Zwitterionic polymer stationary phase, and preparation and application thereof
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A technology of amphoteric ion and stationary phase, applied in the direction of ion exchange, ion exchange regeneration, ion exchange treatment device, etc., to achieve the effect of novel structure, mild reaction conditions, and industrialization
Inactive Publication Date: 2018-06-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Embodiment 1
[0034] Weigh 10g spherical silica gel (particle size is 5μm, pore size is 20nm, specific surface area is 150m 2 / g), placed in a 250mL glass flask, added 150mL of 5% hydrochloric acid solution, heated to reflux for 12 hours, cooled to room temperature, filtered, washed with water until neutral, and dried at 150°C for 24 hours.
[0035] Put the dried silica gel in a 100mL three-neck glass bottle, add 50mL of toluene to the silica gel under the condition of passing dry nitrogen, stir evenly, then add 6mL of mercaptopropyltriethoxysilane dropwise, at 115°C The reaction was stirred at reflux for 16 hours. The reaction system was filtered, washed successively with methanol, water, tetrahydrofuran and methanol, and the product was dried at 80°C for 12 hours to obtain mercaptopropyl silica gel.
[0036] Put the dried mercaptopropyl silica gel in a 250 mL three-neck glass bottle, add 5.64 g of vinylimidazole, 4.32 g of acrylic acid, 40 mL of methanol and water, and mix thoroughly. T...
Embodiment 2
[0038] Use (3-acrylamidopropyl) trimethylammonium chloride to replace vinylimidazole in Example 1, other raw materials and steps and reaction conditions are all the same as Example 1, and the synthetic steps of Example 1 can obtain (3- Acrylamidopropyl)trimethylammonium chloride and acrylic acid copolymerized zwitterionic polymer stationary phase.
Embodiment 3
[0040] Use vinylpyridine to replace vinylimidazole in embodiment 1, other raw materials and steps and reaction conditions are all
[0041] Same as Example 1, according to the synthesis steps of Example 1, a zwitterionic polymer stationary phase copolymerized with vinylpyridine and acrylic acid can be obtained.
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Abstract
The invention relates to a stationary phase of liquid chromatography. A zwitterionic polymer stationary phase is characterized by being constructed through a manner of anion-cation copolymerization. The zwitterionic polymer stationary phase has a structural formula which is described in the description. In the structural formula, Silica is silica gel; n or m is equal to an integer of 1 to 100; R1is one selected from the group consisting of H or CH3; -R2 is a side chain with a cation radical; and -R3 is a side chain with an anion radical. The zwitterionic polymer stationary phase is prepared by using a controllable anion-cation free radical copolymerization reaction. The method has the following advantages: the rate of the polymerization reaction is controlled through an RAFT reagent in the process of polymerization; reaction conditions are mild; and a polymer stationary phase prepared by using the method provided by the invention has controllable molecular weight, narrow distributionrange and uniform bonding density. The zwitterionic polymer stationary phase provided by the invention can be used as a separation material, and is widely applied to the fields of hydrophilic interaction chromatography, glycopeptide enrichment, heavy metal adsorption, etc.
Description
technical field [0001] The invention relates to a silica gel matrix separation material, in particular to a novel zwitterionic polymer stationary phase and its preparation method and application. Background technique [0002] Hydrophilic Interaction Liquid Chromatography (HILIC) is a chromatographic technique for separating polar compounds, which was first proposed by Alpert in 1990 (Alpert, A.J.etal, J.Chromatogr.1990.499, 177-196 .). As an effective supplement to RPLC, the HILIC mode has been widely used in recent years, and the types of hydrophilic stationary phases are becoming more and more abundant [Guo, Y. et al., J. Chromatogr. A, 2005, 1074, 71-80; Jandera, P. et al., J. Sep. Sci, 2008, 31, 1421-1437; P. et al., J. Sep. Sci, 2006, 29, 1784-1821; Buszewski, B. et al., Anal. Bioanal. Chem, 2012, 402, 231-247.]. However, most of the currently reported hydrophilic stationary phases are small-molecule bonded phases, which are restricted by the specific surface area a...
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