Fast Determination of Eleven Food Additives in River Water Using C18 Functionalized Magnetic Organic Polymer Nanocomposite Followed by High-Performance Liquid Chromatography.

A novel magnetic nanomaterial with Fe3O4 as the core, PS-DVB as the shell layer, and the surface modified with C18 (C18-PS-DVB-Fe3O4) had been synthesized by seeded emulsion polymerization. C18-PS-DVB-Fe3O4 retains the advantages of the chemical stability, large porosity, and uniform morphology of organic polymers and has the magnetic properties of Fe3O4. A simple, flexible, and efficient magnetic dispersive solid phase extraction (Mag-dSPE) method for the extraction of preservatives, sweeteners, and colorants in river water was established. C18-PS-DVB-Fe3O4 was used as an adsorbent for Mag-dSPE and was coupled with high-performance liquid chromatography (HPLC) to detect 11 food additives: acesulfame, amaranth, benzoic acid, tartrazine, saccharin sodium, sorbic acid, dehydroacetic acid, sunset yellow, allura red, brilliant blue, and erythrosine. Under the optimum extraction conditions, combined with ChromCoreTMAQC18 (5 µm, 4.6 × 250 mm), 20 mmol/L ammonium acetate aqueous solution and methanol were used as mobile phases, and the detection wavelengths were 240 nm and 410 nm. The limits of detection (LODs) of 11 food additives were 0.6-3.1 µg/L with satisfactory recoveries ranging from 86.53% to 106.32%. And the material could be reused for five cycles without much sacrifice of extraction efficiency. The proposed method has been used to determine food additives in river water samples, and results demonstrate the applicability of the proposed C18-PS-DVB-Fe3O4 Mag-dSPE coupled with the HPLC method to environment monitoring analysis.

Preparation of deep eutectic solvent modified magnetic graphene oxide/metal organic framework nanocomposites for the extraction of three estrogens in cosmetics.

A novel magnetic dispersive solid phase extraction (MDSPE) procedure based on the deep eutectic solvent (DES) modified magnetic graphene oxide/metal organic frameworks nanocomposites (MGO@ZIF-8@DES) was established and used for the efficient enrichment of estradiol, estrone, and diethylstilbestrol in cosmetics (toner, lotion, and cream) for the first time. Then, the three estrogens were separated and determined by UHPLC-UV analysis method. In order to study the features and morphology of the synthesized adsorbents, various techniques such as FT-IR, SEM, and VSM measurements were executed. The MGO@ZIF-8@DES nanocomposites combine the advantages of high adsorption capacity, adequate stability in aqueous solution, and convenient separation from the sample solution. To achieve high extraction recoveries, the Box-Behnken design and single factor experiment were applied in the experimental design. Under the optimum conditions, the method detection limits for three estrogens were 20-30 ng g-1. This approach showed a good correlation coefficient (r more than 0.9998) and reasonable linearity in the range 70-10000 ng g-1. The relative standard deviations for intra-day and inter-day were beneath 7.5% and 8.9%, respectively. The developed MDSPE-UHPLC-UV method was successfully used to determine  three estrogens in cosmetics, and acceptable recoveries in the intervals of 83.5-95.9% were obtained. Finally, three estrogens were not detected in some cosmetic samples. In addition, the Complex GAPI tool was used to evaluate the greenness of the developed pretreatment method. The developed MDSPE-UHPLC-UV method is sensitive, accurate, rapid, and eco-friendly, which provides a promising strategy for determining hormones in different complex samples.

Facile Preparation of Magnetic COF-on-COF for Rapid Adsorption and Determination of Sulforaphane from Cruciferous Vegetables.

