CN1987453A - High molecular type reverse chromatography fixing phase and its preparing method - Google Patents
High molecular type reverse chromatography fixing phase and its preparing method Download PDFInfo
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Abstract
The invention is especially related to fixed phase of reversed phase chromatography (FPRPC) in macromolecule type of a series of different chemical constitution, and preparation method. Possessing macromolecule micro beads in regular spherical porous type, the disclosed FPRPC in macromolecule type possesses basic property of FPRPC. Using the disclosed FPRPC to carry out verification of chromatographic separation indicates that when macromolecule micro beads in porous type acts as FPRPC, pore structure is steady; under condition of compression elution, micro beads does not break up; adsorption-desorption procedure is quick; comparing with chemical bond silicon ball fixed phase in same granularity, FPRPC possesses closed column performance and closed separation. The disclosed FPRPC is applicable to separating and purifying medical bulk drug, and natural drug as well as applicable to enriching and preparing trace quantity substance in biologic and samples.
Description
Technical field
The present invention relates to class reverse-phase chromatography stationary phase and preparation method thereof, particularly a series of different chemical structures high molecular type reverse chromatography stationary phase and preparation method thereof.
Background technology
The reversed phase chromatography separation method is based on solute, a kind of chromatogram mode that the hydrophobic effect between polarity moving phase and non-polar stationary phase surface is set up.This is the widest a kind of clastotype of application surface in high performance liquid chromatography.In pharmaceuticals, most product analyses are to finish with this method, obtain very widespread use at agricultural, medicine, bioengineering, food and environmental science.Numerous organic compounds relevant with the human lives can separate and prepare with reversed phase chromatography.The reverse-phase chromatography stationary phase is the heart of reversed phase chromatography, mostly be porous type chemical bonding alkyl silicon ball stationary phase greatly, for example C18-alkyl, C8 alkyl, C4 alkyl chemistry bonded silica ball stationary phase, also with phenyl, nitro, itrile group, propionitrile base chemical bonding silicon ball fix phase (Zou Hanfa, Zhang Wangkui, Lu Peizhang, " high performance liquid chromatography; Science Press ", calendar year 2001, P.7, P.141-160).As analyzing with the reverse-phase chromatography stationary phase is its granularity particulate group that narrow grade distributes in 0.01mm scope or 0.005mm scope or 0.003mm scope, and preparative chromatography uses its particle size range of chemical bond mould assembly reversed phase chromatography stationary phase at 0.02-0.045mm or in 0.045-0.070mm or 0.071-0.14mm scope.
The rod structure of chemical bonding silicon ball reverse-phase chromatography stationary phase is stable, column efficiency is high, and the filler physical strength is good in chromatographic process, separates favorable reproducibility, and under the condition that is not subjected to sample contamination, it has long serviceable life.It also is that several defectives are arranged then: (1) chemical stability limitation, can only in the PH2-9 scope, use, and can not regenerate with the solution of band strong acid or highly basic, once be subjected to sample contamination to be difficult to regeneration, thus influence its life-span; (2) its preparation requires expensive silicon etherifying reagent, causes the preparation process complicated condition, the production cost height, so price is expensive; (3) in preparation scale chemical bonding silicon ball stationary phase, often contain the residual silicon hydroxyl, easily produce irreversible adsorption, influence product yield.Therefore, above deficiency has limited chemical bonding silicon ball stationarity and has been extensive use of in the mass preparation chromatogram.
Summary of the invention
Purpose of the present invention is the deficiency that overcomes chemical bonding silicon ball bonded stationary phase, and it is raw material that a kind of usefulness chemical materials commonly used is provided, and the preparation method is simple, is easy to industrialized high molecular type reverse chromatography stationary phase and preparation method thereof.
An object of the present invention is to provide a kind of high molecular type reverse chromatography stationary phase
Another object of the present invention provides the preparation method of described high molecular type reverse chromatography stationary phase.
