基于十八烷基三甲基溴化铵修饰的磁性粒子在线磁性固相萃取-高效液相色谱法测定水样中磺酰脲类农药

采用溶胶-凝胶法制备表面修饰了十八烷基三甲基溴化铵的磁性粒子作为萃取剂，研制了一种在线磁性固相萃取（on-line MSPE）装置，建立了on-line MSPE与高效液相色谱联用测定水样中两种磺酰脲类农药（氯磺隆、苄嘧磺隆）的方法。实验优化了在线磁性固相萃取条件并进行方法学考察，证明该方法具有良好的线性关系（两种目标物的线性相关系数均≥ 0.9997）和较低的检出限（两种目标物的检出限分别为0.32和1.12 μg/L）。将此法用于3种环境水样中两种磺酰脲类农药的检测，水样中均检出氯磺隆，均未检出苄嘧磺隆。两种目标物加标回收率为70.0%~113.4%。该方法高效、简便，在分离富集环境水样中磺酰脲类农药方面有一定的应用前景。     

Fabrication of highly crystalline covalent organic framework for solid-phase extraction of three dyes from food and water samples

Herein, a covalent organic framework, which was fabricated at room temperature by using 1,3,5-tris(p-formylphenyl) benzene and 1,3,5-tris(4-aminophenyl)benzene as building blocks, was employed as an adsorbent for solid-phase extraction of dyes including congo red, methyl blue and direct red 80 for the first time. The prepared covalent organic framework was properly characterized by different techniques and the results revealed that it had a uniform spherical structure, high crystallinity, satisfactory surface area, and good thermal stability. Moreover, the adsorption performance of the material was explored by using static and dynamic adsorption experiments and the results indicated that the material showed good adsorption capacities for three dyes with adsorption capacities in the range of 55.25–284.10 mg/g and the adsorption equilibrium can be achieved in 15 min. Further, to achieve the best adsorption effects of the material, the influence parameters such as pH, ionic strength, type of desorption solvent, and the material dosage in the solid-phase extraction column, were optimized in turn. Finally, under optimal conditions, the solid-phase extraction coupled with HPLC was applied to the analysis of dyes in food and water samples. The recoveries of dyes in actual samples were satisfactory, revealing the unique applicability of the material in the sample pretreatment field.     

Preparation of iron‐based MIL‐101 functionalized polydopamine@Fe3O4 magnetic composites for extracting sulfonylurea herbicides from environmental water and vegetable samples

Here, we describe a simple one‐pot solvothermal method for synthesizing MIL‐101(Fe)@polydopamine@Fe₃O₄ composites from polydopamine‐modified Fe₃O₄ particles. The composite was used as a magnetic adsorbent to rapidly extract sulfonylurea herbicides. The herbicides were then analyzed by high‐performance liquid chromatography. The best possible extraction efficiencies were achieved by optimizing the most important extraction parameters, including desorption conditions, extraction time, adsorbent dose, salt concentration, and the pH of the solution. Good linearity was found (correlation coefficients >0.9991) over the herbicide concentration range 1–150 μg/L using the optimal conditions. The limits of detection (the concentrations giving signal/noise ratios of 3) were low, at 0.12–0.34 μg/L, and repeatability was good (the relative standard deviations were <4.8%, n = 6). The method was used successfully to determine four sulfonylurea herbicides in environmental water and vegetable samples, giving satisfactory recoveries of 87.1–108.9%. The extraction efficiency achieved using MIL‐101(Fe)@polydopamine@Fe₃O₄ was compared with the extraction efficiencies achieved using other magnetic composites (polydopamine@Fe₃O₄, Hong Kong University of Science and Technology (HKUST)‐1@polydopamine@Fe₃O₄, and MIL‐100(Fe)@polydopamine@Fe₃O₄). The results showed that the magnetic MIL‐101(Fe)@polydopamine@Fe₃O₄ composites have great potential for the extraction of trace sulfonylurea herbicides from various sample types.     

