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 B Analyt Technol Biomed Life Sci. 2018 Jul 1;1089:70-77. doi: 10.1016/j.jchromb.2018.04.043. Epub 2018 Apr 30.
In this study, a novel ionic liquid-type surfactant modified attapulgite named as 1-dodecyl-3-methylimidazolium bromide-attapulgite (CMIM-ATP) is successfully prepared and applied in dispersive solid phase extraction (dSPE) for the fast determination of pyrethroid residues in tea drinks. The primary factors that influenced the extraction efficiency, including sorbent type, amount of sorbent, extraction time, desorption conditions, pH and ionic strength, are investigated. The optimized results reveal that the extraction and desorption equilibria are rapidly obtained within 1 min. Under the optimized conditions, good linearity (2-500 μg/L) is observed for four pyrethroids in tea drinks with determination coefficients (r) ranged from 0.9992 to 1.0000. The limits of detection (LODs) are 0.6 μg/L for all pesticides. Acceptable extraction recoveries of target analytes are found from 90.28 to 107.56% with relative standard deviations (RSDs) less than 8.30% in real tea drink samples. The batch-to-bath repeatability is evaluated by recovery test on five independent synthesized CMIM-ATP sorbents. Satisfactory batch-to-batch repeatability is obtained with the recovery factors varied in 15%. A small matrix effect is observed using CMIM-ATP as the sorbent for detection pyrethroids in tea drinks.
在这项研究中,成功制备了一种新型的离子液体型表面活性剂修饰的凹凸棒石,命名为 1-十二烷基-3-甲基咪唑溴化盐修饰的凹凸棒石(CMIM-ATP),并将其应用于分散固相萃取(dSPE)中,用于快速测定茶饮料中的拟除虫菊酯残留。考察了影响萃取效率的主要因素,包括吸附剂类型、吸附剂用量、萃取时间、解吸条件、pH 值和离子强度。优化结果表明,萃取和解吸平衡在 1 min 内迅速达到。在优化条件下,四种拟除虫菊酯在茶饮料中的线性范围为 2-500μg/L,相关系数(r)在 0.9992-1.0000 之间。所有农药的检出限(LODs)均为 0.6μg/L。在实际茶饮料样品中,目标分析物的提取回收率在 90.28%至 107.56%之间,相对标准偏差(RSD)小于 8.30%。通过对五个独立合成的 CMIM-ATP 吸附剂进行回收试验评估批间重复性。使用 CMIM-ATP 作为吸附剂检测茶饮料中的拟除虫菊酯时,获得了令人满意的批间重复性,回收率因子变化在 15%以内。观察到使用 CMIM-ATP 作为吸附剂时,基质效应较小。