The objective of the invention is to be achieved through the following technical solutions:
A kind of high molecular type reverse chromatography stationary phase is characterized in that it being to be prepared from by the following method:
A is in crosslinking chemical, and the optional single activity double key compound of adding (or not adding) makes it to be made into polymerization single polymerization monomer, and wherein the weight ratio of crosslinking chemical and single activity double key compound is 100: 0-15: 85;
B, add inertia pore-foaming agent and radical initiator in the polymerization single polymerization monomer that the A step is made into, mix the composition oil phase, wherein the weight ratio of polymerization single polymerization monomer and inertia pore-foaming agent and radical initiator is 80: 20: 0.2-30: 70: 6;
C, add suspension stabilizer in the aqueous solution that contains 5-35% (weight) salting-out agents, the concentration that makes suspension stabilizer is 0.2-5% (weight), fully mixes being made into water;
The volume ratio of D, oil phase and water is 1: 1-1: 15, under high-speed stirred, make oil phase be distributed to aqueous phase fully and form particle diameter less than the little liquid pearl of 0.3mm, heat 60-100 ℃ and carry out free radical copolymerization, generate solid multipolymer microballon, leach microballon after reaction is finished, or/and the solvent wash method is removed impurity in pore-foaming agent and other microballon hole, obtain porous type macromolecule microballon with the way of distillation;
E, the porous type macromolecule microballon that obtains is carried out size grading, obtain the bead that the narrow grain of bead size each section in the 0.01-0.3mm scope distributes, its hole characteristic is: the specific surface area scope is 20-800m
2/ g; Cell size scope: 10-75%; Pore size distribution range: 20-1000A °, its outward appearance be bead size in the 0.01-0.3mm particle size range, the porous type macromolecule microballon of these narrow size-grade distribution can be respectively as the reverse-phase chromatography stationary phase.
Described crosslinking chemical comprises: divinylbenzene, the industry divinylbenzene, trivinyl toluene, divinyl dimethylbenzene, the methacrylate glycol ester, the methacrylate macrogol ester, itaconic acid diene propyl ester, the cyamelide triallyl ester, one or more potpourris in the cyanuric acid triallyl ester, preferably, described crosslinking chemical comprises:: divinylbenzene, the industry divinylbenzene, trivinyl toluene, divinyl dimethylbenzene, the methacrylate glycol ester, the methacrylate macrogol ester, more preferably, described crosslinking chemical comprises:, the industry divinylbenzene, the methacrylate macrogol ester.
Described single activity double key compound comprises: styrene, ethyl styrene, methyl styrene, methyl methacrylate, one or more potpourris in methyl acrylate, ethyl acrylate, butyl acrylate, vinyl cyanide, the methoxy acrylamide, preferably, described single activity double key compound comprises: styrene, ethyl styrene, methyl methacrylate, methyl acrylate, vinyl cyanide, more preferably, described single activity double key compound comprises: styrene, methyl acrylate.
Described inertia pore-foaming agent comprises: aliphatic hydrocarbon (＞C7), aromatic hydrocarbon, 120# industrial naptha, 200# industrial naptha, C4-C8 fatty alcohol, fatty ester (total carbon atom＞C6) and aliphatic ketone (＞one or more potpourris in C6), preferably, described inertia pore-foaming agent comprises: aliphatic hydrocarbon (＞C7), the C4-C8 fatty alcohol.
Described radical initiator is: dibenzoyl peroxide, azoisobutyronitrile, dilauroyl peroxide, and preferred, dibenzoyl peroxide, azoisobutyronitrile.
Described salting-out agents comprise: one or more potpourris in sodium chloride, lime chloride, phosphate, the sulfate.Preferably, described salting-out agents comprise: sodium chloride, sulfate.
Described suspension stabilizer comprises: one or more potpourris in polyvinyl alcohol (PVA), gelatin, carboxymethyl cellulose, the starch.Preferably, polyvinyl alcohol (PVA).