MIL-53(Fe)@聚多巴胺@Fe_3O_4磁性复合材料的制备及其用于环境水样中磺酰脲类除草剂的磁固相萃取

制备了MIL-53(Fe)和聚多巴胺(PDA)修饰的磁性Fe_3O_4复合材料MIL-53(Fe)@PDA@Fe_3O_4,并将其作为吸附剂用于磁固相萃取-高效液相色谱法(MSPE-HPLC)检测环境水样中4种磺酰脲类除草剂(甲嘧磺隆、苄嘧磺隆、吡嘧磺隆和氯嘧磺隆)。实验优化了高效液相色谱条件(乙腈和含0.01%(体积分数)三氟乙酸的水溶液为流动相进行梯度洗脱,检测波长为233 nm)及磁固相萃取条件(洗脱剂为5 mL丙酮,萃取时间为4.5 min,吸附剂用量为60 mg,NaCl加入量为0.5 g,溶液pH值为3),在最佳条件下进行方法学考察,4种磺酰脲类除草剂均得到良好的线性关系,相关系数(r)≥0.998 0。方法的检出限(LOD,S/N=3)为0.28~0.77μg/L。将建立的方法用于3种环境水样中4种磺酰脲类除草剂的检测,其加标回收率为78.8%~109.7%。结果表明,制备的功能化复合材料结合了MIL-53(Fe)和Fe_3O_4的优点,可以简便快速地萃取分离环境水样中磺酰脲类除草剂。     

共价有机框架材料磁固相萃取-高效液相色谱法分析环境水体中对羟基苯甲酸酯

建立了一种基于共价有机框架材料的磁固相萃取-高效液相色谱方法,用于环境水样中对羟基苯甲酸酯的快速灵敏分析。首先以Fe₃O₄纳米粒子为磁核,通过1,3,5-苯三甲醛(Tb)和联苯胺(Bd)在室温下的席夫碱反应合成了磁性共价有机框架材料——Fe₃O₄@TbBd,通过扫描电镜、热重分析、X射线衍射和振动样品磁强计等表征手段证明了该磁性共价有机框架材料具有良好的热稳定性和化学稳定性,且磁响应强度较大,是用于磁固相萃取的理想材料。随后系统研究了影响萃取效率的因素,包括吸附剂用量、萃取时间、pH、解吸溶剂、解吸时间和解吸次数,建立了基于Fe₃O₄@TbBd的磁固相萃取-高效液相色谱测定环境水样中4种对羟基苯甲酸酯的方法。方法的线性范围良好,4种目标物的检出限和定量限范围分别为0.2~0.4 μg/L和0.7~1.4 μg/L,加标回收率为86.1%~110.8%,日内和日间精密度的相对标准偏差(RSD)分别低于5.5%和4.9%。最后将该方法应用于东湖水、长江水和生活废水中对羟基苯甲酸酯的测定,不同加标水平下对羟基苯甲酸酯的回收率在80.7%~117.5%之间,RSD在0.2%~8.8%之间。该方法操作简单,萃取时间短,灵敏度较高且对环境友好,在环境水样中对羟基苯甲酸酯的检测方面有良好的应用潜力。     

Development of ultrasound-assisted emulsification microextraction for the determination of triazine herbicides in environmental water samples by high-performance liquid chromatography

A simple, rapid, efficient, and environmentally friendly method for the determination of some triazine herbicides (simazine, atrazine, prometone, ametryn and prometryne) in water samples was developed by ultrasound-assisted emulsification microextraction (USAEME) coupled with high-performance liquid chromatography-diode array detection (HPLC-DAD). The main parameters that affect the extraction efficiencies, such as the kind and volume of the extraction solvent, ultrasound emulsification time and salt addition, were investigated and optimized. Under the optimum conditions, the method was sensitive and showed a good linearity within a range of 0.5 to 200?ngm?L^?1 for simazine, atrazine, prometone, ametryn and prometryne, with the correlation coefficients (r) varying from 0.9993 to 0.9998. High enrichment factors were obtained ranging from 148 to 225. The limits of detection (LODs) were in the range between 0.06 and 0.1?ngm?L^?1 and the limits of quantification (LOQs) were in the range between 0.2 and 0.3?ngm?L^?1. The recoveries of the analytes from water samples at spiking levels of 5.0 and 50.0?ngm?L^?1 were ranged from 82.4% to 107.0%. The relative standard deviations (RSDs) varied from 3.0% to 4.6%. The results demonstrated that the USAEME-HPLC-DAD method was an ef?cient pretreatment and enrichment procedure for the determination of triazine pesticides in real water samples.     

