Faculty of Life Science and Biotechnology, Key Laboratory of Applied Technology of Marine Biology, Ministry of Education, Ningbo University, 818 Fenghua Road, Ningbo, 315211, P.R. China.
Analyst. 2012 Jan 21;137(2):437-43. doi: 10.1039/c1an15782e. Epub 2011 Nov 21.
A simple, efficient, and environmentally friendly membrane-assisted solvent extraction (MASE) method for the extraction and preconcentration of six pyrethroid insecticides from aquaculture seawater samples followed by gas chromatography-electron capture detection (GC-ECD) was successfully proposed. The operating conditions for MASE, such as the extraction solvent, solvent volume, NaCl concentration, stirring rate, extraction time, and temperature, were optimized. Compared to conventional Florisil-solid phase extraction (SPE), higher extraction recoveries (85.9% to 105.9%) of three spiked levels of the six pyrethroid pesticides in aquaculture seawater were obtained using MASE, and the RSD values were lower than 7.9%. The limits of detection (LOD, signal-to-noise ratio (S/N)=3) and quantification (LOQ, S/N = 10) were in the range of 0.037-0.166 and 0.12-0.55 μg L(-1), respectively. The results demonstrate the excellent applicability of the MASE method in analyzing the six pyrethroid pesticides in aqueous samples. The proposed method exhibited a high potential for routine monitoring analysis of pyrethroid insecticides in seawater samples.
本文提出了一种简单、高效、环保的膜辅助溶剂萃取（MASE）方法，用于从养殖海水中提取和预浓缩六种拟除虫菊酯类杀虫剂，然后用气相色谱-电子捕获检测（GC-ECD）进行分析。优化了 MASE 的操作条件，如萃取溶剂、溶剂体积、NaCl 浓度、搅拌速度、萃取时间和温度。与传统的 Florisil-固相萃取（SPE）相比，MASE 可获得养殖海水中六种拟除虫菊酯类杀虫剂三个加标水平的更高萃取回收率（85.9%至 105.9%），且 RSD 值低于 7.9%。检出限（LOD，信噪比（S/N）=3）和定量限（LOQ，S/N = 10）的范围分别为 0.037-0.166μg/L 和 0.12-0.55μg/L。结果表明，MASE 方法在分析水样中的六种拟除虫菊酯类杀虫剂方面具有优异的适用性。该方法在海水中拟除虫菊酯类杀虫剂的常规监测分析中具有很高的应用潜力。
