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目的制备一种新型磁性多孔碳材料一γ-Fe_2O_3/C,并建立一种简单可靠的富集水中孔雀石绿的方法。方法先利用水热法合成MOF-MIL-53(Fe),再以其为模板通过微波辅助高温离子热法合成γ-Fe_2O_3/C,利用XRD、FT-IR、SEM、TEM等手段对γ-Fe_2O_3/C进行表征,并将其作为MSPE吸附剂富集环境水样中的孔雀石绿,同时对吸附剂用量、洗脱剂种类、萃取时间以及洗脱次数等影响磁固相萃取效率的因素进行优化。结果孔雀石绿在50~5000μg/L的浓度范围内线性关系良好,相关系数大于0.9995,方法检出限为11.07μg/L,添加低、中、高3个浓度水平下的回收率范围为84.0%~102.0%,相对标准偏差小于5%(n=5)。结论本研究制备的纳米材料可适用于日常环境水样中的孔雀石绿的检测。
Aim To prepare γ-Fe 2 O 3 / C, a new type of magnetic porous carbon material, and to establish a simple and reliable method for enriching malachite green in water. Methods Firstly, MOF-MIL-53 (Fe) was synthesized by hydrothermal method, and then γ-Fe2O3 / C was synthesized by microwave-assisted high temperature ionothermal method using it as template. Fe_2O_3 / C was used as MSPE adsorbent to enrich malachite green in environmental water samples. Factors influencing the efficiency of magnetic solid phase extraction, such as the amount of adsorbent, the type of eluent, the extraction time and the number of elution, optimize. Results The calibration curve of malachite green showed good linearity in the concentration range of 50-5000μg / L with the correlation coefficient greater than 0.9995. The detection limit of the method was 11.07μg / L. The recoveries of malachite green at low, medium and high concentrations were 84.0 % ~ 102.0%, relative standard deviation less than 5% (n = 5). Conclusion The nanomaterials prepared in this study are suitable for the detection of malachite green in routine environmental water samples.