Ionic‐liquid‐functionalized magnetic particles as an adsorbent for the magnetic SPE of sulfonylurea herbicides in environmental water samples

In this paper, a new ionic‐liquid‐functionalized magnetic material was prepared based on the immobilization of an ionic liquid on silica magnetic particles that could be successfully used as an adsorbent for the magnetic SPE of five sulfonylurea herbicides (bensulfuron‐methyl, prosulfuron, pyrazosulfuron‐ethyl, chlorimuron‐ethyl and triflusulfuron‐methyl) from environmental water samples. The main parameters affecting the extraction efficiency such as desorption conditions, sample pH, extraction time and so on, were optimized using the Taguchi method. Good linearities were obtained with correlation coefficients ranging from 0.9992 to 0.9999 in the concentration range of 0.1–50 μg L^?1 and the LODs were 0.053–0.091 μg L^?1. Under the optimum conditions, the enrichment factors of the method were 1155–1380 and the recoveries ranged from 77.8 to 104.4%. The proposed method was reliable and could be applied to the residue analysis of sulfonylurea herbicides in environmental water samples (tap, reservoir and river).     

亚胺连接的多孔共价有机骨架材料结合固相萃取-液相色谱-串联质谱检测蜂蜜中雌激素

以亚胺连接的多孔共价有机骨架材料(IL-COF-1)作为固相萃取的吸附剂,建立了液相色谱-串联质谱快速检测蜂蜜样品中痕量雌激素的方法。该研究选择雌二醇、己烯雌酚、雌三醇、β-雌二醇和炔雌醇5种雌激素作为目标分析物。在蜂蜜样品中添加雌激素,采用单因素优化法对影响萃取效果的重要因素进行优化,获得最佳条件:IL-COF-1用量为30 mg,样品流速为3 mL/min,样品溶液pH值为7,以5 mL的1%(v/v)氨水-甲醇溶液进行洗脱,流速为0.4 mL/min,萃取过程中不添加NaCl。采用高效液相色谱-三重四极杆质谱联用技术对提取物中的雌激素进行定量分析。以乙腈和5 mmol/L的乙酸铵溶液作为流动相进行梯度洗脱,经C18色谱柱分离,采用电喷雾离子源、质谱多反应监测和负离子扫描模式,实现了蜂蜜样品中5种雌激素的快速定性定量分析。在最佳条件下,方法验证结果中雌三醇、β-雌二醇和炔雌醇的线性范围为1~500 ng/g,雌二醇和己烯雌酚的线性范围为0.1~100 ng/g,相关系数(r)为0.9934~0.9972。检出限(S/N=3)为0.01~0.30 ng/g,定量限(S/N=10)为0.05~0.95 ng/g。添加50 ng/g 5种雌激素进行重复性实验,日内精密度相对标准偏差(RSD)为3.2%~6.6%,日间精密度RSD为4.2%~7.9%。基于IL-COF-1的固相萃取-液相色谱-串联质谱法具有快速准确、灵敏度高等特点,适用于蜂蜜中雌激素的分析和检测。将该方法应用于4个实际蜂蜜样品中雌激素的检测,均未检出目标物;在低中高3个水平下,5种雌激素的加标回收率为80.1%~115.2%,结果令人满意。     

Selective magnetic solid-phase extraction of amide herbicides from fish samples coupled with ultra-high-performance liquid chromatography with tandem mass spectrometry

An efficient magnetic dummy template molecularly imprinted polymer nanocomposite was prepared using multi-walled carbon nanotubes as a support and metolachlor deschloro as a dummy template. The obtained nanocomposites were characterized using Fourier transform infrared spectroscopy, vibrating sample magnetometry, scanning electron microscopy, and transmission electron microscopy. The adsorption performance of the obtained nanocomposites was evaluated through binding experiments, including static adsorption, kinetic adsorption, and selective recognition studies. The obtained nanocomposites were successfully applied as selective sorbents for the magnetic solid-phase extraction of seven amide herbicides (alachlor, acetochlor, pretilachlor, butachlor, metolachlor, diethatyl ethyl, and dimethachlor) coupled with liquid chromatography-tandem mass spectrometry from fish samples. Under the optimized conditions, the limit of detection was 0.01–0.1 μg/kg. The obtained recoveries of the amide herbicides from the fish samples were in the range of 88.0 to 102.1% with a relative standard deviation of less than 7.5%. This method, which eliminated the effect of template leakage on qualitative and quantitative analysis was found to be superior to the methods reported in the literature. The results indicated that it could be successfully applied to analyze amide herbicides in fish samples with satisfactory recoveries.     

