合成并以元素分析、红外及电镜等方法表征Fe_3O_4/羟丙基-β-环糊精聚合物磁性纳米材料(CM-HP-β-CDCP-MNPs),以此作为固相萃取剂,建立磁性固相萃取-紫外可见光谱法分离分析孔雀石绿的新方法。考察影响吸附和洗脱的条件(pH,萃取剂用量,洗脱剂类型用量,萃取用洗脱时间等)。结果表明:室温下,pH 7.0时,CM-HP-β-CDCP-MNPs能快速定量吸附孔雀石绿(吸附率92%);乙醇在30min内可脱附孔雀石绿(脱附率90%);CM-HP-β-CDCP-MNPs可重复使用5次。在最佳实验条件下,该方法的富集倍数为7.5,检出限为5.6ng·mL~(-1),线性范围为0.08~8.00μg·mL~(-1),测定样品中的孔雀石绿结果令人满意。利用红外光谱初步讨论Fe_3O_4/羟丙基-β-环糊精聚合物纳米材料吸附机理。
In this paper,carboxymethyl-hydroxypropyl-β-cyclodextrin polymer modified magnetic particles Fe_3O_4(CM-HP-β-CDCP-MNPs)were prepared and applied to magnetic solid phase extraction of malachite green combined with UV-Visible spectrometry detection.The synthesized magnetic particles were characterized by element analysis,Fourier transform infrared spectra and transmission electron microscopy.Several variables affecting the extraction and desorption of malachite green such as pH,the amount of adsorbent,the type and volume of eluent,extraction and desorption time,and temperature were investigated.Under the optimum conditions,malachite green could be adsorbed by CM-HP-β-CDCP-MNPs(RE% =92),and elution by C_2H_5OH(EE%=90).the preconcentration factor of the proposed method was approximately 7.5,the CM-HP-β-CDCP-MNPs could be used repeatedly for 5times and offered better recovery.The linear range and detection limit(DL)were found to be 0.08~8.00μg·mL~(-1) and 5.6ng·mL~(-1) respectively.This technique had been successfully applied to the determination of malachite green in real samples.The inclusion interaction of CM-HP-β-CDCP-MNPs with malachite green was studied through FTIR.