CN101041125A - The preparation and application of poly(glycidylmethacrylate-co-ethylene dimethacrylate) inverted medium and compatible medium - Google Patents
The preparation and application of poly(glycidylmethacrylate-co-ethylene dimethacrylate) inverted medium and compatible medium Download PDFInfo
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- CN101041125A CN101041125A CN 200610041941 CN200610041941A CN101041125A CN 101041125 A CN101041125 A CN 101041125A CN 200610041941 CN200610041941 CN 200610041941 CN 200610041941 A CN200610041941 A CN 200610041941A CN 101041125 A CN101041125 A CN 101041125A
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Abstract
The invention relates to a preparing method for C18-PGMA, C18-PGMA reversed-phase medium and iminodiacetic acid-PGMA metal chelating medium by chemical reaction, in which polyvinyl glycidyl methacrylate microsphere is used as matrix. C18-PGMA and C18-PGMA reversed-phase medium can eliminate DTT and bhc pesticide residue in effect. The iminodiacetic acid-PGMA metal chelating medium can eliminate Hg and Pb harmful heavy metal ion.
Description
The preparation of poly (glycidylmethacrylate--co-ethylene dimethacrylate) inverted medium and affinity media
The present invention relates to a kind of preparation method who uses poly (glycidylmethacrylate--co-ethylene dimethacrylate) (PGMA) microballoon as the inverted medium and the metal-chelating medium of matrix.
Use PGMA to have very superior performance as all kinds of chromatographic isolation aspect as the matrix of separating medium.
At present, in the separation of natural products and relevant chemical products, people mainly use the separating medium of silica gel as matrix, are that the matrix medium accounts for more than 70% of output aggregate use amount with C18 and C8 silica gel wherein.But silica matrix product disadvantage is that the pH scope of application is narrow, and between 6-9, and many separating substances scopes are outside this pH scope.People attempt to find better matrix to replace the silica matrix product always.Organic microballoon matrix has had effect preferably because the pH scope of application can reach 2-13 as replacing silica gel product.But the hydrophobicity of organic microballoon substrate products is stronger, and biocompatibility is relatively poor, also defines its certain applications.People begin target lock-on to make organic microballoon have better biocompatibility aspect the transformation of organic microballoon.PGMA is a hydrophilic organic polymer microballoon, and it not only has the characteristics of organic microballoon but also have good biological compatibility, can use in the scope of pH2-13, the shortcoming that to have overcome silica gel and other nonpolar microballoons be substrate products.
Yu Xiao, Zhao Rui, analytical chemistry, 2000,28 (5), 544-548.Use the PGMA microballoon as matrix, utilize the reduction ammonia process that heparin is connected on the PGMA microballoon, prepared heparin-PGMA affinity media, be used for the separation and purification of antithrombase and human serum albumins, obtained good separating effect.
The present invention connects octadecyl (C18), eight alkyl (C8), iminodiacetic acid (IDA) to the PGMA microballoon by chemical reaction, is prepared into C18-PGMA and C8-PGMA inverted medium and IDA-PGMA metallic chelate affinity medium.Above-mentioned three kinds of products and relevant preparation method do not see report in document and the relevant patent at home and abroad.
The present invention is intended to preparation, and both to have had the pH scope of application wide, has PGMA series C18-PGMA and the C8-PGMA inverted medium and the IDA-PGMA metallic chelate affinity medium of biocompatibility characteristics again.
1, C18-PGMA inverted medium preparation
The PGMA microballoon is positioned in the container, adds organic solvent and dilute, under stirring condition, add octadecyl trichlorosilane or chlorination octadecane, 60-90 ℃, reacted 2-10 hour, with an organic solvent clean, obtain the C18-PGMA new product.
2, C8-PGMA inverted medium preparation method
The PGMA microballoon is positioned in the container, adds organic solvent and dilute, under stirring condition, add eight alkyl trichlorosilanes or chlorination octane, 60-90 ℃, reacted 2-10 hour, with an organic solvent clean, obtain the C8-PGMA new product.
3, IDA-PGMA metal-chelating medium preparation
The PGMA microballoon is positioned in the container, adds the aqueous solution and dilute, under stirring condition, add iminodiacetic acid, 60-90 ℃, reacted 5-10 hour, use the aqueous solution to clean, obtain the IDA-PGMA new product.
The poly (glycidylmethacrylate--co-ethylene dimethacrylate) media applications
1.C18-PGMA and the C8-PGMA inverted medium is applied to remove residues of pesticides
C18-PGMA and C8-PGMA inverted medium are filled in the chromatographic column, the extract solution of solution that will contain agricultural chemicals and be DTT, BHC is by the methanol-water system, determine the retention time of DTT and BHC, DTT methanol content be 40-60% flow mutually in can effectively remove, clearance rate reaches more than 95%.BHC methanol content be 30-50% flow mutually in can effectively remove, clearance rate reaches more than 95%.
2.IDA-PGMA metallic chelate affinity medium is applied to remove heavy metal ion
The IDA-PGMA metallic chelate affinity medium is filled in the chromatographic column, the extract that will contain harmful heavy metal ion solution such as heavy metal Pb, Hg passes through chromatographic column, use the EDTA solution of pH9.0 to carry out can effectively removing in the wash-out, clearance rate reaches more than 95%.