Sulforaphane (SFN) is a natural isothiocyanate compound widely abundant in cruciferous vegetables with multiple bioactive functions. However, traditional analytical methods for the extraction and determination of SFN are cumbersome, time-consuming, and low sensitivity with large amounts of organic solvents. Herein, novel magnetic COF-on-COFs (MB-COFs) were fabricated using Fe3O4 as a magnetic core and COFs-1 grown with COFs-2 as a shell, and they were used as efficient adsorbents of magnetic dispersive solid-phase extraction for rapid quantification of SFN in cruciferous vegetables by combining with HPLC-MS/MS. At the optimal ratio of COFs-1 to COFs-2, MB-COFs had a spherical cluster-like structure and a rough surface, with a sufficient magnetic response for rapid magnetic separation (1 min). Due to the introduction of Fe3O4 and COFs-2, MB-COFs exhibited outstanding extraction efficiencies for SFN (92.5-97.3%), which was about 18-72% higher than that of the bare COFs. Moreover, MB-COFs showed good adsorption capacity (Qm of 18.0 mg/g), rapid adsorption (5 min) and desorption (30 s) to SFN, and favorable reusability (≥7 cycles) by virtue of their unique hierarchical porous structure. The adsorption kinetic data were well fitted by the pseudo-second-order, Ritchie-second-order, intra-particle diffusion, and Elovich models, while the adsorption isotherm data were highly consistent with the Langmuir, Temkin, and Redlich-Peterson models. Finally, under the optimized conditions, the developed method showed a wide linear range (0.001-0.5 mg/L), high sensitivity (limits of quantification of 0.18-0.31 µg/L), satisfactory recoveries (82.2-96.2%) and precisions (1.8-7.9%), and a negligible matrix effect (0.82-0.97). Compared to previous methods, the proposed method is faster and more sensitive and significantly reduces the use of organic solvents, which can achieve the efficient detection of large-scale samples in practical scenarios. This work reveals the high practical potential of MB-COFs as adsorbents for efficient extraction and sensitive analysis of SFN in cruciferous vegetables.

Application of magnetic dispersive solid phase extraction combined with solidification of floating organic droplet-based dispersive liquid-liquid microextraction and GC-MS in the extraction and determination of polycyclic aromatic hydrocarbons in honey.

A magnetic dispersive solid phase extraction method combined with solidification of floating organic droplet-based dispersive liquid-liquid microextraction has been validated for the extraction of polycyclic aromatic hydrocarbons from honey samples. For this purpose, a carbonised cellulose-ferromagnetic nanocomposite was used as a sorbent through the magnetic dispersive solid phase extraction. For preparation of the sorbent, first, carbonised cellulose nanoparticles were created by treating cellulose filter paper with concentrated solution of sulfuric acid. Then, the prepared nanoparticles were loaded onto Fe3O4 nanoparticles through coprecipitation. In the extraction process, first, a few mg of the sorbent was added to the diluted honey solution and dispersed in it using vortex agitation. The particles were then separated and the adsorbed analytes were eluted with an organic solvent. The eluent was taken and after mixing with a water-immiscible extraction solvent was used in the following solidification of floating organic droplet-based dispersive liquid-liquid microextraction procedure. By performing the extraction process under the obtained optimum conditions, low limits of detection (0.08-0.17 ng g-1) and quantification (0.27-0.57 ng g-1), satisfactory precision (relative standard deviations ≤ 5.0%), and wide linear range (0.57-500 ng g-1) with great coefficients of determination (r2≥ 0.9986) were obtained.

Automatic MDSPE Combined with DART-HRMS for the Rapid Quantitation of 21 Synthetic Cathinones in Urine.

A new, rapid, and automated method for the quantitation of 21 synthetic cathinones in urine was established using magnetic dispersive solid-phase extraction (MDSPE) in combination with direct analysis in real time-high-resolution mass spectrometry (DART-HRMS). Sample preparation and quantitation were verified by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methcathinone-D3, α-PVP-D8, and proadifen (SKF525A) were used as internal standards. Magnetic HLB extractant and NaH2PO4/NaOH buffer (0.2 M, pH 7) were used in automatic MDSPE. All 21 synthetic cathinones could be detected and analyzed by DART-HRMS in under 1 min. It was proven that the linearities of 21 synthetic cathinones were suitable (R2 > 0.99) in the concentration ranges of 0.5-100 ng/mL or 1-100 ng/mL. The precision and accuracy values were all within ±15%, and the samples were stable under various conditions. The average time of each sample from preprocessing to completion of detection was approximately 2 min, allowing for rapid sample analysis. The relative error (RE) of the concentrations obtained by DART-HRMS and LC-MS/MS were within ±13.61%, and the linear coefficient (R) was 0.9964. The results of DART-HRMS and LC-MS/MS provided equivalent values at the 95% confidence level. In summary, a simple, fast, and convenient quantitation method via DART-HRMS was established. This application can be utilized to reduce backlogs and promote rapid case processing.

