Department of Chemistry, National Chung-Hsing University, 250 Kuo-Kuang Road, Taichung 402, Taiwan.
J Chromatogr A. 2010 Jul 30;1217(31):5043-9. doi: 10.1016/j.chroma.2010.06.006. Epub 2010 Jun 9.
An in-syringe ultrasound-assisted emulsification microextraction (USAEME) was developed for the extraction of organophosphorus pesticides (OPPs) from water samples. The OPPs subsequently analyzed gas chromatography (GC) using a microelectron capture detector (muECD). Ultrasound radiation was applied to accelerate the emulsification of microL-level low-density organic solvent in aqueous solutions to enhance the microextraction efficiency of OPPs in the sample preparation for GC-muECD. Parameters affecting the efficiency of USAEME, such as the extraction solvent, solvent volume, pH, salt-addition, and extraction time were thoroughly investigated. Based on experimental results, OPPs were extracted from a 5mL aqueous sample by the addition of 20microL toluene as the extraction solvent, followed by ultrasonication for 30s, and then centrifugation for 3min at 3200rpm, offered the best extraction efficiency. Detections were linear in the concentration of 0.01-1microg/L with detection limits between 1ng/L and 2ng/L for OPPs. Enrichment factors ranged from 330 to 699. Three spiked aqueous samples were analyzed, and recovery ranged from 90.1% to 104.7% for farm-field water, and 90.1% to 101.8% for industrial wastewater. The proposed method provides a simple, rapid, sensitive, inexpensive, and eco-friendly process for determining OPPs in water samples.
一种在注射器内超声辅助乳化微萃取（USAEME）被开发用于从水样中萃取有机磷农药（OPPs）。随后，使用微电子捕获检测器（μECD）对 OPPs 进行气相色谱（GC）分析。超声辐射被应用于加速微升级低密度有机溶剂在水溶液中的乳化，以增强 OPPs 在 GC-μECD 样品制备中的微萃取效率。对影响 USAEME 效率的参数进行了深入研究，例如萃取溶剂、溶剂体积、pH 值、加盐和萃取时间。基于实验结果，通过在 5mL 水样中加入 20μL 甲苯作为萃取溶剂，然后进行 30s 的超声处理，再在 3200rpm 下离心 3min，可获得最佳的萃取效率。对于 OPPs，检测在 0.01-1μg/L 的浓度范围内呈线性，检测限在 1ng/L 到 2ng/L 之间。富集因子范围为 330 到 699。对三个加标水样进行分析，农田水的回收率在 90.1%到 104.7%之间，工业废水的回收率在 90.1%到 101.8%之间。该方法为水样中 OPPs 的测定提供了一种简单、快速、灵敏、经济和环保的过程。
