scholarly journals An Eco-Friendly Hydrophobic Deep Eutectic Solvent-Based Dispersive Liquid–Liquid Microextraction for the Determination of Neonicotinoid Insecticide Residues in Water, Soil and Egg Yolk Samples

Molecules ◽  
2020 ◽  
Vol 25 (12) ◽  
pp. 2785 ◽  
Author(s):  
Rawikan Kachangoon ◽  
Jitlada Vichapong ◽  
Yanawath Santaladchaiyakit ◽  
Rodjana Burakham ◽  
Supalax Srijaranai

A green, simple and sensitive hydrophobic DES-based dispersive liquid–liquid microextraction coupled with high-performance liquid chromatography (HPLC) was developed for the analysis of neonicotinoid insecticide residues in various samples. A hydrophobic deep eutectic solvent (DES) was synthesized using decanoic acid as a hydrogen bond donor and tetrabutylammonium bromide (TBABr) as a hydrogen bond-acceptor. DESs were synthesized and characterized by Fourier transform-infrared (FTIR) spectroscopy. Two disperser solvents were substituted with surfactants and acetonitrile, which could afford more effective emulsification and make the extraction relatively greener. The hydrophobic DES extraction phase occurred 10 min after centrifugation, being easy to be collected for analysis. Several parameters were investigated and optimized. Under the optimum condition, the calibration curve of this method was linear in the range of 0.003–1.0-µg·mL−1, with a correlation coefficient (R2) higher than 0.99 and a good repeatability, with the relative standard deviations (RSDs) were less than 5.00%. The limits of detection were in the range of 0.001–0.003 µg·mL−1; the limits of quantitation were in the range of 0.003–0.009 µg·mL·mL−1. Finally, the presented method was implemented to determine the neonicotinoid insecticide residues in water, soil, egg yolk samples and acceptable recoveries were obtained.

2020 ◽  
Vol 58 (9) ◽  
pp. 880-886
Author(s):  
Xiao Li ◽  
Tao Yuan ◽  
Ting Zhao ◽  
Xiaomei Wu ◽  
Yaling Yang

Abstract An environmentally friendly method for the determination of testosterone and methyltestosterone by acid–base-induced deep eutectic solvents liquid–liquid microextraction (DES-ABLLME) combining with high-performance liquid chromatography was established. The deep eutectic solvent (DES) consisting of menthol:lauric acid:decanoic acid (3:1:1) can act as both hydrogen bond donor and hydrogen bond acceptor. In this approach, ammonia solution (NH3•H2O) is used as an emulsifier to react with DESs in the extraction process to generate salt and form milky white solution, achieving high extraction efficiency. Hydrochloric acid was used as a phase separator to change the emulsification state and promote the separation of extraction agent from water phase. A series of parameters were optimized including the volume of DES and the emulsifying agent, glucose concentration as well as hydrochloric acid volume. The method was linear in the range 0.5–100 μg mL−1 with a correlation coefficient (R) of 0.9999, and the limits of detection were 0.067 and 0.2 μg mL−1 for testosterone and methyltestosterone, respectively. This method was applied to analyze testosterone and methyltestosterone in milk samples, and the recoveries were between 89.2 and 108.2%.


2021 ◽  
Vol 8 (3) ◽  
Author(s):  
Nur ‘An Nisaa Mohamad Yusoff ◽  
Nurul Yani Rahim ◽  
Rania Edrees Adam Mohammad ◽  
Noorfatimah Yahaya ◽  
Mazidatulakmam Miskam

An emulsification liquid–liquid microextraction (ELLME) method was successfully developed using phenolic-based deep eutectic solvent (DES) as an extraction solvent for the determination of phenoxy acid herbicides, 3,6-dichloro-2-methoxybenzoic acid (dicamba) and 2-methyl-4-chlorophenoxyacetic acid (MCPA) in environmental water samples. Five different phenolics-based DESs were successfully synthesized by using phenol (DES 1), 2-chlorophenol (DES 2), 3-chlorophenol (DES 3), 4-chlorophenol (DES 4) and 3,4-dichlorophenol (DES 6) as the hydrogen-bond donor (HBD) and choline chloride as the hydrogen-bond acceptor (HBA). The DESs were mixed at 1 : 2 ratio. A homogeneous solution (clear solution) was observed upon the completion of successful synthesis. The synthesized DESs were characterized by using Fourier transform infrared and nuclear magnetic resonance (NMR). Under optimum ELLME conditions (50 µl of DES 2 as extraction solvent; 100 µl of THF as emulsifier solvent; pH 2; extraction time 5 min), enrichment factor obtained for dicamba and MCPA were 43.1 and 59.7, respectively. The limit of detection and limit of quantification obtained for dicamba were 1.66 and 5.03 µg l −1 , respectively, meanwhile for MCPA were 1.69 and 5.12 µg l −1 , respectively. The developed ELLME-DES method was applied on paddy field water samples, with extraction recoveries in the range of 79–91% for dicamba and 82–96% for MCPA.


2021 ◽  
Author(s):  
Beiqi Wu ◽  
Zhengyan Guo ◽  
Xiuting Li ◽  
Xin Huang ◽  
Chao Teng ◽  
...  

This work presents a novel and green analytical procedure involving a deep eutectic solvent-based dispersive liquid-liquid microextraction with solidification of floating organic droplets (DES-DLLME-SFOD) followed by HPLC to measure three...


Toxins ◽  
2021 ◽  
Vol 13 (1) ◽  
pp. 57
Author(s):  
Ainhoa Oller-Ruiz ◽  
Natalia Campillo ◽  
Manuel Hernández-Córdoba ◽  
Javier Gilabert ◽  
Pilar Viñas

The use of dispersive liquid–liquid microextraction (DLLME) is proposed for the preconcentration of thirteen lipophilic marine toxins in seawater samples. For this purpose, 0.5 mL of methanol and 440 µL of chloroform were injected into 12 mL of sample. The enriched organic phase, once evaporated and reconstituted in methanol, was analyzed by reversed-phase liquid chromatography with triple-quadrupole tandem mass spectrometry. A central composite design multivariate method was used to optimize the interrelated parameters affecting DLLME efficiency. The absence of any matrix effect in the samples allowed them to be quantified against aqueous standards. The optimized procedure was validated by recovery studies, which provided values in the 82–123% range. The detection limits varied between 0.2 and 5.7 ng L−1, depending on the analyte, and the intraday precision values were in the 0.1–7.5% range in terms of relative standard deviation. Ten water samples taken from different points of the Mar Menor lagoon were analyzed and were found to be free of the studied toxins.


2021 ◽  
Author(s):  
Huazi Wang ◽  
Qinqin Xu ◽  
Jinglong Jiao ◽  
Hai Wu

A solidified floating organic drop-dispersive liquid-liquid microextraction (SFOD-DLLME) was established for extraction of four benzophenone-ultraviolet filters (BP-UV filters) from water samples using a fatty acid deep eutectic solvent (DES) as...


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