Liquid chromatography stationary phase based on three cation liquids and its preparation method and application
A three-cation, liquid chromatography technology, applied in the separation of hydrophilic substances and hydrophobic substances, three-cation liquid-bonded silica gel liquid chromatography stationary phase and its preparation field, to achieve good retention and separation selectivity, column The effect of high efficiency and novel structure
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Embodiment 1
[0027] Embodiment one: the preparation of three cation liquids
[0028] 1-vinylimidazole and 2,4,6-tribromomethyltrimethylbenzene were mixed with methanol and isopropanol in a molar ratio of 7:1, stirred and heated to reflux under the protection of argon for 6 days, after cooling , the solvent was removed by rotary evaporation in vacuo, and the remaining mixture was washed with ethyl acetate to remove unreacted raw materials to obtain a white solid, that is, a tricationic liquid 1,3,5-{tris(3-vinylimidazole)methyl}trimethylbenzene Tribromide, dried under vacuum at 60°C. Next, dissolve 4g of the three cation liquid tribromide in water, and add 5.5 moles of the three cation liquid tribromide equivalent lithium salt (LiNTf 2 ) aqueous solution, after stirring at room temperature for more than 48 hours, take out the upper water layer, and then continue to wash with water four times to obtain the three cation liquid 1,3,5-{three ( 3-vinylimidazole)methyl}trimethylbenzenetris(bis-...
Embodiment 2
[0030] Example 2: Preparation of three cation liquid-bonded silica gel stationary phases
[0031] Silica balls (particle size 5μm, pore size 10nm, specific surface area 310m 2 g -1 ) dispersed in anhydrous toluene and stirred evenly, adding (3-mercaptopropyl)trimethoxysilane equivalent to 1.3 times the number of moles of silicon hydroxyl groups on the surface of silicon balls, heated and refluxed for 24 hours under argon protection, centrifuged, and washed with methanol Five times to obtain silica spheres with 3-mercaptopropyl groups bonded to the surface, which were dried in vacuum at 60°C.
[0032] The prepared tricationic liquids TCIL1 and TCIL2 were respectively bonded to the surface of silicon spheres with 3-mercaptopropyl groups bonded to the surface through the click chemical reaction of thiols and double bonds. Take two parts of silicon spheres with 3-mercaptopropyl groups bonded on the surface, each 3.2g, and disperse them in two parts of methanol respectively, and ...
Embodiment 3
[0034] Example 3: Evaluation of three cationic liquid-bonded silica gel stationary phases
[0035] First, elemental analysis was carried out on the three cation liquid bonded silica gel stationary phases, the results are as follows: TCIL bonded silica gel (C% 9.62, N% 2.22, H% 1.22) and TCIL2 bonded silica gel (C% 9.21, N% 2.24, H %1.10), the corresponding surface bonding amounts are 0.73 and 0.74 μmol / m based on N element loading 2 .
[0036] Secondly, evaluate the reversed-phase retention behavior of the prepared two kinds of stationary phases based on three cation liquids, and separate benzene series, condensed rings and Tanaka test mixtures under reversed-phase chromatographic conditions. The separation chromatogram is as follows image 3 with Figure 4 shown. Naphthalene was used as the probe, and the mobile phase was ACN / H 2 O(50 / 50, v / v) isocratic elution, DAD 254nm detection, and flow rate of 0.4mL / min, the column efficiencies of the two stationary phases TCIL1 and...
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