluene is 1:(5.2 ~ 6.3): (8.7 ~ 9.6).
4. prepare the method for lincomycin molecularly imprinted polymer as claimed in claim 1, it is characterized in that step 3) in lincomycin, methacrylic acid, Ethylene glycol dimethacrylate amount of substance ratio be 1:(4 ~ 6): (20 ~ 25); Polyvinyl alcohol, sodium lauryl sulphate mass ratio are 1:(4 ~ 5); Octanol and chloroform volume ratio are (5 ~ 7): (9 ~ 10).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110041556A (en) * | 2019-03-06 | 2019-07-23 | 华南农业大学 | A kind of decis molecularly imprinted polymer and its preparation method and application |
| CN110193290A (en) * | 2019-05-30 | 2019-09-03 | 江苏大学 | A kind of preparation method and application based on click chemistry trace lincomycin molecular compound film |
| CN110818836A (en) * | 2019-11-21 | 2020-02-21 | 武汉工程大学 | Vitamin E molecularly imprinted polymer, two-step swelling preparation method and application thereof |
| CN111359677A (en) * | 2020-03-13 | 2020-07-03 | 湖北文理学院 | Preparation method of photoelectric catalyst for selectively degrading dibutyl phthalate |
| CN113996275A (en) * | 2021-11-23 | 2022-02-01 | 东北林业大学 | Preparation of camptothecin molecularly imprinted polymer and method for separating and purifying camptothecin from camptotheca acuminata fruits |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101648981A (en) * | 2009-09-22 | 2010-02-17 | 南阳普康药业有限公司 | Extraction and refinement process of lincomycin |
| CN102746348A (en) * | 2011-04-19 | 2012-10-24 | 上海医药工业研究院 | Method for separation of lincomycin |
| CN104356179A (en) * | 2014-10-15 | 2015-02-18 | 江西国药有限责任公司 | Lincomycin hydrochloride purification technology |
-
2015
- 2015-07-03 CN CN201510388347.2A patent/CN104910324A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101648981A (en) * | 2009-09-22 | 2010-02-17 | 南阳普康药业有限公司 | Extraction and refinement process of lincomycin |
| CN102746348A (en) * | 2011-04-19 | 2012-10-24 | 上海医药工业研究院 | Method for separation of lincomycin |
| CN104356179A (en) * | 2014-10-15 | 2015-02-18 | 江西国药有限责任公司 | Lincomycin hydrochloride purification technology |
Non-Patent Citations (1)
| Title |
|---|
| 张佑红 等: ""分子印迹聚合物对林可霉素的静态吸附"", 《武汉工程大学学报》 * |
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| CN110041556A (en) * | 2019-03-06 | 2019-07-23 | 华南农业大学 | A kind of decis molecularly imprinted polymer and its preparation method and application |
| CN110193290A (en) * | 2019-05-30 | 2019-09-03 | 江苏大学 | A kind of preparation method and application based on click chemistry trace lincomycin molecular compound film |
| CN110818836A (en) * | 2019-11-21 | 2020-02-21 | 武汉工程大学 | Vitamin E molecularly imprinted polymer, two-step swelling preparation method and application thereof |
| CN111359677A (en) * | 2020-03-13 | 2020-07-03 | 湖北文理学院 | Preparation method of photoelectric catalyst for selectively degrading dibutyl phthalate |
| CN111359677B (en) * | 2020-03-13 | 2023-03-28 | 湖北文理学院 | Preparation method of photoelectric catalyst for selectively degrading dibutyl phthalate |
| CN113996275A (en) * | 2021-11-23 | 2022-02-01 | 东北林业大学 | Preparation of camptothecin molecularly imprinted polymer and method for separating and purifying camptothecin from camptotheca acuminata fruits |
| CN113996275B (en) * | 2021-11-23 | 2024-04-19 | 东北林业大学 | Preparation of camptothecine molecularly imprinted polymer and method for separating and purifying camptothecine in camptotheca acuminata fruits |
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Application publication date: 20150916 |