The preparation method of a kind of high molecular type reverse chromatography stationary phase of the present invention may further comprise the steps;
A is in crosslinking chemical, and the optional single activity double key compound of adding (or not adding) makes it to be made into polymerization single polymerization monomer;
B, in the polymerization single polymerization monomer that the A step is made into, add inertia pore-foaming agent and radical initiator, mix the composition oil phase;
C, in containing the aqueous solution of salting-out agents, add suspension stabilizer, fully mix being made into water;
D, under high-speed stirred, make oil phase be distributed to aqueous phase fully and form particle diameter less than the little liquid pearl of 0.3mm, heat 60-100 ℃ and carry out free radical copolymerization, generate solid multipolymer microballon, after finishing, reaction leaches microballon, or/and the solvent wash method is removed impurity in pore-foaming agent and other microballon hole, obtain porous type macromolecule microballon with the way of distillation, the particle size range of these microballons is 0.005-0.3mm;
E, the porous type macromolecule microballon that obtains is carried out size grading, obtain the bead of the narrow size-grade distribution of each section, the porous type macromolecule microballon of these narrow size-grade distribution can be respectively as the reverse-phase chromatography stationary phase.
High molecular type reverse chromatography stationary phase of the present invention is to have more regular spherical porous type macromolecule microballon, has the fundamental property of reverse-phase chromatography stationary phase.Through using high molecular type reverse chromatography stationary phase of the present invention to carry out the chromatographic resolution checking, show when these porous type macromolecule microballons are made the stationary phase of reverse-phase chromatography, its pore structure is stable, in separation the pressurization elution requirement under, these microballons are not broken, the absorption-desorption process is quick, with same particle sizes chemical bonding silicon ball stationary phase than close column efficiency and close degree of separation are arranged.They can use in the PH1-14 scope, and wherein a few class stationary phase can be used strong acid, strong base solution regeneration, and its chemical stability and column life are better than chemical bonding silicon ball stationary phase.High molecular type reverse chromatography stationary phase provided by the present invention can be used in mass preparation medical material medicine, and the separation of natural drug and purifying preparation also can be used for the enrichment and the preparation of micro substance in biological field and the environmental sample.They are the complementary goods in the mass preparation reverse-phase chromatography or the substitute of chemical bonding silicon ball stationary phase.
Embodiment
Below adopt embodiment to specify a kind of high molecular type reverse chromatography stationary phase of the present invention and preparation method thereof.
Embodiment 1
A joins 280g divinylbenzene and 290g vinyl xylene, ethyl vinyl benzene in the 120g methyl styrene in container, and stirring makes it to be made into polymerization single polymerization monomer;
B, in the polymerization single polymerization monomer that the A step is made into, add the 300g n-heptanol and the 3.5g dibenzoyl peroxide mixes, form oil phase;
C, in the reactor of high speed agitator is housed, 15 gelatin and 150g sodium chloride are joined in the 3000g water, heated and stirred is fully mixed and is made into water;
D, oil phase is joined aqueous phase, under high-speed stirred, make oil phase be distributed to aqueous phase fully and form particle diameter less than the little liquid pearl of 0.3mm, heat 60-65 ℃ and kept 8 hours, slowly be warming up to 100 ℃ then and carry out free radical copolymerization, generate solid multipolymer microballon, after finishing, reaction leaches microballon, water steam steams pore-foaming agent, with acetone flush away residual solvent and other impurity, obtains porous type macromolecule microballon;
E, use the sieve method classification, getting granularity is 0.3-0.2mm, 0.2-0.13mm, 0.13-0.074mm, 0.074-0.40mm, 0.40-0.030mm, 0.030-0.010mm six groups of microballons, all can be used as the reverse-phase chromatography stationary phase of different purposes, its chemical constitution is ring-alkylated styrenes-divinyl benzene copolymer, this type of small porous particle specific surface scope 500-550m
2/ g, cell size scope 35-40%, pore size distribution is a 30-1000A ° of scope.