One Pot Synthesis of Nanofiber-Coated Magnetic Composites as Magnetic Dispersive Solid-Phase Extraction Adsorbents for Rapid Determination of Tetracyclines in Aquatic Food Products.

A magnetic adsorbent based on a C-nanofiber (Fe3O4@C-NFs) nanocomposite was synthesized using a simple one-pot co-precipitation method. The characterized results showed that the obtained C-nanofiber-coated magnetic nanoparticles had many attractive features such as a large specific surface area and a highly interwoven and branched mesoporous structure, as well as distinguished magnetism. The nanocomposite was then used as an adsorbent in the magnetic solid phase extraction (MSPE) of four typical tetracyclines (oxytetracycline, tetracycline, chlortetracycline, and doxycycline) in aquatic products. The TCs in the extract were determined using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Experimental variables of MSPE, including the sorbent amount, pH condition, adsorption and desorption time, and desorption solvent, were investigated and optimized systematically. The method validation indicated that the developed method showed good linearity (R2 > 0.995) in the range of 1.0-200 ng/mL. The average recoveries at the spiked levels ranged from 90.7% to 102.7% with intra-day and inter-day relative standard deviations (RSDs, n = 6) ranging from 3.72% to 8.17% and 4.20% to 9.69%, respectively. The limit of detection (LOD) and limit of quantification (LOQ) for the four kinds of TCs were 0.7 µg/kg and 2.0 µg/kg, respectively. Finally, MSPE based on C-nanofiber-coated magnetic nanoparticles was successfully applied to TC analysis in real aquatic products (grass carp, large yellow croaker, snakehead, mandarin fish, Penaeus vannamei, swimming crab, etc.). Compared with traditional extraction methods, the proposed method for TC analysis in aquatic products is more sensitive, effective, recyclable, and environmentally friendly.

Polycarbonate-coated magnetic nanoparticles for the extraction of imipramine and its primary metabolite from urine.

This study introduces a reliable and inexpensive magnetic dispersive solid phase extraction to extract imipramine and its primary metabolite (desipramine) from urine samples. To accomplish this aim, Fe3 O4 magnetic nanoparticles were synthesized by sonication, subsequently, polycarbonate was precipitated gradually onto the surface of them to form the adsorbent. Extraction recoveries of 85% and 76%, enrichment factors of 57 and 51, limits of detection of 2.5 and 2.8 µg/L, and limits of quantification of 8.3 and 9.3 µg/L were obtained for imipramine and desipramine under the optimal conditions, respectively. In addition, relative standard deviations for intra- (n = 6) and inter-day (n = 5) precisions at two concentrations (50 and 100 µg/L of each analyte) were less than or equal to 4%. Short extraction time, good repeatability, high enrichment factors, and simplicity are the main advantages of the proposed method.

Amino acid ionic liquid-based magnetic dispersive solid-phase extraction for benzimidazole residue analysis in fruit juice and human serum based on theoretical screening.

The theoretical screening and design of green solvents to reduce organic solvents and to develop green and efficient sample pretreatment methods have attracted extensive attention. Here, benzimidazoles (BZDs) with potential reproductive toxicity were used as target compounds, and amino acid ionic liquids (AAILs) were designed and selected via a theoretical calculation. With the functionalized AAIL as monomers, and POSS as the crosslinking agent, novel specific magnetic nanoparticles (Fe3O4@SiO2@MAPs@AAIL-POSS) were prepared and used to develop the magnetic dispersive solid-phase extraction (MDSPE) of trace BZDs from fruit juice and human serum. In the evaluation of the method, Fe3O4@SiO2@MAPs@AAIL-POSS showed specific adsorption, recyclable ability, high adsorption efficiency, a good recovery rate, and a low coefficient of variation. In addition, the adsorption behavior of Fe3O4@SiO2@MAPs@AAIL-POSS on BZDs was verified by investigating the kinetic and thermodynamic of the adsorption process. The study design provides ideas for green rapid detection methods of other food pollutants.

