Ruan Chunqiang, Zhao Xiang, Liu Chenglan
Key Laboratory of Natural Pesticide and Chemical Biology, Ministry of Education, South China Agricultural University, Guangzhou, P. R. China.
J Sep Sci. 2015 Sep;38(17):2931-7. doi: 10.1002/jssc.201401162. Epub 2015 Jul 15.
In this study, a simple and low-organic-solvent-consuming method combining an acetonitrile-partitioning extraction procedure followed by "quick, easy, cheap, effective, rugged and safe" cleanup with ionic-liquid-based dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection was developed for the determination of diflubenzuron and chlorbenzuron in grapes and pears. Ionic-liquid-based dispersive liquid-liquid microextraction was performed using the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate as the extractive solvent and acetonitrile extract as the dispersive solvent. The main factors influencing the efficiency of the dispersive liquid-liquid microextraction were evaluated, including the extractive solvent type and volume and the dispersive solvent volume. The validation parameters indicated the suitability of the method for routine analyses of benzoylurea insecticides in a large number of samples. The relative recoveries at three spiked levels ranged between 98.6 and 109.3% with relative standard deviations of less than 5.2%. The limit of detection was 0.005 mg/kg for the two insecticides. The proposed method was successfully used for the rapid determination of diflubenzuron and chlorbenzuron residues in real fruit samples.
本研究开发了一种简单且有机溶剂消耗低的方法，该方法结合乙腈分配萃取程序，随后采用基于离子液体的分散液液微萃取进行“快速、简便、廉价、高效、耐用和安全”的净化，并使用二极管阵列检测的高效液相色谱法来测定葡萄和梨中的敌敌畏和灭幼脲。基于离子液体的分散液液微萃取使用离子液体1-己基-3-甲基咪唑六氟磷酸盐作为萃取溶剂，乙腈萃取物作为分散溶剂。评估了影响分散液液微萃取效率的主要因素，包括萃取溶剂类型和体积以及分散溶剂体积。验证参数表明该方法适用于大量样品中苯甲酰脲类杀虫剂的常规分析。三个加标水平下的相对回收率在98.6%至109.3%之间，相对标准偏差小于5.2%。两种杀虫剂的检测限均为0.005 mg/kg。所提出的方法成功用于实际水果样品中敌敌畏和灭幼脲残留的快速测定。