Embodiment 2
A joins 280g divinylbenzene and 290g vinyl xylene, ethyl vinyl benzene in the 120g styrene in container, and stirring makes it to be made into polymerization single polymerization monomer;
B, in the polymerization single polymerization monomer that the A step is made into, add the 300g 2-Ethylhexyl Alcohol and the 7g azoisobutyronitrile mixes, form oil phase;
C, in the reactor of high speed agitator is housed, 15g polyvinyl alcohol (PVA) and 200g lime chloride are joined in the 3000g water, agitating heating is fully mixed and is made into water;
D, oil phase is joined aqueous phase, under high-speed stirred, make oil phase be distributed to aqueous phase fully and form particle diameter less than the little liquid pearl of 0.3mm, heat 60-65 ℃ and kept 8 hours, slowly be warming up to 100 ℃ and carry out free radical copolymerization, generate solid multipolymer microballon, after finishing, reaction leaches microballon, water steam steams pore-foaming agent, with acetone flush away residual solvent and other impurity, obtains porous type macromolecule microballon;
E, use the sieve method classification, the microballon of the approximate six groups of narrow size-grade distribution of granularity and embodiment 1, all can be used as the reverse-phase chromatography stationary phase of different purposes, its chemical constitution is a styrene diethylene benzene copoly mer, and its pore structure is close with the embodiment of the invention 1 product.
Embodiment 3
The composition of device, water is identical with the embodiment of the invention 1, oil phase consists of: 300g methacrylate glycol ester, 200g itaconic acid diallyl ester, 95g methyl methacrylate, 400g toluene, 6g azoisobutyronitrile, operation steps and condition are identical with the embodiment of the invention 1, obtain porous type macromolecule microballon; Use the sieve method classification, obtain granularity 0.3-0.2mm respectively, 0.2-0.13mm, 0.13-0.074mm, 0.074-0.04mm, 0.04-0.03mm, 0.03-0.01mm five groups of porous beads of particle diameter, its chemical constitution are cross-linked poly methyl propylene methyl esters type multipolymer, pore structure is specific surface area 100-120m
2/ g, cell size 40-50%, pore diameter distribution 50-800A °, these group microballons can be made the reverse-phase chromatography stationary phase respectively.
Embodiment 4
The composition of device, water is identical with the embodiment of the invention 1, oil phase consists of: 300g methacrylate tirethylene glycol ester, 100g trimerization isonitrile acid triallyl ester, the 194g methyl acrylate, the 6g azoisobutyronitrile, 300g butyl acetate, 100g200# industrial naptha, operation steps and condition are identical with the embodiment of the invention 2, obtain porous type macromolecule microballon; Use the sieve method classification, obtain varigrained porous beads group respectively, its chemical constitution is a cross linked polyacrylate methyl esters type multipolymer, and its pore structure is 100-120m for its specific surface area
2/ g, cell size are 45-50%, and pore size distribution range: 40-800A °, the porous beads of each group all can be used as the reverse-phase chromatography stationary phase.
Embodiment 5
The composition of device, water is identical with the embodiment of the invention 2, oil phase is formed: the 400g triallyl cyanurate, the 150g butyl acrylate, 44g industry divinylbenzene, 200g diethyl ethyl alcohol, 200g heptane, 6g azoisobutyronitrile, operation steps and condition are identical with the embodiment of the invention 2, obtain porous type macromolecule microballon; Obtain six groups of varigrained porous beads by the sieve method classification, its chemical constitution is butyl polyacrylate one triallyl cyanurate one divinyl benzene copolymer.Its pore structure is close with the embodiment of the invention 4 products, and the porous beads of each group can be respectively as the reverse-phase chromatography stationary phase.
Embodiment 6
The composition of device, water is identical with the embodiment of the invention 1, and oil phase is formed: 245g industry divinylbenzene, 150g cyamelide triallyl, 200g vinyl cyanide, 5g dibenzoyl peroxide, 300g cyclohexanone, 100g heptane.Operation steps and condition are identical with the embodiment of the invention 1, obtain porous type macromolecule microballon; Use the sieve method classification, obtain six groups of varigrained porous beads, its chemical constitution is trimerization isonitrile acid one divinylbenzene, one acrylonitrile copolymer or claims the crosslinked polypropylene lonitrile copolymer that its pore structure is close with the embodiment of the invention 5 products, can make the reverse-phase chromatography stationary phase respectively.