Magnetic dispersive solid-phase extraction of some pesticides from fruit juices using monodisperse nanosorbent combined with dispersive liquid-liquid micro-extraction.

In this study, the new synthesized magnetic nanoparticles based on amorphous carbon have been used as a sorbent in magnetic dispersive solid-phase extraction prior to dispersive liquid-liquid micro-extraction. The developed method was applied for analysis of ten pesticides from different fruit juice samples by gas chromatography-flame ionization detection. In this work, a few mg of the sorbent is added into an aqueous solution containing the analytes. Adsorption and desorption of the compounds of interest are accelerated by vortexing and sonication, respectively. To achieve high enrichment factors, a suitable organic solvent (iso-propanol) is used to elute the target analytes from the nanosorbent. The obtained iso-propanol is phased and 1,1,2-trichloroethane are employed as the disperser and extraction solvents, respectively, in the following micro-extraction procedure. The synthesized magnetic nanoparticles were characterized by scanning electron microscope, X-ray diffraction, vibrating sample magnetometer, and Fourier-transform infrared spectrophotometer. To achieve the high extraction efficiency and optimum conditions, all parameters that could affect the extraction yield were investigated. Under optimum conditions, the method had broad linear ranges with a proper linearity (r2 ≥ 0.9987). Limits of detection and quantification for analysis of the selected pesticides were found in the ranges of 0.5-1.0 and 1.7-3.3 µg L-1, respectively. High enrichment factors and extraction recoveries were obtained in the ranges of 321-438 and 64-88%, respectively. To evaluate repeatability of the method, it was performed on two sets of standard solutions at the concentrations of 10 and 50 µg L-1 (each analyte). Relative standard deviations varied in the ranges of 2-6% and 4-7% for intra- (n = 6) and inter-day (n = 5) precisions, respectively.

Magnetic solid-phase extraction based on GO/Fe3O4 coupled with UPLC-MS/MS for determining nitroimidazoles and their metabolites in honey.

A magnetic graphene oxide (GO/Fe3O4) nanocomposite was synthesized in one step by a chemical coprecipitation method, which was further used for magnetic solid-phase extraction (MSPE). This study aimed to combine GO/Fe3O4 with ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to detect the nitroimidazoles (NDZs) and their three major metabolites in honey samples. GO/Fe3O4 was characterized by transmission electron microscopy (TEM), Fourier transform-infrared (FT-IR) spectroscopy, and magnetic property measurement system (MPMS), and the influencing parameters such as adsorbent amount, pH of the dissolved sample solution, sample volume, type and volume of the eluent, shaking speed, and adsorption and desorption time were optimized. Under the optimized conditions, the limits of detection (LOD) and quantitation (LOQ) of the method were 0.003-0.08 µg kg-1 and 0.009-0.3 µg kg-1, respectively, with good linearity reported in the range of 0.5-20 µg kg-1 (R2 ≥ 0.9991). The average recoveries of 10 analytes were in the range of 66.0%-90.8% with relative standard deviations (RSD) lower than 6.9% (n = 6). The preparation of GO/Fe3O4 and the extraction process were convenient and rapid, and consumed small amounts of organic solvents. The optimized method was successfully applied for extracting NDZs and their three major metabolites from honey samples with good accuracy.

Green Synthesis of Molecularly Imprinted Polymers for Dispersive Magnetic Solid-Phase Extraction of Erythrosine B Associated with Smartphone Detection in Food Samples.

Monitoring synthetic colorants in foods is important due to their potential toxicity and pathogenicity. We propose here a new and simple method for the extraction and determination of erythrosine B (ERT-B) in food samples. A composite of polydopamine-based molecularly imprinted polymers coating magnetic nanoparticles (Fe3O4@PDA@MIP) was synthesized using a green approach and exploited for the magnetic dispersive solid-phase extraction (MDSPE) of ERT-B. Fe3O4@PDA@MIP provides a rapid extraction of ERT-B, exhibiting good reusability and preconcentration ability. Moreover, the MIP showed a relatively good imprinting factor (3.0 ± 0.05), demonstrating excellent selectivity against patent blue (an interfering dye) and other food matrix components. The proposed MDSPE was coupled to colorimetric smartphone-based detection that allowed us to obtain similar performances of UV-Vis spectroscopy detection. The smartphone-based optical detection facilitated the determination of ERT-B in the 0.5-10 mg/L range, with a limit of detection of 0.04 mg/L. The developed method was successfully employed to determine ERT-B in food samples (juice, candy, and candied cherries) with good recovery values (82-97%).

