Surfactant modified coconut husk fiber as a green alternative sorbent for micro-solid phase extraction of triazole fungicides at trace level in environmental water, soybean milk, fruit juice and alcoholic beverage samples.

In this work, micro-solid phase extraction using surfactant modified biosorbent was investigated for trace level determination of triazole fungicides prior to their analysis by high performance liquid chromatography. Coconut husk fiber (CHF) was selected as an effective biosorbent in the extraction process. Fourier transform infrared spectrometry, scanning electron microscopy and transmission electron microscopy methods were used to characterize the modified biosorbent. Various factors affecting the extraction efficiency of the proposed method were studied including the amount of coconut husk fiber biosorbent (0.1 g), kind and concentration of surfactant as a modifier (sodium dodecyl sulfate, 10 mmol L-1), kind and volume of desorption solvent (methanol, 150 µL), and extraction period (including vortex adsorption time, centrifugation adsorption time, vortex desorption time and centrifugation adsorption time approximately 10 min). Under the selected conditions, the calibration plot was found to be linear in the range of 9-300 µg L-1 with a coefficient for determination of greater than 0.99. The limits of detection and limits of quantification for the studied triazole fungicides were 3.00 and 9.00 µg L-1, respectively. Finally, the proposed method was successfully applied to determine triazole fungicides in environmental water, soybean milk, fruit juice and alcoholic beverage samples with acceptable recoveries obtained in the range of 67.0% to 105.0%.

Biomass waste-derived magnetic material coated with dual-dummy-template molecularly imprinted polymer for simultaneous extraction of organophosphorus and carbamate pesticides.

An eco-friendly biomass waste-derived magnetic material coated with a dual-dummy-template molecularly imprinted polymer was fabricated using aqueous ethanol as a green porogen, lower amounts of toxic compounds as template molecules, and tyrosine and tryptophan as biocompatible binary monomers. The binding characteristics and selectivity of the material toward pesticides were assessed. High adsorption capacities ranging from 150.11 to 509.09 mg g-1 and imprinting factors reaching 2.2 were achieved within just 30 s. The material was applied for extraction of organophosphorus and carbamate pesticides prior to HPLC analysis. Under the optimum conditions, low limits of detection and quantitation were achieved, with ranges of 0.05-1.49 µg/L and 0.18-5.00 µg/L, respectively. The established approach enables efficient analysis of vegetable and fruit samples, yielding satisfactory recoveries ranging between 80 and 110 %. The method showed promise as an analytical method for the sensitive enrichment of pesticide residues in vegetable and fruit samples.

Molecularly imprinted polymer-coated paper for the selective extraction of organophosphorus pesticides from fruits, vegetables, and cereal grains.

Biodegradable molecularly imprinted polymer-coated paper (MIP@paper) was effectively produced by polymerization using azinphos-methyl as a template molecule, terephthalic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linker, and aqueous ethanol as a green porogenic solvent. The material was subsequently composited onto cellulose paper, which served as the natural substrate, by dip coating with the aid of chitosan and citric acid natural adhesive. The properties, such as static and dynamic adsorption, selectivity, and reusability, were assessed. At rapid adsorption equilibrium (10 min), the MIP@paper had a high adsorption capacity in the range of 2.5-3.7 mg g-1 and good recognition with imprinting factors up to 2.1. In addition, the proposed MIP@paper was utilized efficiently as a sorbent for dispersive solid phase extraction (d-SPE) of eight organophosphorus pesticides (OPPs) prior to high-performance liquid chromatography (HPLC) analysis. The d-SPE-HPLC method displayed low detection limits of 1.2-4.5 µg kg-1 and significant enrichment factors (up to 320-fold). The proposed method was effectively applied for the determination of OPP residues in agricultural products, including fruits, vegetables, and cereal grains, with satisfactory spiked recoveries (80.1-119.1 %). Thus, the MIP@paper material provided a selective and environmentally favorable method for extracting and determining organophosphorus pesticides.

A magnetic molecularly imprinted polymer based on an eco-friendly deep eutectic solvent for the selective recognition of dichlorodiphenyl trichloroethane and its degradation products in fruits and vegetables.

