Comparison of two ultrasound‐enhanced microextractions combined with HPLC for determining acaricides in water

An ultrasound‐enhanced in situ solvent formation microextraction has been developed first time and compared with ultrasound‐enhanced ionic‐liquid‐assisted dispersive liquid–liquid microextraction for the HPLC analysis of acaricides in environmental water samples. A ionic liquid ([C₈MIM][PF₆]) was used as the green extraction solvent through two pathways. The experimental parameters, such as the type and volume of both of the extraction solvent disperser solvent, ultrasonication time, and salt addition, were investigated and optimized. The analytical performance using the optimized conditions proved the feasibility of the developed methods for the quantitation of trace levels of acaricides by obtaining limits of detection that range from 0.54 to 3.68 μg/L. The in situ solvent formation microextraction method possesses more positive characteristics than the ionic‐liquid‐assisted dispersive liquid–liquid microextraction method (except for spirodiclofen determination) when comparing the validation parameters. Both methods were successfully applied to determining acaricides in real water samples.     

Facile preparation of a polydopamine‐based monolith for multiple monolithic fiber solid‐phase microextraction of triazine herbicides in environmental water samples

A new multiple monolithic fiber solid‐phase microextraction using a polydopamine‐based monolith as the extraction medium is proposed. The monolith was synthesized by facile in situ copolymerization of N‐methacryldopamine and dual cross‐linkers (divinylbenzene/ethylenedimethacrylate) in the presence of N ,N‐dimethylformamide. The effect of the contents of N‐methacryldopamine and porogen in the polymerization mixture on the extraction performance was investigated thoroughly. A series of characterization studies was performed to validate the structure and properties of the monolith. The prepared multiple monolithic fibers were used for the extraction of triazine herbicides in environmental water samples. After the optimization of the extraction parameters, a convenient, sensitive, cost‐effective, and environmentally friendly method for the determination of trace triazine herbicides in water samples was developed by coupling multiple monolithic fibers solid‐phase microextraction with high‐performance liquid chromatography and diode array detection. The results indicated that the limits of detection and quantification for the target compounds were 0.031–0.14 and 0.10–0.45 μg/L, respectively. Good precision and reproducibility were obtained with the relative standard deviations below 10%. The developed method was applied to the analysis of the triazine herbicides in different water samples (lake, river, and farmland waters). The recoveries of the method were in the range between 79.6 and 117%.     

Temperature‐controlled ionic liquid‐dispersive liquid‐phase microextraction for preconcentration of chlorotoluron,diethofencarb and chlorbenzuron in water samples

This article describes a new, rapid and sensitive method for the determination of chlorotoluron, diethofencarb and chlorbenzuron from water samples with temperature‐controlled ionic liquid‐dispersive liquid‐phase microextraction. In the preconcentration procedure, ionic liquid 1‐hexyl‐3‐methylimidazolium hexafluorophosphate [C₆MIM] [PF₆] was employed as the extraction solvent. The parameters, such as volume of [C₆MIM] [PF₆], sample pH, extraction time, centrifuging time, temperature and salting‐out effect, were investigated in detail. Under the optimal extraction conditions, it has been found that three analytes had excellent LODs (S/N=3) in the range of 0.04–0.43 μg/L. The RSDs (n=6) were in the range of 1.3–4.7%. The proposed method was evaluated with lake water, tap water and melted snow water samples. The experimental results indicated that the proposed method had excellent prospect and would be widely used in the future.     

A simple solvent collection technique for a dispersive liquid–liquid microextraction of parabens from aqueous samples using low‐density organic solvent

A simple technique for the collection of an extraction solvent lighter than water after dispersive liquid–liquid microextraction combined with high‐performance liquid chromatography with ultraviolet detection was developed for the determination of four paraben preservatives in aqueous samples. After the extraction procedure, low‐density organic solvent together with some little aqueous phase was separated by using a disposable glass Pasteur pipette. Next, the flow of the aqueous phase was stopped by successive dipping the capillary tip of the pipette into anhydrous Na₂SO₄. The upper organic layer was then removed simply with a microsyringe and injected into the high‐performance liquid chromatography system. Experimental parameters that affect the extraction efficiency were investigated and optimized. Under optimal extraction conditions, the extraction recoveries ranged from 25 to 86%. Good linearity with coefficients with the square of correlation coefficients ranging from 0.9984 to 0.9998 was observed in the concentration range of 0.001–0.5 μg/mL. The relative standard deviations ranged from 4.1 to 9.3% (n = 5) for all compounds. The limits of detection ranged from 0.021 to 0.046 ng/mL. The method was successfully applied for the determination of parabens in tap water and fruit juice samples and good recoveries (61–108%) were achieved for spiked samples.     

