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

以聚苯乙烯包覆的四氧化三铁微球(Fe_(3)O_(4)@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2.5~2000μg/L的浓度范围内线性关系较好,检出限在0.076~0.207μg/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Fe_(3)O_(4)@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。

In this study,magnetic polystyrene(Fe_(3)O_(4)@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 2.5~2000μg/L.The LODs for chlorophenols were in the range of 0.076~0.207μg/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 Fe_(3)O_(4)@PS as a MSPE absorbent performed effective extraction efficiency and simplified operation process in the trace analysis of CPs.