A new magnetic molecularly imprinted polymer was successfully synthesized using a ternary deep eutectic solvent derived from caffeic acid-choline chloride-formic acid as a functional monomer, thymol-menthol deep eutectic solvent as a template, ethylene glycol dimethacrylate as a cross-linker, potassium peroxodisulfate as an initiator, and aqueous ethanol solution (90% (v/v)) as a porogen. The synthesized material was characterized and applied for magnetic solid-phase extraction of dichlorodiphenyl trichloroethane and its degradation products. Optimization of the extraction condition was carried out using the central composite design and response surface methodology. The good analytical performance of magnetic solid phase extraction/gas chromatography‒mass spectrometry using the proposed adsorbent shows a wide linear range of 0.07-500 ng g-1 with R2 greater than 0.992. Low detection limits and quantitation limits were observed in the ranges of 0.01-2.00 ng g-1 and 0.07-2.50 ng g-1, respectively. The precisions shown in terms of relative standard deviations were lower than 7.0% for intraday (n=5) and 8.6% for interday (n=5 × 3) experiments. The proposed method was applied for preconcentration and determination of dichlorodiphenyl trichloroethane and its degradation products in fruit and vegetable samples. The satisfactory recoveries of the real samples at three spiked concentrations were obtained in the range of 79.1%-110.9% with RSDs lower than 7.5%. The findings highlight the importance of developing efficient sorbents for the enrichment of persistent organic pollutants in food matrices.

Trace-Level Determination of Triazole Fungicides Using Effervescence-Assisted Liquid-Liquid Microextraction Based on Ternary Deep Eutectic Solvent Prior to High-Performance Liquid Chromatography.

A simple and sensitive preconcentration method, namely, effervescence-assisted liquid-liquid microextraction based on the ternary deep eutectic solvent method, was developed for enrichment of triazole fungicide residues prior to their determination by high-performance liquid chromatography coupled with UV detection. In this method, a ternary deep eutectic solvent (as extractant) was prepared by combination of octanoic acid, decanoic acid, and dodecanoic acid. The solution was well dispersed with sodium bicarbonate (as effervescence powder) without using auxiliary devices. In order to obtain relatively high extraction efficiency, analytical parameters were investigated and optimized. Under optimum conditions, the proposed method showed good linearity within the range of 1-1000 µg L-1 with a coefficient for determination (R2) greater than 0.997. The low limits of detection (LODs) were in the range of 0.3-1.0 µg L-1. The precisions were assessed from the relative standard deviations (RSDs) of retention time and peak area obtained from intra- (n = 3) and inter-day (n = 5 × 5) experiments, which were greater than 1.21 and 4.79%, respectively. Moreover, the proposed method provided high enrichment factors ranging from 112 to 142 folds. A matrix-match calibration method was used for analysis of real samples. Finally, the developed method was successfully applied for determination of the triazole fungicide in environmental water (near agricultural area), honey, and bean samples, and it represents a promising alternative method for analysis of triazoles. The recoveries of the studied triazoles were obtained in the range of 82-106% with an RSD less than 4.89.

A ternary deep eutectic solvent-modified magnetic mixed iron hydroxide@MIL-101(Cr)-NH2 composite as a sorbent in magnetic solid phase extraction of organochlorine pesticides prior to GC-MS.

A green solvent of ternary deep eutectic solvent (menthol-thymol-dodecanoic acid) was prepared and used as a functional reagent to modify a magnetic mixed iron hydroxide@MIL-101(Cr)-NH2 composite. The proposed sorbent (MIH@MIL-101(Cr)-NH2-TDES) was applied in magnetic solid phase extraction (MSPE) for the enrichment of organochlorine pesticides. The analytes were quantitively analyzed by GC-MS. The relationships of experimental parameters for preparing the proposed sorbent and the MSPE method were studied through a Box-Behnken design and a central composite design, respectively. Their optimized conditions were investigated using response surface methodology. Application of the MIH@MIL-101(Cr)-NH2-TDES sorbent in MSPE successfully enhanced the sensitivity of GC-MS analysis, giving enrichment factors in the range of 56-168. The MSPE/GC-MS method was developed using MIH@MIL-101(Cr)-NH2-TDES as a sorbent and was successfully employed for the preconcentration/determination of organochlorine residues in honey and tea samples. The satisfactory detection limits were in the ranges of 0.07-0.80 ng g-1 and 0.7-8.5 ng g-1 for honey and tea samples, respectively. Acceptable recoveries were obtained in the ranges of 81.7-107.3% and 85.4-109.3% for the spiked honey and tea samples, respectively, with RSDs lower than 10.0%.