Application of ionic‐liquid‐supported magnetic dispersive solid‐phase microextraction for the determination of acaricides in fruit juice samples

In this study, ionic liquid (IL) supported magnetic dispersive solid‐phase microextraction was developed and a systematic investigation was conducted on imidazolium ILs for their extraction performance. This nano‐based pretreatment procedure was then applied for the determination of acaricides in fruit juice samples for the first time. A feature of this technique is that the commonly laborious chemical modification of magnetic nanoparticles (MNPs) was skillfully circumvented. Because of the combination of ILs, dispersive liquid–liquid microextraction, and dispersive MNP solid‐phase microextraction, the extraction efficiency can be significantly improved using commercial MNPs. Parameters of the extraction method were investigated by one‐factor‐at‐a‐time approach. The optimal experimental conditions were as follows: emulsification for 2 min by sonication with the addition of 50 μL [C₆MIM][NTf₂] in the dispersive liquid–liquid microextraction step and vortexing for 90 s after adding 40 mg spherical barium ferrite nanoparticles (20 nm). The desorption time was 2 min. Good linearity (0.5–500 ng/mL) and detection limits within the range of 0.05–0.53 ng/mL were achieved. The application of the proposed method was demonstrated by the analysis of real fruit juice samples, in which recoveries between 85.1 and 99.6% were obtained.     

Extraction and preconcentration of tylosin from milk samples through functionalized TiO2 nanoparticles reinforced with a hollow fiber membrane as a novel solid/liquid‐phase microextraction technique

The aim of this study was to introduce a novel, simple, and highly sensitive preparation method for determination of tylosin in different milk samples. In the so‐called functionalized TiO₂ hollow fiber solid/liquid‐phase microextraction method, the acceptor phase is functionalized TiO₂ nanoparticles that are dispersed in the organic solvent and held in the pores and lumen of a porous polypropylene hollow fiber membrane. An effective functionalization of TiO₂ nanoparticles has been done in the presence of aqueous H₂O₂ and a mild acidic ambient under UV irradiation. This novel extraction method showed excellent extraction efficiency and a high enrichment factor (540.2) in comparison with conventional hollow fiber liquid‐phase microextraction. All the experiments were monitored at λ_max = 284 nm using a simple double beam UV‐visible spectrophotometer. A Taguchi orthogonal array experimental design with an OA₁₆ (4⁵) matrix was employed to optimize the factors affecting the efficiency of hollow fiber solid/liquid‐phase microextraction such as pH, stirring rate, salt addition, extraction time, and the volume of donor phase. This developed method was successfully applied for the separation and determination of tylosin in milk samples with a linear concentration range of 0.51–7000 μg/L (r² = 0.991) and 0.21 μg/L as the limit of detection.     

Optimization of dispersive liquid–liquid microextraction with central composite design for preconcentration of chlordiazepoxide drug and its determination by HPLC‐UV

A simple, rapid, and sensitive method based on dispersive liquid–liquid microextraction combined with HPLC‐UV detection applied for the quantification of chlordiazepoxide in some real samples. The effect of different extraction conditions on the extraction efficiency of the chlordiazepoxide drug was investigated and optimized using central composite design as a conventional efficient tool. Optimum extraction condition values of variables were set as 210 μL chloroform, 1.8 mL methanol, 1.0 min extraction time, 5.0 min centrifugation at 5000 rpm min^?1, neutral pH, 7.0% w/v NaCl. The separation was reached in less than 8.0 min using a C₁₈ column using isocratic binary mobile phase (acetonitrile/water (60:40, v/v)) with flow rate of 1.0 mL min^?1. The linear response (r² > 0.998) was achieved in the range of 0.005–10 μg mL^?1 with detection limit 0.0005 μg mL^?1. The applicability of this method for simultaneous extraction and determination of chlordiazepoxide in four different matrices (water, urine, plasma, and chlordiazepoxide tablet) were investigated using standard addition method. Average recoveries at two spiking levels were over the range of 91.3–102.5% with RSD < 5.0% (n = 3). The obtained results show that dispersive liquid–liquid microextraction combined with HPLC‐UV is a fast and simple method for the determination of chlordiazepoxide in real samples.     