One-pot synthesis of magnetic sulfonated covalent organic polymer for extraction of protoberberine alkaloids in herbs and human plasma

A novel magnetic sulfonated covalent organic polymer was prepared for magnetic solid-phase extraction of protoberberine alkaloids. The magnetic sulfonated covalent organic polymer was rapidly synthesized under mild conditions. The physicochemical properties of the prepared materials were characterized by Fourier-transform infrared spectrometry, transmission electron microscopy, and X-ray photoelectron spectroscopy. Several extraction parameters were systematically investigated, including desorption time, pH of sample solution, acetonitrile content, acetic acid content in the eluent, extraction time, and sample volume. By coupling magnetic solid-phase extraction and high-performance liquid chromatography, an efficient and sensitive method for the extraction and determination of protoberberine alkaloids in complex samples was developed. The proposed method showed great linearity (r > 0.9989), low limits of detection (0.2–0.3 ng/ml), and high precision (relative standard deviations ≤ 5.74%). The proposed method was further applied to the analysis of protoberberine alkaloids in Cortex phellodendri and human plasma samples. The recoveries were 91.50%–110.31% with relative standard deviations less than 6.63% in Cortex phellodendri and 96.12%–111.20% with relative standard deviations lower than 5.56% in plasma samples.     

N-Methylimidazolium ionic liquid-functionalized silica as a sorbent for selective solid-phase extraction of 12 sulfonylurea herbicides in environmental water and soil samples

A novel material for solid-phase extraction (SPE) was synthesized by chemical immobilization of a functionalized N-methylimidazolium ionic liquid on silica gel. Cartridges packed with the synthetic material were successfully applied to the pre-concentration of trace-level thifensulfuron-methyl, metsulfuron-methyl, chlorsulfuron, sulfometuron-methyl, rimsulfuron, ethametsulfuron, tribenuron-methyl, bensulfuron-methyl, prosulfuron, pyrazosulfuron, chlorimuron-ethyl and primisulfuron from environmental water and soil samples. The 12 sulfonylurea herbicides (SUs) obtained a good resolution in less than 50 min using HPLC with a UV detector. The recovery studies using the ionic liquid-functionalized silica as a sorbent were performed by three consecutive extractions of water and soil samples at two spiked levels. The average recovery for each analyte was in the range of 53.8–118.2% for the water samples and 60.9–121.3% for the soil sample, with RSDs lower than 11.3% in all cases. The ionic liquid-functionalized silica cartridges showed higher selectivity for the SUs than commercially available C₁₈ cartridges did.     

Pressurized-liquid extraction for determination of imidazolinone herbicides in soil

Summary A rapid and simple method has been developed for determination of imidazolinone (IMI) residues in soil. Extraction of the analytes from the soil matrix was performed with a pressurized-liquid-extraction apparatus built in this laboratory. Four different types of soil sample (clay, clay loam, sandy clay loam, and silty loam) were fortified with target compounds at levels of 10 and 50 ng g⁻¹ by a procedure which can mimic weathered soils. The samples were then dried and packed in a 25 cm×4.6 mm i. d. stainless steel column; this was placed inside a GC oven and extracted by passing an aqueous solution of KCl (0.1m, 20 mL) through the column at 90°C. Quantification of the analytes in the final extract (50-μL injection) was performed by reversed-phase liquid chromatography-mass spectrometry with a TurbolonSpray interface. Recoveries of the analytes were greater than 83% andRSD less than 7%. The method detection limit was in the 1–2.5ng g⁻¹ range in analysis by time-scheduled selected-ion monitoring (SIM).     