A biobased magnetic dual-dummy-template molecularly imprinted polymer using a deep eutectic solvent as a coporogen for highly selective enrichment of organophosphates.

An eco-friendly magnetic dual-dummy-template molecularly imprinted polymer (MDDMIP) was prepared by a "one-pot" green synthesis using mixed-valence iron hydroxide as the magnetic material, a deep eutectic solvent as the coporogen, and caffeic acid and glutamic acid as binary monomers. The adsorption properties toward organophosphorus pesticides (OPPs) were investigated. High adsorption capacities (269.65-304.93 mg g-1), quick adsorption times (20 s), and high imprinting factors (2.28-3.83) were obtained. The proposed MDDMIP was utilized for magnetic solid phase extraction (MSPE) of OPPs prior to quantification by high performance liquid chromatography (HPLC). The developed method exhibited outstanding linearity (0.05-500 µg L-1), low detection limits (0.003-0.015 µg L-1), and excellent enrichment factors (940-1310 folds). The MSPE-HPLC method was successfully applied for the detection of OPPs in vegetable, fruit, and grain samples with acceptable recoveries (80-119%). This method is a good potential method for the analysis of pesticide residues in complex matrices.

Modified Peanut Shell as an Eco-Friendly Biosorbent for Effective Extraction of Triazole Fungicide Residues in Surface Water and Honey Samples before Their Determination by High-Performance Liquid Chromatography.

An eco-friendly sample preparation method that is based on the use of a modified peanut shell as an efficient biosorbent for the extraction of triazole residues before their analysis by high-performance liquid chromatography was reported. The four triazole fungicides were separated on a Purospher STAR RP-18 endcapped (4.6 × 150 mm, 5 µm) column with a mobile phase of 50% (v/v) acetonitrile at a flow rate of 1.0 mL min-1 and detection wavelength set at 220 nm. Peanut shells modified by didodecyldimethylammonium bromide were selected as an effective biosorbent material in the microextraction method. Scanning electron microscopy, transmission electron microscopy, and Fourier transform infrared spectroscopy were used to characterize the biosorbent. The effect of dominant parameters on the proposed microextraction method including the amount of sorbent, kind and concentration of surfactant, sodium hydroxide concentration, kind and amount of salt, sample volume, adsorption time, kind and volume desorption solvent, and desorption time was studied. Under the optimum condition, a good analytical performance for the proposed microextraction method was obtained with a wide linear range within the range of 9-1000 µg L-1, and low limits of detection (0.03 µg L-1 for all analytes) were obtained. Enrichment factors were achieved within the range of 30-51. The intra and interday precision values were evaluated in terms of percentage relative standard deviations (%RSD) and were less than 0.09 and 5.34% for the retention time and peak area, respectively. The proposed microextraction methods were used for extraction and analysis of triazole fungicides in water and honey samples. The recoveries in a satisfactory range of 70.0-118.8% were obtained.

An In Situ Formation of Ionic Liquid for Enrichment of Triazole Fungicides in Food Applications Followed by HPLC Determination.

An in situ formation of ionic liquid was used for preconcentration of four triazole fungicides in food samples. The microextraction method was used for the first time in the literature for preconcentration of triazole fungicides. In the developed method, tributylhexadecylphosphonium bromide ([P44412]Br) and potassium hexafluorophosphate (KPF6) were used for the formation of hydrophobic ionic liquid. After centrifugation, the fine microdroplets were produced in one step, providing the extraction step in a quick and environmentally friendly manner. The functional group of the hydrophobic ionic liquid was investigated using FT-IR. Various extraction parameters were studied and optimized. In the extraction method, 0.01 g of [P44412]Br and 0.01 g of KPF6, centrifugation at 4500 rpm for 10 min were used. The optimized technique provided a good linear range (90-1000 µg L-1) and high extraction recovery, with a low limit of detection (30-50 µg L-1). Methods for the proposed in situ formation of ionic liquid were successfully applied to honey, fruit juice, and egg matrices. The recoveries were obtained in a satisfactory range of 62-112%. The results confirmed the suitability of the proposed microextraction method for selective extraction and quantification of triazole fungicides.