Development of a fabric phase sorptive extraction with high‐performance liquid chromatography and ultraviolet detection method for the analysis of alkyl phenols in environmental samples

A novel analytical method has been developed and validated for the quantification of alkyl phenols in aqueous and soil samples. Fabric phase sorptive extraction, a new sorptive microextraction technique, has been employed for the preconcentration of some endocrine‐disruptor alkylphenol molecules, namely, 4‐tert‐butylphenol, 4‐sec‐butylphenol, 4‐tert‐amylphenol, and 4‐cumylphenol, followed by high‐performance liquid chromatography with ultraviolet detection. Various parameters influencing the fabric phase sorptive extraction performance, namely, extraction time, eluting solvent, elution time and pH of the sample matrix, were optimized. The chromatographic separation was carried out with a mobile phase of acetonitrile/water (60:40 v/v) at an isocratic flow rate of 1.0 mL/min using a reversed‐phase C₁₈ column at λ_max 225 nm. The calibration curves of target analytes were prepared in the concentration range 5–500 ng/mL with good coefficient of determination values (R² > 0.992). Extraction efficiency values were 74.0, 75.6, 78.0, and 78.3 for 4‐tert‐butylphenol, 4‐sec‐butylphenol, 4‐tert‐amylphenol, and 4‐cumylphenol, respectively. The limits of detection range from 0.161 to 0.192 ng/mL. Subsequently, the new fabric phase sorptive extraction with high‐performance liquid chromatography and ultraviolet detection was successfully applied for the recovery of alkyl phenols from spiked ground water, river water, and treated water from a sewage treatment plant, and soil and sludge samples.     

Study of enrichment factors for six β‐blockers in aliphatic alcohols by hollow‐fiber liquid‐phase microextraction

The selectivity of a suitable organic solvent is key for extraction in liquid‐phase microextraction experiments. Nevertheless, the screening process remains a daunting task. Our research aimed to study the relationship between extraction efficiency and extraction solvents, analytes, and finally select the appropriate extraction solvent. In the present article, β‐blockers and six extraction solvents were chosen as the models and hollow‐fiber liquid‐phase microextraction was conducted. The relationship was built by statistical analysis on the data. Factors affecting extraction efficiency including the logarithms of the octanol/water partition coefficient (logP_o/w) of analytes, acid dissociation constants, the logarithms of the octanol/water partition coefficient of solvents and pH of the sample solution were investigated. The results showed that a low water solubility of extraction solvent is the foundation to ensure higher extraction efficiency. Moreover, when ΔlogP_o/w > 0, a higher extraction efficiency is observed at lower ΔlogP_o/w, on the contrary, when ΔlogP_o/w < 0, extraction efficiency is higher as the absolute value of ΔlogP_o/w becomes greater. Finally, the relationship between enrichment factor and extraction solvents, analytes was established and a helpful guidance was provided for the selection of an optimal solvent to obtain the best extraction efficiency by liquid‐phase microextraction.     

