Preparation of a surface imprinted material and its application in the enantiomeric resolution of glutamic acid
A technology of surface imprinting and glutamic acid, which is applied in the preparation of organic compounds, cyanide reaction preparation, ion exchange, etc., can solve the problems of inability to achieve fast, efficient, and large-scale separation, narrow application range, and high cost. It achieves the effect of facilitating regeneration and repeated use, good elution performance, good recognition selectivity and binding affinity
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Embodiment 1
[0042] Example 1: Preparation of molecular surface imprinted material MIP-PSSS / PSA
[0043] The preparation process specifically includes the following steps:
[0044] (1) Activation treatment of polystyrene primary amine resin microspheres:
[0045] Add 100mL of N,N-dimethylformamide solution to 30g of dried primary amine resin microspheres, soak at 30°C for 12 hours, then filter with suction, put them in a vacuum oven for drying treatment, and the primary amine Activation of amino groups on the surface of resin microspheres;
[0046] (2) Graft polymerization of sodium p-styrenesulfonate on the surface of primary amine resin microspheres:
[0047] The primary amine resin microsphere of 0.2g activation is joined in the four-necked flask, and adds 42mL solvent (V 甲醇 :V 水 =5:2), 0.2887g (0.6235% of the total mass) of SSS, blow nitrogen for 30 minutes and start stirring with a water bath to heat up. When the temperature reaches 50°C, add 0.0600g of initiator ammonium persulfa...
Embodiment 2
[0053] Embodiment 2: investigate the recognition performance of MIP-PSSS / PSA to two kinds of enantiomers L-Glu and D-Glu
[0054] 1. Determination of isothermal binding performance
[0055] Static and dynamic methods were used to measure the binding properties of the surface imprinted material MIP-PSSS / PSA to the two enantiomers of glutamic acid. Similarly, first measure the binding kinetics of MIP-PSSS / PSA to L-Glu and D-Glu, determine the time when the combination reaches equilibrium (also around 2h), and then measure the binding performance on this basis.
[0056] (1) Static method: at a constant temperature of 30°C, put 50 mL of L-Glu solutions whose concentration ranges from 0.03 to 0.30 g / L into several conical flasks with stoppers, and add about 0.03 The imprinted particulate material MIP-PSSS / PSA of g was shaken in a constant temperature oscillator for 2 hours to make the combination reach equilibrium, and the supernatant was collected by stratification, and L-Glu in ...
Embodiment 3
[0065] Embodiment 3: binding selectivity experiment (enantiomer resolution experiment)
[0066] In order to further investigate the recognition characteristics of imprinted materials for L-Glu, a competitive adsorption experiment of MIP-PSSS / PSA for L-Glu and D-Glu was carried out: L-Glu and D-Glu were prepared at a concentration of 0.1 g / L Binary mixed solution (racemate solution, optical rotation is zero), take 50 mL of mixed solution in a stoppered Erlenmeyer flask, add 0.03 g of imprinted particulate material MIP-PSSS / PSA, shake in a constant temperature shaker After 2.5 h, let the adsorption reach equilibrium, stand for separation, measure the total equilibrium concentration of glutamic acid in the supernatant by spectrophotometry, and measure the optical rotation and specific optical rotation of the supernatant by a polarimeter. It was found that the supernatant had optical rotation at this time, and its optical rotation direction was the same as that of D-Glu. The resu...
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