A microextraction method was developed based on utilization of a novel ionic liquid (IL) [C₄MIM][NCA] as disperser and conventional ILs as extractor (IL-IL-DLLME). This method was integrated with an in-situ metathesis reaction to achieve high extraction efficiency by eliminating the loss of analytes in the discarded disperser after microextraction. Ultrasonic energy was compared to traditional mechanical shaking to accelerate the in-situ metathesis reaction. A 3-min ultrasonic treatment provided similar extraction efficiency as a 120-min mechanical shaking. Due to their strong acidity and lower solubility than traditional hydrophilic ILs, utilization of [C₄MIM][NCA] in the IL-IL-DLLME procedure increased extraction recoveries (ERs) for triclosan (TCS) and methyltriclosan (MTCS) by 10-12% and also avoided an extra pH adjustment step. A series of operational parameters were optimized using single-factor screening and central composite design as follows: 65 µL extraction solvent, 150 µL [C₄MIM][BF₄] and [C₄MIM][NCA] (132/18, v/v, μL) as dispersive solvent, 0.16 g NH₄PF₆ and 3.3 min ultrasonic time. Under optimized conditions with a fortification of 100 µg kg^-1, ERs were 92.6-93.4% for TCS and 92.7-94.2% for MTCS in bovine milk and chicken egg samples. LODs for TCS and MTCS were 0.16-0.24 µg kg^-1 and the enrichment factors were 21.8-23.1. Inter- and intra-day precisions had relative standard deviations of 3.3-5.4% for the optimized method. Overall, this newly developed IL-IL-DLLME method was effective for detecting trace levels of TCS and MTCS in real-world, animal-based foods. Prominent advantages of the new method include high precision and accuracy, high extraction efficiency, simple analytical operations, and no use of organic solvents making the procedure environmentally benign.

基于利用新型离子液体（IL）[C ₄ MIM] [NCA]作为分散剂和常规ILs作为提取剂（IL-IL-DLLME）的研究，开发了一种微萃取方法。该方法与原位复分解反应集成在一起，可通过消除微萃取后消除废弃分散器中分析物的损失来实现高提取效率。将超声能量与传统机械振动进行了比较，以加快原位复分解反应的速度。3分钟的超声波处理提供的提取效率与120分钟的机械振荡相似。由于它们的强酸度和比传统的亲水性IL更低的溶解度，因此[C ₄IL-IL-DLLME程序中的MIM] [NCA]将三氯生（TCS）和甲基三氯生（MTCS）的提取回收率（ER）提高了10-12％，并且还避免了额外的pH调节步骤。使用单因素筛选和中心复合设计优化了一系列操作参数，如下所示：65 µL萃取溶剂，150 µL [C ₄ MIM] [BF ₄ ]和[C ₄ MIM] [NCA]（132/18，v / v，μL）作为分散溶剂，0.16 g NH ₄ PF ₆和3.3分钟超声时间。在强化条件为100 µg kg ^-1的优化条件下，牛和鸡蛋样品中TCS的ERs分别为92.6-93.4％和MTCS的92.7-94.2％。TCS和MTCS的LOD为0.16-0.24 µg kg ^-1富集因子为21.8-23.1。对于优化方法，日间和日内精度的相对标准偏差为3.3-5.4％。总体而言，这种新开发的IL-IL-DLLME方法可有效检测现实动物食品中痕量的TCS和MTCS。新方法的显着优势包括高精度和高精度，高提取效率，简单的分析操作以及无需使用有机溶剂，因此该程序对环境无害。