Ultrapreconcentration and determination of organophosphorus pesticides in water by solid‐phase extraction combined with dispersive liquid–liquid microextraction and high‐performance liquid chromatography

Solid‐phase extraction coupled with dispersive liquid–liquid microextraction was developed as an ultra‐preconcentration method for the determination of four organophosphorus pesticides (isocarbophos, parathion‐methyl, triazophos and fenitrothion) in water samples. The analytes considered in this study were rapidly extracted and concentrated from large volumes of aqueous solutions (100 mL) by solid‐phase extraction coupled with dispersive liquid–liquid microextraction and then analyzed using high performance liquid chromatography. Experimental variables including type and volume of elution solvent, volume and flow rate of sample solution, salt concentration, type and volume of extraction solvent and sample solution pH were investigated for the solid‐phase extraction coupled with dispersive liquid–liquid microextraction with these analytes, and the best results were obtained using methanol as eluent and ethylene chloride as extraction solvent. Under the optimal conditions, an exhaustive extraction for four analytes (recoveries >86.9%) and high enrichment factors were attained. The limits of detection were between 0.021 and 0.15 μg/L. The relative standard deviations for 0.5 μg/L of the pesticides in water were in the range of 1.9–6.8% (n = 5). The proposed strategy offered the advantages of simple operation, high enrichment factor and sensitivity and was successfully applied to the determination of four organophosphorus pesticides in water samples.     

Use of volatile organic solvents in headspace liquid‐phase microextraction by direct cooling of the organic drop using a simple cooling capsule

A low‐cost and simple cooling‐assisted headspace liquid‐phase microextraction device for the extraction and determination of 2,6,6‐trimethyl‐1,3 cyclohexadiene‐1‐carboxaldehyde (safranal) in Saffron samples, using volatile organic solvents, was fabricated and evaluated. The main part of the cooling‐assisted headspace liquid‐phase microextraction system was a cooling capsule, with a Teflon microcup to hold the extracting organic solvent, which is able to directly cool down the extraction phase while the sample matrix is simultaneously heated. Different experimental factors such as type of organic extraction solvent, sample temperature, extraction solvent temperature, and extraction time were optimized. The optimal conditions were obtained as: extraction solvent, methanol (10 μL); extraction temperature, 60°C; extraction solvent temperature, 0°C; and extraction time, 20 min. Good linearity of the calibration curve (R² = 0.995) was obtained in the concentration range of 0.01–50.0 μg/mL. The limit of detection was 0.001 μg/mL. The relative standard deviation for 1.0 μg/mL of safranal was 10.7% (n = 6). The proposed cooling‐assisted headspace liquid‐phase microextraction device was coupled (off‐line) to high‐performance liquid chromatography and used for the determination of safranal in Saffron samples. Reasonable agreement was observed between the results of the cooling‐assisted headspace liquid‐phase microextraction high‐performance liquid chromatography method and those obtained by a validated ultrasound‐assisted solvent extraction procedure.     

Ionic liquid-based single-drop liquid-phase microextraction combined with high-performance liquid chromatography for the determination of sulfonamides in environmental water

A simple, rapid and environment‐friendly technique of single‐drop liquid‐phase microextraction has been developed for the determination of sulfonamides in environmental water. Several important parameters including stirring rate, extraction solvent, extraction pH, salinity and extraction time were optimized to maximize the extract efficiency. Extraction solvent 1‐octyl‐3‐methylimidazolium hexafluorophosphate [C₈MIM][PF₆] ionic liquid showed better extraction efficiency than 1‐butyl‐3‐methylimidazolium hexafluorophosphate [C₄MIM][PF₆] and 1‐octanol. The optimum experimental conditions were: pH, 4.5; sodium chloride content, 36% w/v; extraction time, 20 min. This method provided low detection limits (0.5–1 ng/mL), good repeatability (the RSD ranging from 4.2 to 9.9%, n=5) and wide linear range (1–1500 ng/mL), with determination coefficients (r²) higher than 0.9989 for all the target compounds. Real sample analysis showed relative recoveries between 63.5 and 115.8% for all the target compounds.     

