Yu Ling, Guo Guiquan, Zhao Jun, Zhao Linnan, Xia Aiqing, He Xu, Xing Cuijuan, Dong Lili, Wang Fang
College of Chemistry and Chemical Engineering, Xingtai University, Xingtai 054001, China.
Xingtai Department of Ecology and Environment, Xingtai 054001, China.
J Anal Methods Chem. 2021 Mar 13;2021:6622063. doi: 10.1155/2021/6622063. eCollection 2021.
A fast method based on FeO magnetic nanoparticles (FeO MNPs) modified QuEChERS integrated to dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry was established for the determination of 8 organochlorine pesticides (OCPs) in green leafy vegetables. The factors involved in the purification by QuEChERS and concentration by DLLME were optimized. In the QuEChERS process, FeO MNPs were used as a new impurity adsorbent after the sample extraction procedure by acetonitrile, which achieved phase separation rapidly. Carbon black was used as an alternative to costly graphitized carbon black without affecting the recovery. In the process of DLLME, 1 mL of the extract obtained by QuEChERS was used as the dispersive solvent, 40 L of chloroform was used as the extractive solvent, and 4 mL of water was added. Making them mix well, then the dispersed liquid-liquid microextraction concentration was subsequently carried out. The enrichment factors of 8 OCPs ranged from 22.8 to 36.6. The recoveries of the proposed method ranged from 78.6% to 107.7%, and the relative standard deviations were not more than 7.5%. The limits of detection and limits of quantification were 0.15-0.32 g/kg and 0.45-0.96 g/kg, respectively. The method has been successfully applied to the determination of OCPs in green leafy vegetable samples.
建立了一种基于氧化亚铁磁性纳米颗粒(FeO MNPs)修饰的QuEChERS结合分散液液微萃取(DLLME)与气相色谱 - 质谱联用的快速方法,用于测定绿叶蔬菜中的8种有机氯农药(OCPs)。对QuEChERS净化和DLLME浓缩过程中的相关因素进行了优化。在QuEChERS过程中,乙腈萃取样品后,FeO MNPs用作新型杂质吸附剂,可快速实现相分离。炭黑用作昂贵的石墨化炭黑的替代品,且不影响回收率。在DLLME过程中,将1 mL QuEChERS得到的萃取液用作分散溶剂,40 μL氯仿用作萃取溶剂,并加入4 mL水。使其充分混合,随后进行分散液液微萃取浓缩。8种OCPs的富集因子在22.8至36.6之间。该方法的回收率在78.6%至107.7%之间,相对标准偏差不超过7.5%。检测限和定量限分别为0.15 - 0.32 μg/kg和0.45 - 0.96 μg/kg。该方法已成功应用于绿叶蔬菜样品中OCPs的测定。