Lactose-based intelligent polymer and application thereof
An intelligent polymer and polymer technology, applied in the field of biochemistry, can solve the problems of accurate sugar chain structure distinction and chromatographic separation problems, and achieve the effect of high separation efficiency
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Embodiment 1
[0043] Synthesis of Lactose Functional Monomer
[0044] 1) Add 200mL of acetic anhydride solution into the reaction vessel, add 1mL of perchloric acid, slowly add 20g of the required lactose, stir for 30min, place in an ice bath, add 6g of red phosphorus, 20mL of bromine, 14mL of water in sequence, and then The reaction was stirred for 4h. The resulting mixture was filtered and dried, washed three times with a mixed solvent of 50% petroleum ether / ether, evaporated under reduced pressure and spin-dried to obtain a derivative of lactose in which the bromo group at the first position was substituted and the other hydroxyl groups were protected by acetyl groups;
[0045] 2) Add 20g of the above product into a clean reaction vessel, dissolve it with 150mL of chloroform, then add 150mL of saturated sodium carbonate solution, add 5g of tetrabutylammonium iodide, 8g of p-hydroxybenzaldehyde, react at 60 degrees Celsius for 12h, and then The water layer was removed, and the dried mi...
Embodiment 2
[0048] Synthesis of Intelligent Polymers Grafted from Polyacrylamide to Lactose
[0049]
[0050] In lactose polymer, x: 0.01~0.7;
[0051] Take x=0.2 as an example,
[0052] Add 1g of polyacrylamide and 0.2g of lactose monomer in turn to the reaction vessel, and add 10mL of H at the same time. 2 O and 15mL methanol were used as solvents, stirred at 40°C for 12 hours, and the obtained product was placed in a dialysis bag and dialyzed in a mixed solution of methanol and water with a volume content of 50% for 3 days, and then freeze-dried to obtain an intelligent polymer of polyacrylamide grafted lactose white solid.
[0053] Characterization data of smart polymers grafted with polyacrylamide lactose 1 H NMR (500MHz, D2O): δ (ppm): 1.62 (m, 80H, C-CH 2 ),2.19(d,40H,C-CH),3.36-3.96(m,11H,CH-OH and CH 2 -OH), 4.41(t, J=3.0Hz, 1H, CH-OH), 5.11(d, J=7.9Hz, 1H, O-CH-O), 5.24(d, J=7.8Hz, 1H, O -CH-O), 7.21(d, J=8.9Hz, 2H, Ph-H), 7.89(d, J=8.8Hz, 2H, Ph-H), 9.76(s, 1H, CH=N).I...
Embodiment 3
[0055] The preparation of the intelligent polymer column chromatographic separation material of polyacrylamide grafted lactose comprises the following steps:
[0056] 1) Add 10 g of porous silica gel and 30 mL of 5 wt % HCl into a 50 mL round bottom flask, mix them, and stir at room temperature for 48 h. A large amount of white solid powder was obtained by suction filtration, which was washed several times with 30mL ultrapure water; after vacuum drying, a hydroxylated silica gel product was obtained;
[0057] 2) Dissolve 30mmol of 3-aminopropyltriethoxysilane in 20mL of tetrahydrofuran, then slowly add carbon disulfide dropwise, and stir the reaction in an ice bath for 3h. After returning to normal temperature, 3.8 g of dicyandiamide was added, followed by 3 drops of triethylamine and 20 mL of tetrahydrofuran, and the mixture was heated to 40° C. and continued to stir for 3 h. This solution is distilled under reduced pressure to obtain 3-(triethoxysilane) propyl isothiocyanat...
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