Xu Qinqin, Qiao Kexin, Yan Chen, Liu Zikai, Lu Runhua, Zhou Wenfeng
Department of Applied Chemistry, China Agricultural University, Yuanmingyuan West Road 2#, Haidian District, Beijing 100193, China.
Anal Methods. 2020 Jun 26;12(24):3115-3122. doi: 10.1039/d0ay00562b.
In this study, a simple, rapid, precise, and environmentally friendly microextraction named dispersive micro-solid phase extraction based on a graphene/polydopamine composite as a sorbent was investigated for the analysis of four pyrethroids (fenpropathrin, cyhalothrin, etofenprox and bifenthrin) in water samples. The graphene/polydopamine composite was successfully synthesized using a one-step method, and was characterized by scanning electron microscopy, transmission electron microscopy, energy-dispersive spectroscopy and X-ray photoelectron spectroscopy. The simplicity and rapidity of dispersive micro-solid phase extraction and the high surface area and adsorptivity of the graphene/polydopamine composite were combined in the proposed method. Several main parameters, including the amount of the sorbent, extraction time, ionic strength and desorption conditions, were independently optimized and the results were compared to find the best extraction setup for dispersive micro-solid phase extraction. Under the optimal conditions, good linearity was observed for all the target analytes, with the coefficient of determination ranging from 0.9997 to 0.9999. The extraction recoveries obtained using the proposed method ranged from 76.81% to 85.29%, and the limits of detection varied from 1.5 to 3 μg L-1. In addition, the relative standard deviation values for the intra-day precision were between 0.41% and 3.00%, while the inter-day precision showed relative standard deviation values ranging from 1.61% to 5.59%. Overall, the figures of merit of the entire procedure showed that this technique could produce satisfactory results in the detection of pyrethroids in water samples or other organic pollutants in the future.
在本研究中，研究了一种基于石墨烯/聚多巴胺复合材料作为吸附剂的简单、快速、精确且环保的微萃取方法——分散微固相萃取，用于分析水样中的四种拟除虫菊酯（甲氰菊酯、氯氟氰菊酯、醚菊酯和联苯菊酯）。采用一步法成功合成了石墨烯/聚多巴胺复合材料，并通过扫描电子显微镜、透射电子显微镜、能量色散光谱和X射线光电子能谱对其进行了表征。所提出的方法结合了分散微固相萃取的简单性和快速性以及石墨烯/聚多巴胺复合材料的高比表面积和吸附性。对几个主要参数，包括吸附剂用量、萃取时间、离子强度和解吸条件进行了独立优化，并比较结果以找到分散微固相萃取的最佳萃取设置。在最佳条件下，所有目标分析物均呈现良好的线性，测定系数范围为0.9997至0.9999。使用所提出的方法获得的萃取回收率在76.81%至85.29%之间，检测限在1.5至3 μg L-1之间。此外，日内精密度的相对标准偏差值在0.41%至3.00%之间，而日间精密度的相对标准偏差值在1.61%至5.59%之间。总体而言，整个方法的性能指标表明，该技术在未来检测水样中的拟除虫菊酯或其他有机污染物时能够产生令人满意的结果。