Embodiment 7
The composition of device, water is identical with the embodiment of the invention 1, and oil phase consists of: 144g industry divinylbenzene, 250g methacrylate glycol ester, 200g vinylacetate, 6g azoisobutyronitrile, 200g isooctane, 200g 2-Ethylhexyl Alcohol.Operation steps and condition are identical with the embodiment of the invention 1, use the sieve method classification, obtain six groups of different grain size porous type macromolecule microballons; Its chemical constitution is methacrylate glycol ester one divinylbenzene one vinyl acetate copolymer, or claims cross-linking polyethylene acetate multipolymer, and its pore structure is close with the embodiment of the invention 3 products, can make the reverse-phase chromatography stationary phase respectively.
Embodiment 8
A joins 250g methacrylate glycol ester and 145g industry divinylbenzene in the 100 methoxy acrylamides and to stir in container, makes it to be made into polymerization single polymerization monomer;
B, add the 5g dibenzoyl peroxide in the polymerization single polymerization monomer that the A step is made into, 500g toluene mixes, and forms oil phase;
C, in the reactor of high speed agitator is housed, 300g sodium chloride, 15g gelatin and 50g sodium hydrogen phosphate are joined in the 3000g water, agitating heating is fully mixed and is made into water, with proper amount of sodium hydroxide water PH is transferred to PH7.5;
D, oil phase is joined aqueous phase, under high-speed stirred, make oil phase be distributed to aqueous phase fully and form particle diameter less than the little liquid pearl of 0.3mm, heat 60-65 ℃ and kept 8 hours, slowly be warming up to 100 ℃ and carry out free radical copolymerization, generate solid multipolymer microballon, after finishing, reaction leaches microballon, water steam steams pore-foaming agent, with acetone flush away residual solvent and other impurity, obtains porous type macromolecule microballon;
E, use the sieve method classification, get six groups of varigrained porous beads, all can be used as the reverse-phase chromatography stationary phase of different purposes, its chemical constitution claims the crosslinked methacrylic amide copolymer again for poly-methacrylate glycol ester one divinylbenzene one methoxy acrylamide copolymer.Its pore structure and the embodiment of the invention 3 products are approaching.
Embodiment 9
The composition of device, water is identical with the embodiment of the invention 8, and oil phase consists of: 200g itaconic acid diallyl ester, 295g industry divinylbenzene, 300g ethyl butyrate, 200g120# gasoline, 5g dibenzoyl peroxide.Operation steps and condition are identical with the embodiment of the invention 8, obtain porous type macromolecule microballon; Use the sieve method classification, obtain the porous beads that six groups narrow grains distribute, its chemical constitution is crosslinked poly-itaconic acid diallyl ester copolymer, and its pore structure is close with embodiment 2 products, can be respectively as the reverse-phase chromatography stationary phase.
Embodiment 10
The composition of device, water is identical with the embodiment of the invention 8, and oil phase consists of: 200g cyamelide triallyl ester, 295g industry divinylbenzene, the 5g dibenzoyl peroxide, the 300g n-octyl alcohol, operation steps and condition are identical with the embodiment of the invention 8, obtain porous type macromolecule microballon; Carry out grain size segregation with sieve method, obtain the porous beads of six groups of narrow size-grade distribution, its chemical constitution is crosslinked poly-cyamelide triallyl ester copolymer type porous beads.Every group of microballon all can be made the reverse-phase chromatography stationary phase.Its pore structure is close with embodiment 2 products.
It below is the effect example of a kind of high molecular type reverse chromatography stationary phase of the present invention;
Effect example 1
Particle size range with the embodiment of the invention 1 gained is the 0.07-0.040mm stationary phase, dress up the chromatographic column of Ф 40 * 900mm chromatographic bed, with 95% ethanol balance chromatographic column, there is the zeyssatite 20g of (content of lycopene 62%) of 10g tomato ethyl acetate extract to place column cap load, carry out gradient elution with 95% ethanol/dichloromethane mixed liquor as eluent, the concentration volume ratio rose to 50: 50 from 95: 5, substep is collected eluate, carrying out HPLC analyzes, collection contains the lycopene cut, and it is carried out vacuum distillation except that desolvating, and gets the pure product of 5.5g lycopene, concentration is 99.1%, and yield is 88%.