Natural deep eutectic solvent-decorated magnetic layered double hydroxide as a sorbent for the enrichment of organochlorine pesticides in environmental samples.

A newly designed magnetic layered double hydroxide composite modified with a natural deep eutectic solvent derived from choline chloride and sucrose was synthesized and applied as a sorbent for the enrichment of organochlorine pesticides. The magnetic solid phase extraction (MSPE) procedure was optimized via a small central composite design and response surface methodology. The MSPE method was able to preconcentrate the organochlorine residues in environmental samples prior to GC-MS analysis. Good analytical performance of the proposed method was observed with an enrichment factor of up to 158 and low limits of detection in the ranges of 0.002-0.015 µg·L-1 and 0.03-0.10 ng·g-1 for water and soil, respectively. Satisfactory recoveries for spiked water and soil samples were obtained in the ranges of 80.9-104.7% (RSDs<7.9) and 88.8-104.1% (RSDs<7.3), respectively. This finding highlights the role of natural deep eutectic solvents as modifying agents for magnetic layered double hydroxides, which enhance the efficiency of extraction of the target analytes. The developed MSPE/GC-MS procedure was sensitive and reliable for the determination of trace organochlorine residues in environmental samples.

Magnetic Solid-Phase Extraction of Carbamate Pesticides Using Magnetic Metal-Organic Frameworks Derived from Benzoate Ligands, Followed by Digital Image Colorimetric Screening and High-Performance Liquid Chromatography Analysis.

Magnetic sorbents based on iron-aluminum-mixed metal hydroxides composited with metal-organic frameworks (MOFs) were designed and synthesized using different benzoate ligands, including terephthalic acid, 2-aminoterephthalic acid, 2,5-dihydroxyterephthalic acid, 1,3,5-benzenetricarboxylic acid, and 1,2,4,5-benzenetetracarboxylic acid. The magnetic MOF derived from terephthalic acid ligand exhibited an excellent extraction efficiency, with adsorption capacities in the range of 2193-4196 mg kg-1, and was applied for magnetic solid-phase extraction (MSPE) of carbamate pesticides, that is, bendiocarb, carbosulfan, carbofuran, carbaryl, propoxur, isoprocarb, and promecarb. Simple digital image colorimetry based on the diazotization reaction and high-performance liquid chromatography (HPLC) were utilized for fast screening and quantification purposes, respectively. A good analytical performance for a simple screening approach using portable equipment was obtained with detection limits in the range of 1.0-18.0 µg L-1. Under the optimized MSPE-HPLC conditions, the entire developed procedure provided a wide linear range between 0.015 and 1000 µg L-1, low limits of detection, and limits of quantitation ranging from 0.005 to 0.090 and 0.015-0.300 µg L-1, respectively. Enrichment factors up to 184 were achieved. The intra- and interday relative standard deviations were below 6.7 and 9.4%, respectively. The proposed MSPE-digital image colorimetry and MSPE-HPLC methods were successfully applied for screening and determining carbamate pesticides in fruits and vegetables. The recoveries were obtained in a satisfactory range of 71.5-122.8%. This discovery has led to the development of integration methods using newly synthesized sorbent materials for the enrichment of carbamate pesticides prior to their analysis in complicated samples. The developed MSPE coupled with digital image colorimetry was efficient for fast carbamate contamination screening, while MSPE-HPLC offered a sensitive analytical methodology for quantifying contaminated samples.

A water-compatible magnetic dual-template molecularly imprinted polymer fabricated from a ternary biobased deep eutectic solvent for the selective enrichment of organophosphorus in fruits and vegetables.

