Yang Xiaoling, Zhang Panjie, Li Xiaobing, Hu Lu, Gao Haixiang, Zhang Sanbing, Zhou Wenfeng, Lu Runhua
Department of Applied Chemistry, China Agricultural University, Yuanmingyuan West Road 2#, Haidian District, Beijing 100193, China.
Department of Applied Chemistry, China Agricultural University, Yuanmingyuan West Road 2#, Haidian District, Beijing 100193, China.
Talanta. 2016 Jun 1;153:353-9. doi: 10.1016/j.talanta.2016.03.007. Epub 2016 Mar 7.
In this research, an effervescence-assisted β-cyclodextrin/attapulgite composite (β-CD/ATP) for the in-syringe dispersive solid-phase extraction (EAIS-DSPE) of pyrethroids in environmental samples was developed for the first time. A syringe was used to conduct the extraction procedure and a small amount of β-CD/ATP was dispersed into the solution with the release of carbon dioxide when the effervescent tablet components dissolved in water. Then, the sorbent was recovered using a filter membrane, and the analytes were directly eluted using acetonitrile. In the process, the β-CD/ATP sorbent resulted in an excellent extraction efficiency compared to commercially available sorbents such as C18 and HLB. Moreover, in the extraction procedure, both the β-cyclodextrin inclusion interactions (especially the hydrophobic effects) and the special structure of the ATP contributed to the efficient enrichment of pyrethroids in aqueous media. The amount of β-CD/ATP sorbent, the volume of desorption, the ratio of NaH2PO4/Na2CO3, the volume of the sample, and the pH were screened using a Plackett-Burman design. All factors affecting the procedure were optimized by applying a central composite design. Under the optimized conditions, a good repeatability (RSDs) ranging from 1.7 to 2.3, linearity (2.5-500μgL(-1)), limits of detection (LODs) (0.15-1.03μgL(-1)), and an acceptable recoveries (76.8-86.5%) were achieved. Finally, the proposed method was successfully applied for the determination of pyrethroids in environmental samples including river water, reservoir water and lake water.
在本研究中,首次开发了一种用于环境样品中拟除虫菊酯的注射器内泡腾辅助β-环糊精/凹凸棒土复合材料(β-CD/ATP)分散固相萃取(EAIS-DSPE)方法。使用注射器进行萃取过程,当泡腾片成分溶解于水时,少量β-CD/ATP随着二氧化碳的释放分散于溶液中。然后,使用滤膜回收吸附剂,并用乙腈直接洗脱分析物。在此过程中,与市售吸附剂如C18和HLB相比,β-CD/ATP吸附剂具有出色的萃取效率。此外,在萃取过程中,β-环糊精包合作用(尤其是疏水作用)和ATP的特殊结构共同促进了拟除虫菊酯在水介质中的高效富集。使用Plackett-Burman设计筛选了β-CD/ATP吸附剂的用量、解吸体积、NaH2PO4/Na2CO3比例、样品体积和pH值。通过应用中心复合设计对影响该过程的所有因素进行了优化。在优化条件下,实现了良好的重复性(相对标准偏差为1.7%至2.3%)、线性(2.5 - 500μg L(-1))、检测限(0.15 - 1.03μg L(-1))和可接受的回收率(76.8% - 86.5%)。最后,所提出的方法成功应用于河水、水库水和湖水等环境样品中拟除虫菊酯的测定。