磁性固相萃取结合气质联用仪检测造纸废水中的氯酚类化合物

Magnetic Solid-phase Extraction Combined with GC-MS for Chlorophenols Analysis in Papermaking Wastewater

中文关键词:  磁性聚苯乙烯微球  气质联用  造纸废水  氯酚

Key Words:Fe₃O₄@PS  GC-MS  papermaking wastewater  chlorophenols

中文摘要:

      以聚苯乙烯包覆的四氧化三铁微球（Fe₃O₄@PS）作为磁性固相萃取（MSPE）的吸附剂，结合气质联用仪（GC-MS）测定造纸废水中的氯酚类（CPs）化合物。通过透射电子显微镜（TEM）、X射线衍射仪（XRD）和傅里叶变换红外光谱仪（FT-IR）对吸附剂材料进行表征分析。优化了MSPE过程中材料用量、超声萃取时间和洗脱条件等影响因素。结果显示，20 mg吸附剂材料、超声萃取7 min、2 mL乙醇作为洗脱溶剂是最佳的MSPE条件。在最优条件下进行方法学评价和实际水样加标试验，结果显示，在2.5~2000 μg/L的浓度范围内线性关系较好，检出限在0.076~0.207 μg/L之间，相关系数介于0.9966~0.9994之间。实际水样加标结果显示两种氯酚物质的加标回收率介于83.39%~109.40%之间。实验结果表明，以Fe₃O₄@PS作为MSPE吸附剂，可以较大程度提高CPs化合物的萃取效率并简化操作流程。

Abstract:

      In this study， magnetic polystyrene （Fe₃O₄@PS） microspheres were used as adsorbents in solid phase extraction combined with GC-MS to evaluate the efficiency of extracting chlorophenols （CPs） from papermaking wastewater. The novel microspheres were characterized by transmission electron microscope （TEM）， X-ray diffraction （XRD） and fourier-transform infrared spectroscopy （FT-IR）. The main influence parameters of the magnetic solid-phase extraction （MSPE）， such as the amount of sorbent， extraction time and elution condition， were investigated and optimized. The results demonstrated that 20 mg of sorbent， 7 min of desorption time and 2 mL of eluent solvent were chosen as the optimum conditions. Under the optimum conditions， an excellent linearity was observed in the range of 2.5~2000 μg/L. The LODs for chlorophenols were in the range of 0.076~0.207 μg/L and the correlation coefficients ranging from 0.9966~0.9994. The proposed method was successfully applied for the analysis of papermaking wastewater samples with recoveries ranging from 83.39%~109.40%. The above results demonstrated that Fe₃O₄@PS as a MSPE absorbent performed effective extraction efficiency and simplified operation process in the trace analysis of CPs.