A water-compatible magnetic dual template molecularly imprinted polymer using a ternary deep eutectic solvent as a functional monomer was synthesized via a green synthesis method based on one-pot reversible addition/fragmentation chain transfer precipitation polymerization. The resulting material, DES-MDMIP, shows excellent adsorption capacity (218.62 mg g-1) in rapid adsorption time (30 s) and outstanding selectivity factors of 4.45 for organophosphorus pesticides. The sorbent was applied in magnetic solid-phase extraction prior to HPLC analysis. The developed methodology provides linearity between 0.05 and 2000.00 µg L-1. Low detection limits of 0.015-0.030 µg L-1 and enrichment factors of up to 691 were achieved. The applicability of the method facilitates the efficient determination of fruit and vegetable samples with satisfactory recoveries in the range of 80-117%. The newly designed water-compatible DES-MDMIP sorbent, along with a simple and rapid extraction process, demonstrated a powerful analytical approach for the practical analysis of pesticide residues.

Co-precipitation based on layered double hydroxides and anionic surfactants for preconcentration of six benzoylurea insecticides in soft drinks before simultaneous analysis by high-performance liquid chromatography.

Layered-double hydroxides (LDHs) modified with anionic surfactants via a co-precipitation method were developed for preconcentrating and simultaneous analysis of six benzoylurea insecticides (BUs) by high-performance liquid chromatography (HPLC). The anionic surfactants with different chain lengths, including sodium dodecylbenzene sulfonate (SDBS), sodium dodecyl sulfate (SDS), sodium 1-nonane sulfonate (SNS), and sodium 1-hexane sulfonate monohydrate (SHS) were investigated to improve the extraction efficiency of LDHs. The SDBS-LDHs provided the highest efficiency for the enrichment of the BUs studied. Under the chosen conditions, enrichment factors in the range of 38-69 and detection limits in the range of 0.1-0.3 µg L-1 were achieved. Good reproducibilities (RSD < 13.8%) and recoveries (71.4-118.7%) were also obtained. The proposed preconcentration method, used as an in situ procedure offers rapid and simple simultaneous preparation of LDHs and extraction of BUs. The method was successfully applied for residue analysis of BUs in fruit- and flower-derived soft drink samples.

In-Situ Formation of Modified Nickel-Zinc-Layered Double Hydroxide Followed by HPLC Determination of Neonicotinoid Insecticide Residues.

A single-step preconcentration procedure using the in-situ formation of modified nickel-zinc-layered double hydroxides (LDHs) prior to high-performance liquid chromatography (HPLC) is investigated for the determination of neonicotinoid insecticide residues in honey samples. The LDHs could be prepared by the sequential addition of sodium hydroxide, sodium dodecyl sulfate, nickel nitrate 6-hydrate and zinc nitrate 6-hydrate, which were added to the sample solution. The co-precipitate phase and phase separation were obtained by centrifugation, and then the precipitate phase was dissolved in formic acid (concentrate) prior to HPLC analysis. Various analytical parameters affecting extraction efficiency were studied, and the characterization of the LDHs phase was performed using Fourier-transformed infrared spectroscopy and scanning electron microscopy. Under optimum conditions, the limit of detection of the studied neonicotinoids, in real samples, were 30 µg L-1, for all analytes, lower than the maximum residue limits established by the European Union (EU). The developed method provided high enrichment, by a factor of 35. The proposed method was utilized to determine the target insecticides in honey samples, and acceptable recoveries were obtained.

Dissolvable Mg/Al layered double hydroxides and surfactant as an extractant for trace analysis of benzoylurea insecticides by high performance liquid chromatography.

A rapid and simple preconcentration method using dissolvable Mg/Al layered-double hydroxides (LDHs) and high performance liquid chromatography-photodiode array detection (HPLC-PDA) was developed for the analysis of benzoylurea insecticides (BUs) in water and honey samples. The proposed dissolvable LDHs for the extraction can be prepared in one step by the sequential addition of sodium hydroxide, magnesium chloride, aluminium chloride, and sodium dodecyl sulfate into the sample solution containing the target BUs. The co-precipitate phase was simply obtained after centrifugation, and the phase was then dissolved with formic acid before analysis by HPLC. The developed method provided an enrichment factor of 12.5-23.7. LODs were obtained in the range of 0.1-0.3 µg L-1 for deionized water, 0.2-2.0 µg L-1 for environmental waters, and 0.5-2.0 µg L-1 for the analyzed honey samples. Good recoveries ranging from 78.4 to 117.8% and 72.7 to 117.9% for water and honey samples, respectively, were obtained.

