College of Chemical Engineering, Zhejiang University of Technology, Hangzhou, P. R. China.
Department of Chemistry, National Chung-Hsing University, Taichung, Taiwan.
J Sep Sci. 2018 Dec;41(24):4498-4505. doi: 10.1002/jssc.201800860. Epub 2018 Nov 14.
A novel microwave-assisted-demulsification dispersive liquid-liquid microextraction technique was established for determination of three triazole fungicides in environmental water samples by gas chromatography with mass spectrometry. Importantly, microwave irradiation has been applied in demulsification to achieve the phase separation and enrichment of triazole fungicides in water samples successfully with low-density toluene as extractant. The experimental variables, including microwave power, microwave time, ultrasonic time, type and volume of extraction solvent, and effect of salting out were investigated. Under the optimized conditions, the method showed good linearity for myclobutanil, tebuconazole, and difenoconazole in the range of 1-100 μg/L. The limits of detection and the limits of quantification were within the range of 0.14-0.27 and 0.47-0.90 μg/L, respectively. The suitable enrichment factors for three triazole pesticides were in the range of 425-636. The recoveries were between 89.3 and 108.7%, and the relative standard deviations were from 5.4 to 8.6%. Finally, environmental water samples were used to verify the applicability of the proposed method for analysis of triazole fungicides targets. It can be concluded that the developed microwave-assisted-demulsification dispersive liquid-liquid microextraction gas chromatography with mass spectrometry method was a rapid, efficient, reliable, and environmental friendly way for analysis of triazole fungicides in water.
建立了一种新型的微波辅助破乳分散液液微萃取技术，用于通过气相色谱-质谱法测定环境水样中的三种三唑类杀菌剂。重要的是，微波辐射已被应用于破乳，以成功地实现水样品中三唑类杀菌剂的相分离和富集，使用低浓度的甲苯作为萃取剂。实验变量包括微波功率、微波时间、超声时间、萃取溶剂的类型和体积以及盐析效应。在优化条件下，该方法在 1-100μg/L 范围内对戊菌唑、戊唑醇和烯唑醇具有良好的线性关系。检测限和定量限的范围分别为 0.14-0.27 和 0.47-0.90μg/L。三种三唑类农药的适宜富集因子在 425-636 范围内。回收率在 89.3%至 108.7%之间，相对标准偏差在 5.4%至 8.6%之间。最后，使用环境水样验证了所提出的方法用于分析三唑类杀菌剂目标物的适用性。可以得出结论，所开发的微波辅助破乳分散液液微萃取气相色谱-质谱法是一种快速、高效、可靠且环保的方法，用于分析水中的三唑类杀菌剂。