Preparation and application of nano petal-shaped covalent organic frameworks modified polystyrene-divinylbenzene- glycidylmethacrylate microspheres for the extraction of illicit drugs from wastewater.

A novel nano petal-shaped covalent organic frameworks modified magnetic polystyrene-divinylbenzene-glycidylmethacrylate (NP-COF@Mag-PS/DVB/GMA) microsphere has been synthesized. It is a perfect combination of high productivity of PS/DVB/GMA microspheres and excellent enrichment efficiency of COF particles, and the excellent properties of NP-COF@Mag-PS/DVB/GMA microspheres are characterized by scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET) and X-ray photoelectron spectroscopy (XPS). The sorbent can extract illicit drugs via the reverse-phase interactions provided by benzene ring on the polymer backbone and the hydrogen bonding interactions provided by functional group (-NH-) on the COF particles. Based on using NP-COF@Mag-PS/DVB/GMA as sorbents, an easiness-to-handle of magnetic dispersive solid phase extraction (Mag-dSPE) procedure is proposed for the simultaneous preconcentration of 12 illicit drugs from wastewater. The obtained results show high extraction efficiency of NP-COF@Mag-PS/DVB/GMA to illicit drugs with recoveries between 81.6 and 116%. Furthermore, a liquid chromatography-tandem quadrupole mass spectrometry (LC-MS/MS) method for the determination of 12 illicit drugs from wastewater at sub-ppt levels has been proposed and validated with the pretreatment of samples by Mag-dSPE. The limits of quantification (LOQs) for the 12 illicit drugs are between 0.40 and 4.90 ng/L. Validation results on linearity, specificity, trueness and precision, as well as on application to the analysis of 12 illicit drugs in ten real samples demonstrate the applicability to environment monitoring analysis.

Heterogeneous adsorbent based on CeZrO2 nanoparticles doped magnetic graphene oxide used for vortex assisted magnetic dispersive solid phase extraction of erythromycin in chicken.

A simple, fast, and efficient method of vortex assisted magnetic dispersive solid phase extraction for separation and pre-concentration of erythromycin in chicken samples prior to high LC-UV determination has been developed. The novel heterogeneous CeZrO2 nanoparticles doped magnetic graphene oxide, for use as an efficient nanosorbent, was synthetised and applied for the adsorption of erythromycin. The synthetised nanosorbent was characterised using both Fourier-transform infra-red (FT-IR) and energy dispersive X-Ray (EDX) spectroscopy together with field emission scanning electron microscopy-EDX. To obtain the best extraction condition and maximum extraction efficiency of erythromycin, the effect of important parameters including pH, amount of sorbent, vortexing time, ionic strength, sample volume, and desorption conditions were investigated. At optimum conditions, a linear range of 0.25-300 µg kg-1, LOD (S/N = 3) of 0.079 µg kg-1, and LOQ (S/N = 10) of 0.270 µg kg-1 were obtained. The precision of the method was established as having an RSD (%) at 100 µg kg-1 of erythromycin for seven replicates of 2.6% and 3.2% for the intra-day and the inter-day, respectively. Recoveries over 94.0% confirmed a high capability of the proposed method for separation and determination of erythromycin residues in chicken being one of the most important animal products.

Sensitive and selective magnetic dispersive microextraction of diazinon from urine samples by molecularly imprinted polymer based on core-shell metal-organic frameworks.

