Directly suspended-solidified floating organic droplets for the determination of fungicides in water and honey samples
Directly suspended-solidified floating organic droplets for the determination of fungicides in water and honey samples
复制标题
直接悬浮固化漂浮有机液滴用于测定水和蜂蜜样品中的杀菌剂
DOI：
10.1039/c4ay00806e
复制
发表时间：
2014
影响因子：
3.1
通讯作者：
Gao Haixiang
中科院分区：
文献类型：
--
作者：
Li Songqing;Yang Xiaoling;Hu Lu;Cui Xiangqian;Zhang Sanbing;Lu Runhua;Zhou Wenfeng;Gao Haixiang
建立了一种直接悬浮固化有机微滴微萃取（DS-SFO）方法，用于HPLC-DAD检测前对水和蜂蜜样品中的4种杀菌剂（百菌清、三嘧菌酯、环虫腈和三氯虫酯）进行预富集。在这种技术中，不需要特殊的设备或支撑材料。在所需的萃取时间后，通过固化微滴可以很容易地收集萃取相。对影响提取效率的实验参数进行了考察和优化，得出最佳工艺条件为：1-十二醇微滴20 μL为有机萃取剂，水或稀释后的蜂蜜样品3 mL，不加盐，900 rpm， 30℃搅拌90 min。在优化条件下，该方法对水和蜂蜜样品的提取率分别为80% ~ 93%和70% ~ 83%。方法的检出限（LOD）范围为：水样0.20 ~ 1.95 ng mL - 1，蜂蜜1.14 ~ 11.06 ng g - 1。在5-1000 ng mL−1的校准范围内，相对标准偏差（RSD）为0.9980。该方法允许使用绿色溶剂，有机溶剂用量最少，设备和提取工艺简单，操作通量高。最后，该方法成功地应用于实际水和蜂蜜样品中杀菌剂的测定。
A directly suspended-solidified floating organic droplet microextraction (DS-SFO) method was developed for the preconcentration of four fungicides (i.e., chlorothalonil, triadimefon, cyprodinil, and trifloxystrobin) from water and honey samples prior to HPLC-DAD detection. In this technique, no special devices or supporting materials are required. The extraction phase can be easily collected via solidification of the microdroplet after the desired extraction time. The experimental parameters affecting the extraction efficiency were investigated and optimized, which resulted under optimal conditions of a 20 μL microdroplet of 1-dodecanol as the organic extractant, 3 mL of water or diluted honey sample without salt addition, and 90 min of stirring at 900 rpm and 30 °C. Under the optimized conditions, the proposed method achieved high extraction recoveries of 80% to 93% and 70% to 83% for water and honey samples, respectively. The limits of detection (LOD) of the method were in the range of 0.20–1.95 ng mL−1 for water samples and 1.14–11.06 ng g−1 for honey samples. The relative standard deviation (RSD) was 0.9980) over the calibration range of 5–1000 ng mL−1 were obtained. This method allowed the use of green solvents, a minimal usage of organic solvents, simple device and extraction processes, and high-throughput operations. Finally, the proposed method was successfully applied to the determination of fungicides in real water and honey samples.