Effect example 2
Particle size range with the embodiment of the invention 2 gained is the stationary phase of 0.04-0.03mm, dress up the chromatographic column of Ф 40 * 900mm chromatographic bed, with 95% ethanol balance chromatographic column, there is the zeyssatite 20g of (content of lycopene 62%) of 10g tomato ethyl acetate extract to place column cap load, carry out gradient elution with 95% ethanol/dichloromethane mixed liquor as eluent, the concentration volume ratio rose to 50: 50 from 95: 5, substep is collected eluate, carrying out HPLC analyzes, collection contains the lycopene cut, and it is carried out vacuum distillation except that desolvating, and gets the pure product of 5.8g lycopene, concentration is 99.5%, and yield is 93%.
Effect example 3
Stationary phase with the 0.20-0.13mm granularity of the embodiment of the invention 3 gained, dress up the chromatographic column of Ф 40 * 950mm chromatographic bed, after the acetone cleaning, the water flushing, with the thick clindamycin phosphate of 10g (purity 90%) sample introduction soluble in water, make eluent with acetone buffer solution, make gradient elution, the concentration volume ratio rose to 60: 40, and collecting liquid went out thing step by step from 20: 80, collect the clindamycin phosphate cut, distillation removes desolvates with the ethylene dichloride extraction, the organic phase condensing crystallizing is being obtained pure product clindamycin phosphate 8.3g, purity 98%, productive rate 90%.
Effect example 4-13 sees Table 1, and the stationary phase among the embodiment 3 is replaced with the stationary phase described in the table 1, and other condition is identical with embodiment 3 with operation steps.Experimental result is as shown in table 1:
| The effect example | Stationary phase of the present invention and granularity | High-purity clindamycin phosphate product | ||
| Output g | Purity % | Productive rate % | ||
| 4 | Embodiment 3, granularity 0.13-0.074mm microballon | 8.6 | 99 | 94 |
| 5 | Embodiment 3, granularity 0.074-0.04mm microballon | 8.8 | 99.5 | 97 |
| 6 | Embodiment 4, granularity 0.13-0.074mm microballon | 8.6 | 98.7 | 94 |
| 7 | Embodiment 5, granularity 0.13-0.074mm microballon | 8.6 | 98.5 | 94 |
| 8 | Embodiment 6, granularity 0.13-0.074mm microballon | 8.6 | 99.1 | 94 |
| 9 | Embodiment 7, granularity 0.13-0.074mm microballon | 8.7 | 98.6 | 94.5 |
| 10 | Embodiment 8, granularity 0.13-0.074mm microballon | 8.7 | 99.1 | 94 |
| 11 | Embodiment 9, granularity 0.13-0.074mm microballon | 8.6 | 98.7 | 94 |
| 12 | Embodiment 10, granularity 0.13-0.074mm microballon | 8.6 | 98.8 | 94 |
| 13 | Embodiment 10, granularity 0.074-0.04mm microballon | 8.7 | 98.5 | 94 |
Claims (9)
1. high molecular type reverse chromatography stationary phase is characterized in that it being to be prepared from by the following method:
A is in crosslinking chemical, and optional adding or do not add single activity double key compound makes it to be made into polymerization single polymerization monomer, and wherein the weight ratio of crosslinking chemical and single activity double key compound is 100: 0-15: 85;
B, add inertia pore-foaming agent and radical initiator in the polymerization single polymerization monomer that the A step is made into, mix the composition oil phase, wherein the weight ratio of polymerization single polymerization monomer and inertia pore-foaming agent and radical initiator is 80: 20: 0.2-30: 70: 6;
C, add suspension stabilizer in the aqueous solution that contains 5-35% percentage by weight salting-out agents, the concentration that makes suspension stabilizer is the 0.2-5% percentage by weight, fully mixes being made into water;
The volume ratio of D, oil phase and water is 1: 1-1: 15, under high-speed stirred, make oil phase be distributed to aqueous phase fully and form particle diameter less than the little liquid pearl of 0.3mm, heat 60-100 ℃ and carry out free radical copolymerization, generate solid multipolymer microballon, after finishing, reaction leaches microballon, or/and the solvent wash method is removed impurity in pore-foaming agent and other microballon hole, obtain porous type macromolecule microballon with the way of distillation;
E, the porous type macromolecule microballon that obtains is carried out size grading, obtain the bead that the narrow grain of bead size each section in the 0.01-0.3mm scope distributes, its hole characteristic is: the specific surface area scope is 20-800m
2/ g; Cell size scope: 10-75%; Pore size distribution range: 20-1000A °, its outward appearance be bead size in the 0.01-0.3mm particle size range, the porous type macromolecule microballon of these narrow size-grade distribution can be respectively as the reverse-phase chromatography stationary phase.