A core-shell magnetic metal-organic framework (Fe3O4 SiO2/ PAEDTC@ MIL- 101 (Fe)) was synthesized as the substrate and then covered with a surface molecularly imprinted polymer (MIP) layer. Next, Fe3O4 SiO2/ PAEDTC@ MIL- 101 (Fe) @ MIP was characterized by XRD, FT-IR, BET, VSM, TEM, and FE-SEM techniques and applied for selective, fast, and sensitive magnetic dispersive solid-phase microextraction (M-DµSPE) of diazinon from urine samples by the GC- FID detection method. The key experimental variables affecting M-DµSPE were studied and optimized by central composite design (CCD). Under optimum conditions (5 mL; sample at pH: 7.0, the mass of solid sorbent; 6 mg, extraction time; 4 min, acetonitrile as an eluent solvent; 1.5 mL, and desorption time; 3 min, and then reconstituted with 100 µL of methanol), the proposed method exhibits high sensitivity with limits of detection and quantification of 0.005 and 0.017 ng mL-1, respectively. Excellent extraction recovery (98.5 %), wide linearity range (0.02-200000 ng mL-1, R2 > 0.992), high enrichment factors (47-53), and satisfactory precision (<6.3 % RSD) were achieved. The MIP- MOF@ M-DµSPE -GC-FID method can be used with high precision and wide linearity to extract and analyze trace levels of diazinon in real urine samples.

Magnetic dispersive solid-phase extraction of some polycyclic aromatic hydrocarbons from honey samples using iron (III) oxinate nanocomposite as an efficient sorbent.

In this work, iron (III) oxinate magnetic nanocomposite was synthesized and employed as an efficient sorbent for the magnetic dispersive solid-phase extraction of some polycyclic aromatic hydrocarbons from honey samples. In the following, dispersive liquid-liquid microextraction procedure was used for further preconcentration of the analytes. The prepared sorbent was characterized using Fourier transform infrared spectrophotometry, X-ray diffractometry, vibrating sample magnetometry, energy dispersive X-ray spectroscopy, and scanning electron microscopy. The results verified the successful formation of the magnetic sorbent. In the extraction process, the sorbent was added into an aqueous solution and the mixture was vortexed. After completing the adsorption process, the supernatant phase was separated in the presence of a magnet and the analytes adsorbed onto sorbent were eluted by acetonitrile. Then, microliter-level 1,1,1-trichloroethane was mixed with the obtained acetonitrile and injected into NaCl solution. Finally, one microliter of the sedimented phase was injected into gas chromatography-flame ionization detector after centrifugation. Under the optimum conditions, a great repeatability (relative standard deviation equal or less than 5 and 6% for intra- and interday precisions, respectively), acceptable extraction recoveries (59-84%), high enrichment factors (118-168), and low limits of detection and quantification (0.16-0.36 and 0.56-1.22 ng/g, respectively) were acquired.

Ionic liquid-based magnetic nanoparticles for magnetic dispersive solid-phase extraction: A review.

Due to their highly tunable nature and outstanding physicochemical properties, ionic liquids (ILs) have been widely reported for use in the synthesis of multitudinous magnetic nanoparticles (MNPs). IL-based magnetic nanoparticles (IL-MNPs) have great potential in magnetic dispersive solid-phase extraction (MDSPE). At present, IL-MNPs have been successfully applied in the pretreatment of MDSPE samples from medicines, pesticides, veterinary drugs, heavy metals, dyes, additives, and proteins in agricultural products, foods and beverages, environmental water, and biological samples. In this review, the preparation of IL-MNPs and their application in MDSPE are comprehensively summarized. The structural characteristics of the introduced ILs used to prepare the IL-MNPs and the synthetic routes employed to obtain the IL-MNPs are described, including physical coating and chemical bonding methods. The IL-MNPs are then classified and described according to different modified materials, including silica-based materials, carbon-based materials, metal-organic frameworks, molecularly imprinted polymers and other interesting large/small molecules. Finally, the research prospects and development directions of IL-MNPs in the context of MDSPE are further identified.

Polydopamine-coated magnetic Spirulina nanocomposite for efficient magnetic dispersive solid-phase extraction of aflatoxins in pistachio.

An efficient adsorbent was synthesized and used in magnetic dispersive solid phase extraction (MDSPE) of aflatoxins B1, B2, G1, and G2 at trace levels in pistachio prior to analysis by HPLC equipped with a fluorescence detector. Spirulina (Sp) algae was first magnetized, followed by surface modification with dopamine (Dp). The adsorbent was characterized using FT-IR, XRD, FE-SEM, EDX, VSM, and BET analyses. The effects of different analytical parameters on the extraction performance were evaluated. Under optimal conditions, good limits of detection (LODs) and quantifications (LOQs) were achieved in the ranges of 0.02-0.07 and 0.06-0.21 ng g-1, respectively. The RSDs were 5.9, 6.3, 5.6, and 7.3% for AFB1, G1, B2, and G2, respectively. The proposed method was successfully used to determine AFs in pistachio samples and acceptable recoveries in the range of 72-95% were obtained.

