Xi Xuefei, Yang Miyi, Shen Ganni, Wu Xiaoling, Lu Runhua, Zhou Wenfeng, Zhang Sanbing, Gao Haixiang
Department of Applied Chemistry, China Agricultural University, Haidian District, Beijing, China.
J Sep Sci. 2016 Jan;39(2):391-8. doi: 10.1002/jssc.201500714. Epub 2015 Dec 7.
A simple, sensitive, and efficient method of using a pipette vial to perform dispersive liquid-liquid microextraction based on the solidification of floating organic droplets was coupled with high-performance liquid chromatography (HPLC) and a diode array detector for the preconcentration and analysis of four benzoylurea insecticides in fruit juice. In this method, 1-dodecanol was used as an extractant, and a snipped pipette was used as an experimental vial to simplify the procedure of collecting and separating solidified extractant. The experimental parameters were optimized using a Plackett-Burman design and one-factor-at-a-time method. Under the optimal conditions in the water model, the limits of detection for analytes varied from 0.03 to 0.28 μg/L, and the enrichment factors ranged from 147 to 206. Linearity was achieved for diflubenzuron and flufenoxuron in a range of 0.5-500 μg/L, for hexaflumuron in a range of 1-500 μg/L, and for triflumuron in a range of 5-500 μg/L. The correlation coefficients for the analytes ranged from 0.9986 to 0.9994 with recoveries of 91.4-110.9%. Finally, the developed technique was successfully applied to fruit juice samples with acceptable results. The relative standard deviations of the analytes at two spiking levels (50 and 200 μg/L) varied between 0.2 and 4.5%.
一种基于漂浮有机液滴固化的使用移液管小瓶进行分散液液微萃取的简单、灵敏且高效的方法,与高效液相色谱(HPLC)和二极管阵列检测器联用,用于果汁中四种苯甲酰脲类杀虫剂的预浓缩和分析。在该方法中,使用1-十二醇作为萃取剂,并用剪去头部的移液管作为实验小瓶,以简化收集和分离固化萃取剂的步骤。采用Plackett-Burman设计和单因素法对实验参数进行了优化。在水模型的最佳条件下,分析物的检测限为0.03至0.28μg/L,富集因子为147至206。敌草隆和氟虫脲在0.5 - 500μg/L范围内呈线性,氟铃脲在1 - 500μg/L范围内呈线性,杀铃脲在5 - 500μg/L范围内呈线性。分析物的相关系数在0.9986至0.9994之间,回收率为91.4 - 110.9%。最后,所开发的技术成功应用于果汁样品,结果令人满意。两种加标水平(50和200μg/L)下分析物的相对标准偏差在0.2%至4.5%之间。