磁性三维石墨烯复合材料的制备及其在有机氯农药残留检测中的应用

Preparation of magnetic three-dimensional graphene nanocomposite and its application in the determination of organochlorine pesticides residues

中文关键词:  三维石墨烯  磁固相萃取  气相色谱法  有机氯农药  水样

英文关键词:three-dimensional graphene  magnetic solid phase extraction  gas chromatography  organochlorine pesticides  water sample

中文摘要:

      目的 建立磁性三维石墨烯复合材料(three-dimensional graphene nanocomposite, 3DG)-磁固相萃取-气相色谱法同时测定水样中8种有机氯农药残留。方法 通过氧化还原自组装制备Fe3O4/3DG作为磁固相萃取技术的萃取材料, 将其用于涡旋萃取样品中的有机氯农药残留, 再用丙酮将其解吸, 解吸剂经0.22 μm滤膜过滤后, 采用气相色谱-电子捕获器(gas chromatography-electron capture detector, GC-ECD)分离检测, 外标法定量。结果 制备的磁性三维石墨烯复合材料兼具三维石墨烯高吸附性和Fe3O4强磁性。所建立的方法对8种有机氯农药的检出限范围为0.015~0.070 μg/L, 定量限范围为0.05~0.23 μg/L, 相对标准偏差为4.93%~9.42%, 8种有机磷农药在各自的线性范围内线性关系良好, 线性相关系数r2>0.9950。将本方法应用于环境水样中有机氯农药残留的分析检测, 加标回收率为75.1%~122.4%。结论 本方法操作简便、准确性好、灵敏度高, 适用于水样中8种有机氯农药残留的同时分析。

英文摘要:

      Objective To establish a method for the simultaneously determination of organochlorine pesticide residues in water samples by magnetic three-dimensional graphene nanocomposite (3DG)-magnetic solid phase extraction-gas chromatography. Methods The Fe3O4/3DG was prepared by self-assembly redox reaction and used as the extraction materials of magnetic solid phase extraction, which was used for vortex extraction of organochlorine pesticides in water samples, and then the extraction was desorbed by acetone, separated and detected by gas chromatography-electron capture detector (GC-ECD) and quantified by external standard method after the desorption agent was filtered by a 0.22 μm filter membrane. Results The prepared Fe3O4/3DG presented both high adsorption of 3DG and strong magnetic of Fe3O4. The limits of detection (LOD) of the proposed method for 8 kinds of organochlorine pesticides was 0.015?0.070 μg/L, and the limits of quantification were 0.05?0.23 μg/L, the relative standard deviations were 4.93%?9.42%, the linear relationship of 8 kinds of organophosphorus pesticides was good within their respective linear range with linear correlation coefficients of r2>0.9950. The method was applied to the determination of organochlorine pesticide residues in environmental water samples, and the spiked recoveries were 75.1%?122.4%. Conclusion The method is simple, accurate and sensitive, and suitable for simultaneous determination of 8 kinds of organochlorine pesticide residues in water samples.