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The Fe3O4/SiO2 (400 mg) was dispersed in 100 mL of
methylbenzene for 2.0 h. Then 2.0 mL of MPS was added to
the above dispersion. The reaction mixture was intensely
stirred at 600 rpm under 80 °C for 10 h, the resultant product
collected by an external magnetic field, and rinsed six times
with ethanol and doubly distilled water, respectively. Finally,
the Fe3O4/SiO2-MPS particles obtained were dried under
vacuum at 60 °C for 12 h.
Synthesis of Fe3O4/SiO2-MPS/MIPs
and Fe3O4/SiO2-MPS/FNIPs
Allyl fluorescein was prepared according to the literature [21,
31]. In a typical synthetic procedure, a mixture of fluorescein
(2.00 g, 6.0 mmol), allyl bromide (2.42 g, 20.0mmol), K2CO3
(4.97 g, 36.0 mmol), hydroquinone and iodine (trace), and
anhydrous DMF (60 mL) was heated and stirred at 71 °C in
the dark under N2 for 25 h. The solvent was removed under
reduced pressure. The crude product was recrystallized from
chloroform, and the resulting product was purified by column
chromatography on silica.
The synthesis of Fe3O4/SiO2-MPS/MIPs via a multistep
procedure is illustrated in Fig. 1; 0.4999 g (1 mmol) of LC,
0.2840 g (4 mmol) AM, and 0.03 g AF were dissolved with
10 mL of acetonitrile in a dark environment for 1.0 h. Then the
Fe3O4/SiO2-MPS (0.2 g) was dispersed with 40 mL of acetonitrile
in an ultrasonic bath for 1.5 h. Subsequently, the mixture
of LC/AM/AF was mixed with appropriate amounts of
DVB (0.4, 0.8, 1.6, and 3.2 mL, respectively) and 40 mL
dispersed liquid of Fe3O4/SiO2-MPS for 30 min stirring at
60 °C. At the same time, the solution was sparged with
oxygen-free nitrogen for 10 min in order to purge air. Lastly,
0.1 g of AIBN was added in the flask under N2 protection. The
mixture was stirred at 600 rpm and allowed to proceed at
60 °C under N2 protection for 24 h. After magnetic separation,
the microspheres were eluted with methanol/acetic acid
(100 mL, 90/10 v/v) to remove templates by Soxhlet extractor
and dried in a vacuum at 40 °C for 24 h. Finally, we obtained
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