•The C16mimBr-coated ATP/PANI-PPY/Fe3O4 nanocomposites was first utilized in MMHDSPE.•ATP/PANI-PPY/Fe3O4 nanocomposites were synthesized using a one-pot method.•The technique provided good repeatability and high extraction efficiency.•The method was effectively applied in detecting acaricides in juice samples.In this research, a novel method using magnetic mixed hemimicelles dispersive solid-phase extraction (MMHDSPE) based on C16mimBr-coated attapulgite/polyaniline-polypyrrole/Fe3O4 (ATP/PANI-PPY/Fe3O4) nanocomposites were investigated for enrichment and separation of three acaricides in fruit juice. In this method, we combined the simplicity and speed of dispersive solid-phase extraction, the advantages of mixed hemimicelles and the facility of the phase separation of the magnetic nanoparticles to develop a simple, rapid, sensitive, and effective method for detecting target analytes from the juice samples. ATP/PANI-PPY/Fe3O4 nanocomposites were successfully synthesized using a one-pot method. The as-prepared nanocomposite sorbents were characterized by Fourier transform infrared spectra (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The experimental factors affecting the extraction efficiency including the sorbent type, amount of ATP/PANI-PPY/Fe3O4 nanocomposites, volume of ILs, sonication time, pH, and desorption conditions were optimized. Under the optimal conditions, good linearity was observed for all target analytes, with correlation coefficients (r2) ranging from 0.9994 to 0.9999; the limits of detection (LOD) were in the range of 0.16–0.57 μg L−1, and the recoveries of analytes using the proposed method ranged between 88.67% and 95.10%. The sorbents exhibited excellent repeatability in the range of 1.83–4.24% in extracting the three target analytes. In addition, the intra-day and inter-day precision values were found to be in the range of 0.19–6.24% and 2.23–8.36%, respectively. The method was successfully applied to analyze fruit juice samples by rapid preconcentration of acaricides.

•A novel superparamagnetic ATP/Fe3O4/PANI nanocomposite was first introduced in MDSPE.•ATP/Fe3O4/PANI nanocomposites exhibited fast adsorption and desorption kinetics.•An excellent sorbent-to-sorbent reproducibility was demonstrated in the procedure.•A wider linear range and good recoveries with low LODs were achieved.•The ATP/Fe3O4/PANI-based MDSPE was effective in detecting BUs in river samples.In this study, the superparamagnetic attapulgite/Fe3O4/polyaniline (ATP/Fe3O4/PANI) nanocomposites were successfully synthesized by a one-pot method. Fe (III) was applied as both the oxidant for the oxidative polymerization of aniline and the single iron source of Fe3O4 formed by the redox reaction between aniline and Fe (III). The ATP/Fe3O4/PANI was used as sorbent for magnetic dispersive solid phase extraction (MDSPE) of benzoylurea insecticides (BUs) in environmental water samples. The as-prepared nanocomposite sorbents were characterized by Fourier transform infrared spectra (FT-IR), X Ray diffraction (XRD), scanning electron microscopy(SEM), transmission electron microscopy (TEM), and vibrating sample magnetometry. Various experimental parameters affecting the ATP/Fe3O4/PANI-based MDSPE procedure, including the composition of the nanocomposite sorbents, amount of ATP/Fe3O4/PANI nanocomposites, vortex time, pH, and desorption conditions were investigated. Under the optimal conditions, a good linearity was observed for all target analytes, with correlation coefficients (r2) ranging from 0.9985 to 0.9997; the limits of detection (LOD) were in the range of 0.02–0.43 μg L−1, and the recoveries of analytes using the proposed method ranged between 77.37% and 103.69%. The sorbents exhibited an excellent reproducibility in the range of 1.52–5.27% in extracting the five target analytes. In addition, the intra-day and inter-day precision values were found to be in the range of 0.78–6.86% and 1.66–8.41%, respectively. Finally, the proposed ATP/Fe3O4/PANI-based MDSPE method was successfully applied to analyze river water samples by rapid preconcentration of BUs.

•The β-cyclodextrin/attapulgite composite effervescent tablets were proposed for the first time.•The sorbent was dispersed into the solution with the release of carbon dioxide.•A filter membrane was used to recover the sorbent after the extraction.•The prepared sorbent exhibited highter extraction efficiency for analysis of pyrethroids than C18 and HLB.•No auxiliary apparatus was used throughout the extraction process.In this research, an effervescence-assisted β-cyclodextrin/attapulgite composite (β-CD/ATP) for the in-syringe dispersive solid-phase extraction (EAIS-DSPE) of pyrethroids in environmental samples was developed for the first time. A syringe was used to conduct the extraction procedure and a small amount of β-CD/ATP was dispersed into the solution with the release of carbon dioxide when the effervescent tablet components dissolved in water. Then, the sorbent was recovered using a filter membrane, and the analytes were directly eluted using acetonitrile. In the process, the β-CD/ATP sorbent resulted in an excellent extraction efficiency compared to commercially available sorbents such as C18 and HLB. Moreover, in the extraction procedure, both the β-cyclodextrin inclusion interactions (especially the hydrophobic effects) and the special structure of the ATP contributed to the efficient enrichment of pyrethroids in aqueous media. The amount of β-CD/ATP sorbent, the volume of desorption, the ratio of NaH2PO4/Na2CO3, the volume of the sample, and the pH were screened using a Plackett–Burman design. All factors affecting the procedure were optimized by applying a central composite design. Under the optimized conditions, a good repeatability (RSDs) ranging from 1.7 to 2.3, linearity (2.5–500 μg L−1), limits of detection (LODs) (0.15–1.03 μg L−1), and an acceptable recoveries (76.8–86.5%) were achieved. Finally, the proposed method was successfully applied for the determination of pyrethroids in environmental samples including river water, reservoir water and lake water.

A novel, rapid ionic liquid dispersive liquid–liquid microextraction (IL-DLLME) technique combined with magnetic retrieval (MR-IL-DLLME) has been developed and used to analyze five benzoylurea insecticides (BUs) in environmental water samples. This procedure was based on the magnetic retrieval of the ionic liquid using unmodified magnetic nanoparticles (MNPs). In this experiment, the fine ionic liquid droplets formed in aqueous samples functioned as an extractant for the extraction of BUs; after the extraction process was completed, Fe3O4 MNPs were added as a carrier to retrieve and separate the ionic liquid from the sample solution. After the supernatant was removed, the ionic liquid was desorbed using acetonitrile and subsequently injected directly into an HPLC system for analysis. The optimum experimental parameters are as follows: 20 mg of Fe3O4 (20 nm) as magnetic sorbents; 70 μL of [C6MIM][PF6] as the extraction solvent; 300 μL of acetonitrile as the disperser solvent; a vortex extraction time of 90 s with the vortex agitator set at 2800 rpm and no ionic strength. Under the optimized conditions, good linearity was obtained with correlation coefficients (r) greater than 0.9981. The repeatability and reproducibility of the proposed method were found to be good, and the limits of detection ranged from 0.05 μg L−1 to 0.15 μg L−1. The proposed method was then successfully used for the rapid determination of BUs in real water samples. The recoveries of five BUs at two spiked levels ranged from 79.8 to 91.7% with RSDs less than 6.0%.Highlights► A novel approach (MR-IL-DLLME) was developed. ► [C6MIM][PF6] was chosen as extractant and absorbed by Fe3O4 magnetic nanoparticles. ► The method exceptionally accelerates the sample preparation, extraction was completed within 5 min. ► The method was applied for benzoylurea insecticides in real water samples.