2. a kind of high molecular type reverse chromatography stationary phase according to claim 1, wherein said crosslinking chemical comprises: one or more potpourris in divinylbenzene, industrial divinylbenzene, trivinyl toluene, divinyl dimethylbenzene, methacrylate glycol ester, methacrylate macrogol ester, itaconic acid diene propyl ester, cyamelide triallyl ester, the cyanuric acid triallyl ester.
3. a kind of high molecular type reverse chromatography stationary phase according to claim 1, wherein said single activity double key compound comprises: styrene, ethyl styrene, methyl styrene, methyl methacrylate, one or more potpourris in methyl acrylate, ethyl acrylate, butyl acrylate, vinyl cyanide, the methoxy acrylamide.
4. a kind of high molecular type reverse chromatography stationary phase according to claim 1, wherein said inertia pore-foaming agent comprises: one or more potpourris among aliphatic hydrocarbon carbon atom＞C7, aromatic hydrocarbon, 120# industrial naptha, 200# industrial naptha, C4-C8 fatty alcohol, the total carbon atom＞C6 of fatty ester and the aliphatic ketone＞C6.
5. a kind of high molecular type reverse chromatography stationary phase according to claim 1, wherein said radical initiator is: dibenzoyl peroxide, azoisobutyronitrile, dilauroyl peroxide.
6. a kind of high molecular type reverse chromatography stationary phase according to claim 1, wherein said salting-out agents comprise: one or more potpourris in sodium chloride, lime chloride, phosphate, the sulfate.
7. a kind of high molecular type reverse chromatography stationary phase according to claim 1, wherein said suspension stabilizer comprises: one or more potpourris in polyvinyl alcohol (PVA), gelatin, carboxymethyl cellulose, the starch.
8. according to the preparation method of the described a kind of high molecular type reverse chromatography stationary phase of claim 1, it may further comprise the steps;
A is in crosslinking chemical, and optional adding or do not add single activity double key compound makes it to be made into polymerization single polymerization monomer;
B, in the polymerization single polymerization monomer that the A step is made into, add inertia pore-foaming agent and radical initiator, mix the composition oil phase;
C, in containing the aqueous solution of salting-out agents, add suspension stabilizer, fully mix being made into water;
D, under high-speed stirred, make oil phase be distributed to aqueous phase fully and form particle diameter less than the little liquid pearl of 0.3mm, heat 60-100 ℃ and carry out free radical copolymerization, generate solid multipolymer microballon, after finishing, reaction leaches microballon, or/and the solvent wash method is removed impurity in pore-foaming agent and other microballon hole, obtain porous type macromolecule microballon with the way of distillation;
E, the porous type macromolecule microballon that obtains is carried out size grading, obtain the bead that the narrow grain of each section distributes, the porous type macromolecule microballon of these narrow size-grade distribution can be respectively as the reverse-phase chromatography stationary phase.
9. according to the application of the described a kind of high molecular type reverse chromatography stationary phase of claim 1 in preparative chromatography and process-scale chromatography.
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2006
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