Preparation of magnetic surface molecularly imprinted polymers for the selective extraction of triazines in environmental water samples

ABSTRACT

In this work, a magnetic molecularly imprinted polymer (Fe₃O₄@SiO₂@MIPs) was prepared via a surface-imprinted method for the determination of the triazines in environmental water samples combined with high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). The Fourier transform infrared spectroscopy (FTIR) and vibrating sample magnetometer showed that the Fe₃O₄@SiO₂@MIPs was successfully synthesised and exhibited superparamagnetism. The isotherm adsorption, selectivity and adsorption kinetics experiments showed that the Fe₃O₄@SiO₂@MIPs exhibited excellent specific recognition and fast adsorption equilibrium for triazines. The adsorption process is spontaneous and endothermic. The isotherm adsorption was consistent with Scatchard model and adsorption kinetic fit pseudo-second-order kinetic model. Under the optimised adsorption conditions, the Fe₃O₄@SiO₂@MIPs was directly used to selectively enrich six triazines in environmental water samples. The enrichment volume was up to 500 mL, and the matrix effects were down to 0.7–12.4%. The built method has excellent linearities in the range of 0.25–500 ng L^?1 with R² in the range of 0.998–0.999, lower limit of detections (0.02–0.08 ng L^?1) and higher precision (2.4–7.2%). The Fe₃O₄@SiO₂@MIPs is expected to be widely applied to the direct enrichment of triazines in bulk environmental water samples.     

Preparation of spherical silica hydroxyl-functionalized covalent organic polymer composites for mixed-mode liquid chromatography

Covalent organic polymers are an emerging class of amorphous microporous materials that have raised increasing concerns in analytical chemistry due to their unique structural and surface chemical properties. However, the application of covalent organic polymers as mixed-mode stationary phases in chromatographic separations has rarely been reported. Herein, novel spherical silica hydroxyl-functionalized covalent organic polymer composites were successfully prepared via a layer-by-layer approach. The structure and morphology of the materials were carefully characterized by elemental analysis, Fourier-transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction, thermogravimetric analysis, Brunauer-Emmett-Teller, and contact angle measurements. Baseline separations of various alkylbenzenes, polycyclic aromatic hydrocarbons, and nucleosides and bases were achieved on the prepared stationary phase under reversed-phase/hydrophilic interaction mode. The column efficiencies of 23 853 and 36 580 plates/m were obtained for butylbenzene and uracil, respectively, and the relative standard deviation of the retention time for continuous injections was less than 1.38% (n = 10), suggesting satisfactory column efficiency and repeatability. Additionally, this novel stationary phase realized the complete separation of the endocrine-disrupting chemicals in river water. This work affords a new route for synthesizing covalent organic polymers-based mixed-mode stationary phase and further reveals their great potential in chromatographic separation.     

Evaluation of double solid-phase extraction system for determining triazine herbicides in milk

Summary High-performance liquid chromatography with UV detection was used to determine eight triazine herbicides in milk. Solid-phase extraction was performed using a double trap; first, a nonspecific adsorbent (Carbograph), and then a cation exchanger (SCX). Eluate from the SCX was evaporated to dryness under reduced pressure and redissolved in mobile phase. An aliquot was injected into the chromatograph, which was operated isocratically in the reverse-phase mode with UV detection at 225 nm. Analytical recoveries for the eight triazines ranged from 73.0 % to 92.4 %. The limit of sensitivity of this method was about 0.09 ng mL⁻¹ of milk. The method was validated and evaluated by comparison with a method reported in literature.     

Evaluation of double solid-phase extraction system for determining triazine herbicides in milk

Summary High-performance liquid chromatography with UV detection was used to determine eight triazine herbicides in milk. Solid-phase extraction was performed using a double trap; first, a nonspecific adsorbent (Carbograph), and then a cation exchanger (SCX).Eluate from the SCX was evaporated to dryness under reduced pressure and redissolved in mobile phase. An aliquot was injected into the chromatography, which was operated isocratically in the reverse-phase mode with UV detection at 225 nm.Analytical recoveries for the eight triazines ranged from 73.0% to 92.4%. The limit of sensitivity of this method was about 0.09 ng mL^–1 of milk. The method was validated and evaluated by comparison with a method reported in literature.     

Positively charged covalent organic framework and its application in the dispersive solid-phase extraction of ultraviolet-filters from food packaging material migrants

Abstract

Covalent organic frameworks (COFs) show excellent property, such as high porosity and excellent structure stability and were well applied in fields such as catalysis and adsorption, but most of the COFs showed similar structure and thus similar adsorption performance. Modification of simple COFs to enhance its adsorption performance in separation technique is an important issue. In this study, quaternary ammonium groups with long hydrophobic chain were introduced into a simple COF (TpPa-1) for the first time. The positively charged COF (PC-TpPa-1) can form electrostatic interaction and hydrophobic effect with negatively charged analytes, and showed good adsorption performance for ultraviolet-filters (UV filters). Under the optimum conditions, i.e. adsorbent amount 20?mg, pH?=?7, 1.0?mL acetonitrile as eluent, the obtained recoveries for all UV filters were in the range of 86.4–96.7%.The developed method was successfully applied to the determination of UV filters from food packaging material migrants with the aid of HPLC as a detector.     

