Department of Applied Chemistry, China Agricultural University, Beijing, China.
J Sep Sci. 2017 Sep;40(17):3513-3521. doi: 10.1002/jssc.201700464. Epub 2017 Aug 1.
An ultrasound-assisted, hybrid ionic liquid, dispersive liquid-liquid microextraction method coupled to high-performance liquid chromatography with a variable-wavelength detector was developed to detect ten insecticides, including diflubenzuron, triflumuron, hexaflumuron, flufenoxuron, lufenuron, diafenthiuron, transfluthrin, fenpropathrin, γ-cyhalothrin and deltamethrin, in fruit juices. In this method, an appropriate extraction solvent was chosen based on the partition coefficient of the target compounds. A mixture of 1-octyl-2,3-dimethylimidazolium bis(trifluoromethylsulfonyl)imide and 1-hexyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide was used as the extractant. The extraction efficiency was screened using Plackett-Burman design and optimized using central composite design. Under the optimal conditions, good linearity was obtained for all the analytes in the pure water model and the fruit juice samples. In pure water, the recoveries of the ten insecticides ranged from 85.7 to 108.9%, with relative standard deviations for one day ranging from 1.24 to 2.64%. The limits of detection were in the range of 0.19-0.69 μg/L, and the enrichment factors were in the range of 123-160. The logarithm of the n-octanol/water partition coefficient in this experiment is a useful reference to select a suitable extraction solvent, and the proposed technique was applied for the analysis of ten insecticides in fruit juice with satisfactory results.
建立了一种超声辅助、杂化离子液体、分散液液微萃取方法,结合高效液相色谱和可变波长检测器,用于检测十种杀虫剂,包括除虫脲、伏虫隆、氟铃脲、氟虫脲、氟铃脲、噻虫隆、氟虫腈、氯菊酯、γ-氯氰菊酯和溴氰菊酯,在果汁中。在该方法中,根据目标化合物的分配系数选择适当的萃取溶剂。选择 1-辛基-2,3-二甲基咪唑双(三氟甲磺酰基)亚胺和 1-己基-3-甲基咪唑双(三氟甲磺酰基)亚胺的混合物作为萃取剂。采用 Plackett-Burman 设计筛选萃取效率,并采用中心复合设计进行优化。在最佳条件下,在纯水模型和果汁样品中,所有分析物均具有良好的线性关系。在纯水中,十种杀虫剂的回收率在 85.7%至 108.9%之间,一天内的相对标准偏差在 1.24%至 2.64%之间。检出限在 0.19-0.69μg/L 范围内,富集因子在 123-160 范围内。本实验中 n-辛醇/水分配系数的对数是选择合适萃取溶剂的有用参考,该技术已成功应用于果汁中十种杀虫剂的分析,结果令人满意。