CN100556921C - A kind of preparation method of Stigmasterol molecular blotting polymer microsphere - Google Patents
A kind of preparation method of Stigmasterol molecular blotting polymer microsphere Download PDFInfo
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- CN100556921C CN100556921C CN 200710179795 CN200710179795A CN100556921C CN 100556921 C CN100556921 C CN 100556921C CN 200710179795 CN200710179795 CN 200710179795 CN 200710179795 A CN200710179795 A CN 200710179795A CN 100556921 C CN100556921 C CN 100556921C
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- stigmasterol
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- molecular blotting
- polymer microsphere
- blotting polymer
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Abstract
The invention discloses a kind of preparation method of Stigmasterol molecular blotting polymer microsphere.With Stigmasterol as microsphere, methyl methacrylate is a function monomer, Vinylstyrene is a linking agent, lime carbonate and sodium dodecyl sulfate mixture are dispersion agent, Sodium Persulfate is an initiator, and methyl alcohol (met.) is pore-creating agent, the Stigmasterol molecular blotting polymer microsphere for preparing, particle diameter is little and be evenly distributed, and Stigmasterol is shown special preferably absorption property.Enrichment from soya-bean oil, rapeseed oil deodorization distillate is gone out the highly purified plant sterol of single component in the present invention and the detection of Stigmasterol analysis on Content has great significance.
Description
Technical field
The invention belongs to a kind of preparation method of Stigmasterol molecular blotting polymer microsphere.
Background technology
Plant sterol and derivative thereof have the reduction serum cholesterol, anti-inflammatory, bring down a fever, antiulcer agent, pharmacological effect such as anticancer.Plant sterol content is abundant in the soybean, and the sterol that extraction separation comes out from soybean oil deodorizer distillate mainly comprises Stigmasterol, β-Gu Zaichun and brassicasterol.Because they are structurally similar, the physical properties difference is very little, sees three kinds of following sterol chemical structural formulas, is difficult to isolate the highly purified plant sterol of single component.
The chemical structural formula of three kinds of sterols
Summary of the invention
The purpose of this invention is to provide a kind of preparation method of Stigmasterol molecular blotting polymer microsphere of simple to operate, operation environment safety, the resulting polymers microspherulite diameter is little and be evenly distributed, and Stigmasterol is shown special preferably absorption property.
To achieve these goals, the present invention is by the following technical solutions:
A kind of preparation method of Stigmasterol molecular blotting polymer microsphere, the stirring and dissolving under 60～70 ℃ of conditions with Stigmasterol and methyl methacrylate; The warm water that adds 60～70 ℃ adds Vinylstyrene simultaneously and stirs; Add lime carbonate and sodium lauryl sulphate again, feed and change mechanical stirring into after nitrogen stirs 14min～16min; Add Sodium Persulfate and methyl alcohol, under 50～60 ℃ of conditions, stirred polyase 13 0～40 hour, get median size less than 100nm oyster white polymer microballoon; Polymer microballoon with preparation washs at last, and Stigmasterol content is lower than till the 0.001mg/L in elutriant, filters, dry Stigmasterol molecular blotting polymer microsphere at ambient temperature.The Stigmasterol molecular blotting polymer microsphere that this preparation method obtains, particle diameter is little and be evenly distributed, and Stigmasterol is shown special preferably absorption property.
There is the binding site of determining arrangement in the opening structure that the prepared molecularly imprinted polymer inside of the present invention has many solid shapes and size in the hole, microsphere is had memory and recognition function.Therefore can be used for separating with extracting and have only the different sterols material of side-chain radical.The present invention adopts the Stigmasterol molecularly imprinted polymer of suspension polymerization preparation that Stigmasterol is demonstrated stronger specific adsorption performance, and enrichment from soya-bean oil, rapeseed oil deodorization distillate is gone out the highly purified plant sterol of single component for this and the detection of Stigmasterol analysis on Content has great significance.
In the preparation method of Stigmasterol molecular blotting polymer microsphere of the present invention, Stigmasterol (stig.) is as microsphere, methyl methacrylate (MMA) is a function monomer, Vinylstyrene (VB) is a linking agent, lime carbonate and sodium lauryl sulphate (SDS) mixture is a dispersion agent, Sodium Persulfate is an initiator, and methyl alcohol (met.) is pore-creating agent.Wherein, adopt the purity of Stigmasterol to be higher than 95%, the purity of methyl methacrylate is 98%, and lime carbonate, Vinylstyrene, sodium lauryl sulphate, Sodium Persulfate, methyl alcohol are analytical pure.
In the preparation method of Stigmasterol molecular blotting polymer microsphere of the present invention, various amounts of components ratios are: Stigmasterol (stig.) 2.5g～3.5g: methyl methacrylate (MMA) 35ml～45ml: water consumption 150ml; Vinylstyrene (VB) 14mL～16mL: lime carbonate (CaCO
3) 3.5g～4.5g: sodium lauryl sulphate (SDS) 1.5g～2.5g: Sodium Persulfate (Na
2S
2O
8) 0.35mL～0.45mL: methyl alcohol (met.) 14ml～16ml.
