Yahuan Wang,Zhiwei Wang,Shaomin Wang,Zhimin Chen,Jiafu Chen,Yong Chen,Jianwei Fu
Developing excellent dye adsorbent with high adsorption capability and good reusability and clarifying the interaction mechanism between adsorbent and adsorbate are highly desired for eliminating water pollution. Herein, we present a novel magnetic adsorbent Fe 3 O 4 /poly(cyclotriphosphazene-co-4,4′-sulfonyldiphenol) nanotube modified by glacial acetic acid (defined as Gl-PZSNTs-Fe 3 O 4 ) to remove cationic dye methylene blue (MB) from aqueous solution. Compared with the unmodified magnetic PZSNTs-Fe 3 O 4 , the Gl-PZSNTs-Fe 3 O 4 exhibits rapid adsorption rate and high adsorption capacity. The adsorption equilibrium data was fitted well with Langmuir model, and the adsorption kinetics obeyed the pseudo-second-order kinetics model and Elovich model. Thermodynamic analysis showed that the MB adsorption onto the Gl-PZSNTs-Fe 3 O 4 was endothermic and spontaneous. Especially, through contrasting the adsorption behavior of Gl-PZSNTs-Fe 3 O 4 and PZSNTs-Fe 3 O 4 towards MB dye, we highlighted the importance of glacial acetic acid modification for enhancing the adsorption capacity of the Gl-PZSNTs-Fe 3 O 4 . Meanwhile, we also proposed the adsorption mechanism of the Gl-PZSNTs-Fe 3 O 4 towards MB dye.
A 6-azido-β-cyclodextrin was synthesized and derivatized with p -nitrophenyl isocyanate as chiral ligand. Then the ligand was chemically bonded to mesoporous SBA-15 via a ‘Click Chemistry’ reaction of the azido group with alkynyl group. A new p -nitrophenylcarbamoylated β-cyclodextrin bonded SBA-15 chiral stationary phase (NPCSP) for HPLC was thus obtained. The new stationary phase was first used for enantioseparation of propranolol in human plasma under the polar organic solvent mode. The effects of methanol content, concentration of glacial acetic acid/triethylamine in mobile phase and the temperature on the enantioseparation were studied in detail. The optimized chromatographic conditions were as follows: mobile phase was acetonitrile/methanol/glacial acetic acid/triethylamine (90/10/1.25/2.25, V/V ) at 288 K, with a flow rate of 0.5 mL min −1 , an injection volume of 20 μL and detection wavelength at 290 nm. The resolution was 2.04 with a short run time (< 15 min) under the optimal conditions. The content of propranolol in plasma was quantitatively measured by HPLC-MS under selected ion monitoring mode ([M + H] + m/z 260.10) with hydrochlorothiazide as an internal standard. The good linear relationship was observed in the range of 2.5−50 μg L −1 . The detection limits were 1 μg L −1 according to S/N = 3 for both enantiomers. The experimental results showed that the chiral stationary phase exhibited excellent chiral separation ability to propranolol. The analytical method for propranolol enantiomers was sensitive, accurate, simple and fast, which was can be for the determination of propranolol in plasma and related pharmacokinetic studies.
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