Yang Miyi, Zhang Panjie, Hu Lu, Lu Runhua, Zhou Wenfeng, Zhang Sanbing, Gao Haixiang
Department of Applied Chemistry, China Agricultural University, Yuanmingyuan West Road 2#, Haidian District, Beijing 100193, China.
Department of Applied Chemistry, China Agricultural University, Yuanmingyuan West Road 2#, Haidian District, Beijing 100193, China.
J Chromatogr A. 2014 Sep 19;1360:47-56. doi: 10.1016/j.chroma.2014.07.076. Epub 2014 Aug 1.
A green, simple, and efficient method, ionic liquid-assisted liquid-liquid microextraction based on the solidification of floating organic droplets (ILSFOD-LLME) collected via a bell-shaped collection device (BSCD) coupled to high performance liquid chromatography with a variable-wavelength detector, was developed for the preconcentration and analysis of seven benzoylurea insecticides (BUs) in fruit juice. In the proposed method, the low-density solvent 1-dodecanol and the ionic liquid trihexyl(tetradecyl)phosphonium hexafluorophosphate ([P14, 6, 6, 6]PF6) were used as extractant. The extraction solvent droplet was easily collected and separated by the BSCD without centrifugation. The experimental parameters were optimized by the one-factor-at-a-time approach and were followed using an orthogonal array design. The results indicated the different effects of each parameter for extraction efficiency. Under the optimal conditions in the water model, the limits of detection for the analytes varied from 0.03 to 0.28μgL(-1). The enrichment factors ranged from 160 to 246. Linearities were achieved for hexaflumuron and flufenoxuron in the range of 0.5-500μgL(-1), for triflumuron, lufenuron and diafenthiuron in the range of 1-500μgL(-1), and for diflubenzuron and chlorfluazuron in the range of 5-500μgL(-1); the correlation coefficients for the BUs ranged from 0.9960 to 0.9990 with recoveries of 75.6-113.9%. Finally, the developed technique was successfully applied to real fruit juice with acceptable results. The relative standard deviations (RSDs) of the seven BUs at two spiked levels (50 and 200μgL(-1)) varied between 0.1% and 7.3%.
建立了一种绿色、简便且高效的方法，即基于漂浮有机液滴固化的离子液体辅助液液微萃取法（ILSFOD-LLME），该方法通过钟形收集装置（BSCD）收集，并与配备可变波长检测器的高效液相色谱联用，用于果汁中7种苯甲酰脲类杀虫剂（BUs）的预浓缩和分析。在所提出的方法中，低密度溶剂1-十二醇和离子液体三己基（十四烷基）鏻六氟磷酸盐（[P14, 6, 6, 6]PF6）用作萃取剂。萃取溶剂液滴可通过BSCD轻松收集和分离，无需离心。通过单因素法对实验参数进行优化，并采用正交阵列设计进行跟踪。结果表明各参数对萃取效率有不同影响。在水模型的最佳条件下，分析物的检测限为0.03至0.28μg L(-1)。富集因子范围为160至246。氟铃脲和氟虫脲在0.5 - 500μg L(-1)范围内呈线性，氟啶脲、虱螨脲和双甲脒在1 - 500μg L(-1)范围内呈线性，敌草隆和氯氟氰菊酯在5 - 500μg L(-1)范围内呈线性；BUs的相关系数范围为0.9960至0.9990，回收率为75.6 - 113.9%。最后，所开发的技术成功应用于实际果汁，结果令人满意。七个BUs在两个加标水平（50和200μg L(-1)）下的相对标准偏差（RSD）在0.1%至7.3%之间。