Magnetic dispersive solid phase extraction based on carbonized cellulose-ferromagnetic nanocomposite for screening phthalate esters in aqueous samples.

In this work, a sorbent of the carbonized cellulose-ferromagnetic nanocomposite has been proposed for the magnetic dispersive solid phase extraction of some plasticizers in aqueous samples. Carbonized cellulose nanoparticles were prepared by treatment of cellulose filter paper with concentrated sulfuric acid and then loaded on Fe3O4 nanoparticles using coprecipitation. This sorbent is compatible with aqueous samples and can be considered as a viable sorbent for extraction of plasticizers from aqueous samples. In this study, magnetic dispersive solid phase extraction is followed by a dispersive liquid-liquid microextraction method. This combination makes the proposed approach as an efficient clean-up method with high enrichment factors for the selected analytes. The enriched analytes are monitored by gas chromatography equipped with a flame ionization detector. Parameters affecting the method efficiency were investigated in details. Under the optimized extraction conditions, limits of detection could reach up to of 0.15-0.50 µg L-1. The satisfactory enrichment factors of 286-403 were obtained, and the extraction recoveries were found to be in the range of 57-80%. Relative standard deviations were in the range of 3-7% for intra-day and inter-day precisions for six replicate extractions at 25 µg L-1 of each plasticizer. Calibration curves were linear in wide ranges with coefficients of determination ≥ 0.995. Eventually, efficiency of the prepared sorbent was confirmed by the extraction of some plasticizers from real samples including fruit juices, mineral water, injection solution, cola, and yoghourt drink packed in plastic containers.

Eco-friendly fabrication of a magnetic dual-template molecularly imprinted polymer for the selective enrichment of organophosphorus pesticides for fruits and vegetables.

A magnetic dual-template molecularly imprinted polymer (DMIP) was successfully prepared in an aqueous medium and used as a sorbent for the selective extraction of organophosphorus pesticides prior to analysis by high-performance liquid chromatography (HPLC). The binding properties and selectivity of DMIP toward organophosphorus were evaluated and compared with those of a non-imprinted polymer. The established magnetic dispersive solid-phase extraction (MDSPE) method using DMIP exhibited fast enrichment of the target analytes within 60 s for adsorption and 30 s for desorption. Good linearities in the range of 0.5-2000 µg L-1 with coefficients of determination (R2) greater than 0.9930 were observed. The method provides low limits of detection of 0.062-0.195 µg L-1 and limits of quantification of 0.210-0.640 µg L-1 with relative standard deviations of less than 9.5% for intra- and inter-day analyses. The enrichment factors ranged from 464 to 621. Satisfactory recoveries ranged from 81.3 to 110.0% with relative standard deviations below 11%.

Development of a magnetic dispersive solid phase extraction method by employing folic acid magnetic nanoparticles as an effective, green, and reliable sorbent followed by dispersive liquid-liquid microextraction for the extraction and preconcentration of seven pesticides from fruit juices.

Folic acid magnetic nanoparticles have been prepared and utilized as an effective and reliable sorbent in magnetic dispersive solid phase extraction combined with dispersive liquid-liquid microextraction for the extraction of seven pesticides from different juices before their determination by gas chromatography-flame ionization detector. The sorbent is prepared through ball milling process using a proper mixture of folic acid and magnetic iron oxide. Characterization of the sorbent was done with X-ray diffraction pattern, scanning electron microscopy, and vibrating sample magnetometry. In the current study, limits of detection were in the range 0.12-0.33 µg L-1. Relative standard deviations at a concentration of 40 µg L-1 of each analyte were in the ranges of 2.15-5.14% for intra-day (n = 6) and 3.78-6.91% for inter-day (n = 4) precisions. Extraction recoveries and enrichment factors were obtained in the ranges of 70-88 % and 566-708, respectively. The performance of the method was evaluated by determination the selected pesticides in different samples. Graphical Abstract.