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.

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.

ß-Cyclodextrin Assisted Liquid-Liquid Microextraction Based on Solidification of the Floating Organic Droplets Method for Determination of Neonicotinoid Residues.

An efficient and environment-friendly microextraction method, namely, ß-cyclodextrin assisted liquid-liquid microextraction, based on solidification of the floating organic droplets method coupled with HPLC is investigated for the sensitive determination of trace neonicotinoid pesticide residues. In this method, ß-cyclodextrin is used as a disperser solvent, while 1-octanol is selected as an extraction solvent. ß-cyclodextrins was found to decrease interfacial tension and increase the contact area between the organic and water phases with the help of centrifugation. A cloudy solution was rapidly formed and then centrifuged to complete phase separation. Various key parameters influencing extraction efficiency were systematically investigated and optimized; they include salt addition, concentration of ß-cyclodextrin, and volume of extraction solvent (1-octanol). Under optimum conditions, good linearity was obtained with coefficient for determination (R2) greater than 0.99. A low limit of detection, high enrichment factor, and good recovery (83 - 132) were achieved. This proves that the proposed method can be applied to determine trace neonicotinoid pesticide residues in natural surface water samples.

Magnetic Stirring Assisted Demulsification Dispersive Liquid⁻Liquid Microextraction for Preconcentration of Polycyclic Aromatic Hydrocarbons in Grilled Pork Samples.

A simple microextraction method, magnetic stirring assisted demulsification dispersive liquid⁻liquid microextraction, for preconcentration of five polycyclic aromatic hydrocarbons (fluorene, phenanthrene, anthracene, fluoranthrene, and pyrene) was investigated prior to analysis by high performance liquid chromatography. In this method, a mixture of extraction solvent and disperser solvent was rapidly injected into sample solution. The magnetic stirrer agitator aided the dispersion of the extraction solvent into the sample solution. After the formation of an emulsion, the demulsifier was added, resulting in the rapid separation of the mixture into two phases. No centrifugation step was required. Several parameters affecting the extraction efficiency of the proposed method were studied, including addition of salt, kind and volume of extraction solvent, volume of demulsifier solvent, and extraction times. Under the optimum conditions, high enrichment factor, low limit of detections (LODs) and good precision were gained. The proposed method was successfully applied to analysis of polycyclic aromatic hydrocarbon residues in grilled pork samples.

Ultrasonically Modified Amended-Cloud Point Extraction for Simultaneous Pre-Concentration of Neonicotinoid Insecticide Residues.

An effective pre-concentration method, namely amended-cloud point extraction (CPE), has been developed for the extraction and pre-concentration of neonicotinoid insecticide residues. The studied analytes including clothianidin, imidacloprid, acetamiprid, thiamethoxam and thiacloprid were chosen as a model compound. The amended-CPE procedure included two cloud point processes. Triton™ X-114 was used to extract neonicotinoid residues into the surfactant-rich phase and then the analytes were transferred into an alkaline solution with the help of ultrasound energy. The extracts were then analyzed by high-performance liquid chromatography (HPLC) coupled with a monolithic column. Several factors influencing the extraction efficiency were studied such as kind and concentration of surfactant, type and content of salts, kind and concentration of back extraction agent, and incubation temperature and time. Enrichment factors (EFs) were found in the range of 20⁻333 folds. The limits of detection of the studied neonicotinoids were in the range of 0.0003⁻0.002 µg mL−1 which are below the maximum residue limits (MRLs) established by the European Union (EU). Good repeatability was obtained with relative standard deviations lower than 1.92% and 4.54% for retention time (tR) and peak area, respectively. The developed extraction method was successfully applied for the analysis of water samples. No detectable residues of neonicotinoids in the studied samples were found.