Molecularly imprinted covalent organic polymers for the selective extraction of benzoxazole fluorescent whitening agents from food samples

Molecularly imprinted covalent organic polymers were constructed by an imine‐linking reaction between 1,3,5‐triformylphloroglucinol and 2,6‐diaminopyridine and used for the selective solid‐phase extraction of benzoxazole fluorescent whitening agents from food samples. Binding experiments showed that imprinting sites on molecularly imprinted polymers had higher selectivity for targets compared with those of the corresponding non‐imprinted polymers. Parameters affecting the solid‐phase extraction procedure were examined. Under optimal conditions, actual samples were treated and the eluent was analyzed with high‐performance liquid chromatography with diode‐array detection. The results showed that the established method has a wide linearity, satisfactory detection limits and quantification limits, and acceptable recoveries. Thus, this developed method possesses the practical potential for the selective determination of benzoxazole fluorescent whitening agents in complex food samples.     

Magnetic solid-phase extraction of sulfonylurea herbicides in environmental water samples by Fe3O4@dioctadecyl dimethyl ammonium chloride@silica magnetic particles

A magnetic solid phase extraction (MSPE) method coupled with high-performance liquid chromatography (HPLC) was proposed for the determination of five sulfonylurea herbicides (bensulfuron-methyl, prosulfuron, pyrazosulfuron-ethyl, chlorimuron-ethyl and triflusulfuron-methyl) in environmental water samples. The magnetic adsorbent was prepared by incorporating Fe₃O₄ nanoparticles and surfactant into a silica matrix according to a sol–gel procedure, which can provide surfactant free extracts during the eluting step to avoid chromatographic interference. The prepared adsorbent was used to extract the sulfonylurea herbicides in several kinds of water samples. The main factors affecting the extraction efficiency, including desorption conditions, extraction time, sample volume, and sample solution pH were optimized. Under the optimum conditions, good linearity was obtained within the range of 0.2–50.0 μg L⁻¹ for all analytes, with correlation coefficients ranging from 0.9993 to 0.9999. The enrichment factors were between 1200 and 1410, and the limits of detection were between 0.078 and 0.10 μg L⁻¹. The proposed method was successfully applied in the analysis of sulfonylurea herbicides in environmental samples (tap, reservoir, river, and rice field). The recoveries of the method ranged between 80.4% and 107.1%. This study reported for the first time the use of MSPE procedure in the preconcentration of sulfonylurea herbicides in environmental samples. The procedure proved to be efficient, environmentally friendly, and fast.     

Hollow‐fiber liquid‐phase microextraction combined with capillary HPLC for the selective determination of six sulfonylurea herbicides in environmental waters

A three‐phase hollow‐fiber liquid‐phase microextraction combined with a capillary LC method using diode array detection was proposed for the determination of six sulfonylurea herbicides, triasulfuron, metsulfuron‐methyl, chlorsulfuron, flazasulfuron, chlorimuron‐ethyl, and primisulfuron‐methyl, in environmental water samples. Different factors that can affect the extraction process such as extraction solvent, acidity of the donor phase, composition and pH of the acceptor phase, salt addition, stirring speed, and extraction time were optimized. Under the optimum conditions, detection and quantitation limits between 0.1 – 1.7 and 0.3 – 5.7 μg/L, respectively, and enrichment factors ranging from 71 to 548 were obtained. The calibration curves were linear within the range of 0.3 – 40 μg/L. Intra‐ and interday RSDs were <6.3 and 8.4%, respectively. The relative recoveries of the spiked ground and river water samples were in the range of 69.4 – 119.2 and 77.4 – 111.7%, respectively. The results of the study revealed that the developed methodology involves an efficient sample pretreatment allowing the preconcentration of analytes, combined with the use of a miniaturized separation technique, suitable for the accurate determination of sulfonylurea herbicides in water.