By specific embodiment the present invention is carried out more detailed description below the specific embodiment:
Embodiment 1: take by weighing 10 gram PGMA microballoons, be positioned at the bottom of the garden in the flask, adding 200 milliliters of organic solvents of cyclohexane dilutes, under 300 rev/mins condition, stir, add octadecyl trichlorosilane 10 grams or chlorination octadecane 50 grams, 60-90 ℃, reacted 2-10 hour, use acetone, the aqueous solution to clean successively, obtain the C18-PGMA new product.
Embodiment 2: take by weighing 10 gram PGMA microballoons, be positioned at the bottom of the garden in the flask, adding 200 milliliters of organic solvents of cyclohexane dilutes, under 300 rev/mins condition, stir, add eight alkyl trichlorosilanes, 8 grams or chlorination normal octane 40 grams, 60-90 ℃, reacted 2-10 hour, use acetone, the aqueous solution to clean successively, obtain the C8-PGMA new product.
Embodiment 3: take by weighing 10 gram PGMA microballoons, be positioned at the bottom of the garden in the flask, adding 200 ml water solution dilutes, 40 milliliters of iminodiacetic acids that under 300 rev/mins condition, stir to add 0.5mol/L, 60-90 ℃, reacted 5-10 hour, and used the aqueous solution to clean, obtain the IDA-PGMA new product.
Embodiment 4: take by weighing 10 gram C18-PGMA or C8-PGMA inverted medium and fill in diameter 2.5cm * 25cm chromatographic column, the solution that will contain agricultural chemicals and be 100ppm DTT, BHC 50ppm passes through chromatographic column, mobile phase A solution is 90% water-10% methyl alcohol, and B solution is 10% water-90% methyl alcohol.A solution from 100% is 60 minutes to the 80%B solution gradient time, and flow velocity is 5ml/min, DTT methanol content be 40-60% flow mutually in can effectively remove, clearance rate reaches more than 95%.BHC methanol content be 30-50% flow mutually in can effectively remove, clearance rate reaches more than 95%.
Embodiment 5: the IDA-PGMA metallic chelate affinity medium is filled in diameter 1cm * 10cm chromatographic column, the extract that will contain harmful heavy metal ion solution such as heavy metal 100ppm Pb, Hg passes through chromatographic column, use pH9.0,0.2mol/L NaOAC solution equilibria, use the 0.2mol/L EDTA solution of pH9.0 to carry out effectively to remove in the wash-out, collect heavy metal ion, use atomic absorption spectrography (AAS) to detect, clearance rate reaches more than 95%.
Claims (6)
1. the preparation of poly (glycidylmethacrylate--co-ethylene dimethacrylate) inverted medium and affinity media and application, it is characterized in that with poly (glycidylmethacrylate--co-ethylene dimethacrylate) (PGMA) microballoon be matrix, connect octadecyl, eight alkyl, iminodiacetic acid (IDA) to the PGMA microballoon by chemical reaction, be prepared into C18-PGMA and C8-PGMA inverted medium and IDA-PGMA metallic chelate affinity medium.Chemical time is between 2-10 hour, and reaction temperature is 60-90 ℃.Its application characteristic is that C18-PGMA and C8-PGMA inverted medium can be applicable to remove the residues of pesticides aspect, and the IDA-PGMA metallic chelate affinity medium is mainly used in removes the harmful heavy metal ions.
2. the preparation of poly (glycidylmethacrylate--co-ethylene dimethacrylate) inverted medium according to claim 1 and affinity media, its preparation is characterized in that the chemical crosslinking reagent of C18-PGMA is octadecyl trichlorosilane or chlorination octadecane.
3. the preparation of poly (glycidylmethacrylate--co-ethylene dimethacrylate) inverted medium according to claim 1 and affinity media, its preparation is characterized in that the chemical crosslinking reagent of C8-PGMA is eight alkyl trichlorosilanes or chlorination normal octane.
4. the preparation of poly (glycidylmethacrylate--co-ethylene dimethacrylate) inverted medium according to claim 1 and affinity media, its preparation is characterized in that the chemical crosslinking reagent of IDA-PGMA is iminodiacetic acid.
5. poly (glycidylmethacrylate--co-ethylene dimethacrylate) inverted medium according to claim 1 and affinity media are used, and its application characteristic is that it is DTT, BHC that C18-PGMA and C8-PGMA inverted medium are applied to remove residues of pesticides aspect agricultural chemicals.
6. poly (glycidylmethacrylate--co-ethylene dimethacrylate) inverted medium according to claim 1 and affinity media are used, and its application characteristic is that the IDA-PGMA metallic chelate affinity medium can be applicable to remove harmful heavy metal ions such as heavy metal Pb, Hg.
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| CN 200610041941 CN101041125A (en) | 2006-03-20 | 2006-03-20 | The preparation and application of poly(glycidylmethacrylate-co-ethylene dimethacrylate) inverted medium and compatible medium |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500342A (en) * | 2011-10-19 | 2012-06-20 | 北京工业大学 | Method for loading organic microspheres on porous ceramic support |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500342A (en) * | 2011-10-19 | 2012-06-20 | 北京工业大学 | Method for loading organic microspheres on porous ceramic support |
| CN102500342B (en) * | 2011-10-19 | 2013-07-24 | 北京工业大学 | Method for loading organic microspheres on porous ceramic support |
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Open date: 20070926 |