A kind of preparation method and application of dendrimer functionalized polymer
A technology of dendritic macromolecules and polymers, which is applied in the fields of new chromatography materials and sample pretreatment, to achieve the effects of improving adsorption efficiency and selectivity, rapid and accurate detection, and reducing matrix interference
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Embodiment 1
[0045] Dissolve 10 mmol (2.0 mL) of diethylaminoethyl methacrylate, 40 mmol (5.66 mL) of divinylbenzene and 115 mg of azobisisobutyronitrile in a solution containing toluene (5.68 mL) and 1-dodecanol (2.12 g ) in the porogen solution, prepared into solution A, and then passed nitrogen into solution A for 15 minutes to remove oxygen molecules. 120mg of SiO with a particle size of 12nm 2 Disperse into 10mL water, ultrasonic 10min to make nano-SiO 2 Disperse, then add 4mL of solution A, stir with a homogenizer at 6000rpm for 1min, then pass nitrogen gas for 2min to remove the air above the system, seal it, and polymerize the obtained Pickering emulsion at 60°C for 24h. Suction filter after the reaction, then pass through a 400-mesh stainless steel sieve, and settle with acetone twice, each time for 10 minutes, to obtain polymer PDVB-SiO with a particle size of 15-35 μm 2 . Then take 2g PDVB-SiO 2 Soak in 10mL 40% hydrofluoric acid for 24h to remove SiO on the surface 2 Obtai...
Embodiment 2
[0049] Put 50mg of PDVB into a 3-mL SPE column tube, first equilibrate with 5mL of methanol and 5mL of deionized water, dissolve 7mg of ibuprofen in 30mL of 10mM phosphate buffer (pH 7.0) and load the sample. Drain for 30min, rinse with 5mL methanol, then elute ibuprofen with 5mL1% methanol solution of formic acid, collect the eluent, dilute with methanol / water (1:1), dilute to 250mL, and use high performance liquid chromatography Determination and calculation of ion exchange capacity. The ion exchange capacity determination method of G1-QD, G2-QD, G3-QD, G4-QD and G5-QD is the same as that of PDVB. Table 1 shows the ion exchange capacity results of different generations of dendrimer functionalized polymers.
[0050] Table 1 Determination results of specific surface area, pore volume and ion exchange capacity of dendrimer functionalized polymers of different generations
[0051]
[0052] From Table 1, it can be seen that as the dendrimers grow in the polymer channels, (1)...
Embodiment 3
[0054] Put 200mg G4-QD into a 3-mL SPE column tube, first equilibrate with 5mL methanol and 5mM 10mM phosphate buffer solution, add 10mL 5μg mL -1 Carbamazepine (CAZ), amitriptyline (AMI), hydrocortisone (HYC) and ibuprofen (IBP) in phosphate buffer (pH 7.0) in 1 mL min -1 The speed of sample loading. Drain for 30 minutes, rinse with 5mL of methanol first, then elute with 5mL of methanol solution of 1% formic acid, collect the rinse solution and eluate, each ml as a fraction, blow dry with nitrogen, dilute to 0.5mL, and use HPLC -UV analysis. The efflux curves of different substances are shown in figure 2 ,pass figure 2 It can be seen that carbamazepine (CAZ), amitriptyline (AMT) and hydrocortisone (HYC) can be eluted from the solid-phase extraction column with 2 mL of methanol, but it is necessary to use a methanol solution containing formic acid. The ibuprofen can be eluted, and the results show that the acidic ibuprofen can be selectively retained by the dendrimer fun...
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