In the preparation method of Stigmasterol molecular blotting polymer microsphere of the present invention, described polymer microballoon washs and adopts ethanol solution to wash under ultrasound condition.
Advantage of the present invention is:
The Stigmasterol molecular blotting polymer microsphere preparation method who provides among the present invention, simple to operate, operation environment safety, the resulting polymers particle diameter is little and be evenly distributed, and Stigmasterol is shown special preferably absorption property.Enrichment from soya-bean oil, rapeseed oil deodorization distillate is gone out the highly purified plant sterol of single component to the prepared polymer microballoon of the present invention and the detection of Stigmasterol analysis on Content has great significance.
Description of drawings
Fig. 1 is the Electronic Speculum picture of the Stigmasterol imprinted polymer of embodiments of the invention preparation.
Embodiment
Embodiment
The stirring and dissolving under 60～70 ℃ of conditions with 3g Stigmasterol (purity is higher than 95%) and 40ml methyl methacrylate (purity is 98%); Add the warm water of 60～70 ℃ of 150ml, add 15mL Vinylstyrene (analytical pure) simultaneously and stir fast; Add 4g lime carbonate (analytical pure) and 2g sodium lauryl sulphate (analytical pure) again, feed and change mechanical stirring into after nitrogen stirs 15min; Add 0.4mL Sodium Persulfate (analytical pure) and 15ml methyl alcohol (analytical pure), under 50～60 ℃ of conditions, stirred polyase 13 0～40 hour, get median size less than 100nm oyster white polymer microballoon.At last the polymer microballoon for preparing being placed ethanol solution is to wash under the 2.5Kw condition at ultrasonic power, Stigmasterol content is lower than till the 0.001mg/L in elutriant, filters, dry Stigmasterol molecular blotting polymer microsphere at ambient temperature.
The Stigmasterol imprinted polymer microballoon Electronic Speculum picture of embodiment preparation is seen Fig. 1, and its median size is 48 μ m, and particle diameter distribution width is 1.69; Adopt high performance liquid phase to show to adsorbing forward and backward Stigmasterol solution quality content analysis, this polymer microballoon to the loading capacity of Stigmasterol up to 1.2mg/L; When with the β-Gu Zaichun being the competition substrate, than about 1.75, and absorption property and special absorption property all show satisfactory stability to separation factors of Stigmasterol and two kinds of polymkeric substance of β-Gu Zaichun for it.
Claims (3)
1, a kind of preparation method of Stigmasterol molecular blotting polymer microsphere is characterized in that: the stirring and dissolving under 60～70 ℃ of conditions with Stigmasterol and methyl methacrylate; The warm water that adds 60～70 ℃ adds Vinylstyrene simultaneously and stirs; Add lime carbonate and sodium lauryl sulphate again, feed and change mechanical stirring into after nitrogen stirs 14min～16min; Add Sodium Persulfate and methyl alcohol, under 50～60 ℃ of conditions, stirred polyase 13 0～40 hour, get median size less than 100nm oyster white polymer microballoon; Polymer microballoon with preparation washs at last, Stigmasterol content is lower than till the 0.001mg/L in elutriant, filter, dry Stigmasterol molecular blotting polymer microsphere at ambient temperature, wherein various amounts of components ratios are: Stigmasterol 2.5g～3.5g; Methyl methacrylate 35mL～45mL; Water consumption 150mL; Vinylstyrene 14mL～16mL lime carbonate 3.5g～4.5g; Sodium lauryl sulphate 1.5g～2.5g; Sodium Persulfate 0.35mL～0.45mL; Methyl alcohol 14mL～16mL.
2, the preparation method of Stigmasterol molecular blotting polymer microsphere according to claim 1, it is characterized in that: wherein adopt the purity of Stigmasterol to be higher than 95%, the purity of methyl methacrylate is 98%, and lime carbonate, Vinylstyrene, sodium lauryl sulphate, Sodium Persulfate, methyl alcohol is analytical pure.
3, the preparation method of Stigmasterol molecular blotting polymer microsphere according to claim 1 and 2 is characterized in that, described polymer microballoon washs and adopts ethanol solution to wash under ultrasound condition.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200710179795 CN100556921C (en) | 2007-12-18 | 2007-12-18 | A kind of preparation method of Stigmasterol molecular blotting polymer microsphere |
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| CN 200710179795 CN100556921C (en) | 2007-12-18 | 2007-12-18 | A kind of preparation method of Stigmasterol molecular blotting polymer microsphere |
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| CN100556921C true CN100556921C (en) | 2009-11-04 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250285B (en) * | 2010-05-19 | 2012-11-21 | 中国科学院大连化学物理研究所 | Semi-covalent molecularly imprinted polymer used for selectivity separating phenols, preparation method thereof, and application thereof |
| IT201700066508A1 (en) * | 2017-06-15 | 2018-12-15 | Isagro Spa | SUSPENSIONS CONCENTRATED OF PHYTOSTEROLS AND RELATIVE PREPARATION PROCESS |
| CN108479729B (en) * | 2018-03-22 | 2020-08-28 | 河南科技学院 | Application of low-temperature liquid metal microspheres in preparation of adsorption separation analysis high-molecular porous material |
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