Department of Agro-Environmental Sciences, Graduate School of Bioresource and Bioenvironmental Sciences, Kyushu University, 819-0395, Fukuoka, Japan; Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura 35516, Egypt.
Department of Agro-Environmental Sciences, Graduate School of Bioresource and Bioenvironmental Sciences, Kyushu University, 819-0395, Fukuoka, Japan.
J Chromatogr A. 2020 Oct 11;1629:461498. doi: 10.1016/j.chroma.2020.461498. Epub 2020 Aug 19.
A green air-assisted dispersive liquid-liquid microextraction based on floating organic droplet solidification (DLLME-SFOD) was introduced for the enrichment of five endocrine disrupting compounds (EDCs) from water using a ternary deep eutectic solvent (TDES) as an extracting solvent prior to their determination by HPLC-PDA. The eutectic solvents were synthesized by combining various fatty acids which can concurrently act as both hydrogen bond acceptors (HBA) and hydrogen bond donors (HBD). Adding a third component to classical two-component eutectic solvents allows to purposefully control density, melting point, and viscosity of the synthesized solvents. Ternary and binary eutectic solvents with C9 acid provided excellent extraction efficiency in comparison with other eutectic solvents with C8 acid, while ternary solvents provided superior extraction efficiency to binary ones. Different variables that could influence the microextraction efficiency were optimized applying central composite face-centered design (CCF). At the optimum conditions, the method had low detection limits ranging from 0.96-2.30 µg/L with a preconcentration up to 134-folds. The method showed good linearity from the linear regression with an excellent correlation coefficient (r > 0.999). A good inter- and intraday precision (%RSD < 7%) and%recovery > 90% were achieved proving the method high precision and accuracy. Furthermore, the potential of using the TDES for determining the EDCs from five real water samples was proved through the higher extraction efficiency of the EDCs (90.06-104.43%) with results uncertainty < 20% for most of the compounds. Finally, the method greenness was evaluated by Raynie pictogram, analytical eco-scale, and Green Analytical Procedure Index (GAPI) approaches which confirm the superior eco-friendship of our method in comparison with other reported methods.
基于浮式有机溶剂固化的绿色空气辅助分散液液微萃取（DLLME-SFOD）被引入，用于使用三元深共晶溶剂（TDES）作为萃取溶剂从水中富集五种内分泌干扰化合物（EDCs），然后用 HPLC-PDA 进行测定。共晶溶剂是通过将各种脂肪酸组合合成的，这些脂肪酸可以同时作为氢键受体（HBA）和氢键供体（HBD）。向经典的二元共晶溶剂中添加第三种成分可以有目的地控制合成溶剂的密度、熔点和粘度。与其他具有 C8 酸的共晶溶剂相比，具有 C9 酸的三元和二元共晶溶剂提供了优异的萃取效率，而三元溶剂的萃取效率优于二元溶剂。通过中心复合面心设计（CCF）优化了可以影响微萃取效率的不同变量。在最佳条件下，该方法的检测限低至 0.96-2.30µg/L，浓缩倍数高达 134 倍。该方法具有良好的线性，相关系数（r>0.999）极好。良好的日内和日间精密度（%RSD<7%）和回收率>90%证明了该方法具有较高的精密度和准确性。此外，通过使用 TDES 从五个实际水样中测定 EDCs 证明了该方法具有较高的萃取效率（EDCs 的萃取效率为 90.06-104.43%），大多数化合物的结果不确定性<20%。最后，通过 Raynie 象形图、分析生态标度和绿色分析程序指数（GAPI）方法评估了该方法的绿色度，这证实了与其他报道的方法相比，我们的方法具有更高的生态友好性。