Determination of 19 sulfonamides residues in pork samples by combining QuEChERS with dispersive liquid–liquid microextraction followed by UHPLC–MS/MS

A new simple and rapid pretreatment method for simultaneous determination of 19 sulfonamides in pork samples was developed through combining the QuEChERS method with dispersive liquid–liquid microextraction followed by ultra‐high performance liquid chromatography with tandem mass spectrometry. The sample preparation involves extraction/partitioning with QuEChERS method followed by dispersive liquid–liquid microextraction using tetrachloroethane as extractive solvent and the acetonitrile extract as dispersive solvent that obtained by QuEChERS. The enriched tetrachloroethane organic phase by dispersive liquid–liquid microextraction was evaporated, reconstituted with 100 μL acetonitrile/water (1:9 v/v) and injected into an ultra‐high performance liquid chromatography with a mobile phase composed of acetonitrile and 0.1% v/v formic acid under gradient elution and separated using a BHE C₁₈ column. Various parameters affecting the extraction efficiency were investigated. Matrix‐matched calibration curves were established. Good linear relationships were obtained for all analytes in a range of 2.0–100 μg/kg and the limits of detection were 0.04–0.49 μg/kg. Average recoveries at three spiking levels were in the range of 78.3–106.1% with relative standard deviations less than 12.7% (n = 6). The developed method was successfully applied to determine sulfonamide residues in pork samples.     

Switchable‐hydrophilicity solvent‐based microextraction combined with gas chromatography for the determination of nitroaromatic compounds in water samples

A simple, fast, sensitive, and low‐cost method was developed for the quantification of nitroaromatic compounds in water samples based on CO₂‐assisted liquid‐phase microextraction using a switchable‐hydrophilicity solvent followed by gas chromatography detection. Dipropylamine was used as extraction solvent with switchable hydrophilicity that can be miscible or immiscible upon the addition or removal of CO₂ as a reagent. Experimental parameters affecting the extraction efficiency such as the volume of acceptor phase, the volume of donor phase, pH of donor phase, ionic strength, and extraction time were investigated. Under the optimal conditions, detection limits and preconcentration factors were obtained in the ranges of 0.9–1.8 μg/L and 132–138, respectively. Also, the extraction recoveries of water samples were above 88%. Finally, the developed method was successfully applied to the determination of nitroaromatic compounds in real water samples.     

Determination of N‐nitrosamines by automated dispersive liquid–liquid microextraction integrated with gas chromatography and mass spectrometry

An automated dispersive liquid–liquid microextraction integrated with gas chromatography and mass spectrometric procedure was developed for the determination of three N‐nitrosamines (N‐nitroso‐di‐n‐propylamine, N‐nitrosopiperidine, and N‐nitroso di‐n‐butylamine) in water samples. Response surface methodology was employed to optimize relevant extraction parameters including extraction time, dispersive solvent volume, water sample pH, sodium chloride concentration, and agitation (stirring) speed. The optimal dispersive liquid–liquid microextraction conditions were 28 min of extraction time, 33 μL of methanol as dispersive solvent, 722 rotations per minute of agitation speed, 23% w/v sodium chloride concentration, and pH of 10.5. Under these conditions, good linearity for the analytes in the range from 0.1 to 100 μg/L with coefficients of determination (r²) from 0.988 to 0.998 were obtained. The limits of detection based on a signal‐to‐noise ratio of 3 were between 5.7 and 124 ng/L with corresponding relative standard deviations from 3.4 to 5.9% (n = 4). The relative recoveries of N‐nitroso‐di‐n‐propylamine, N‐nitrosopiperidine, and N‐nitroso di‐n‐butylamine from spiked groundwater and tap water samples at concentrations of 2 μg/L of each analyte (mean ± standard deviation, n = 3) were (93.9 ± 8.7), (90.6 ± 10.7), and (103.7 ± 8.0)%, respectively. The method was applied to determine the N‐nitrosamines in water samples of different complexities, such as tap water, and groundwater, before and after treatment, in a local water treatment plant.     

Reversed‐phase ion‐pair solid‐phase extraction and ion chromatography analysis of pyrrolidinium ionic liquid cations in environmental water samples

A method of reversed‐phase ion‐pair solid‐phase extraction combined with ion chromatography for determination of pyrrolidinium ionic liquid cations (N‐methyl‐N‐ethyl pyrrolidinium, N‐methyl‐N‐propyl pyrrolidinium, and N‐methyl‐N‐butyl pyrrolidinium) in water samples was developed in this study. First, ion‐pair reagent sodium heptanesulfonate was added to the water samples after static, centrifugation and filteration. Then, pyrrolidinium cations in the samples were enriched and purified by a reversed‐phase solid‐phase extraction column, and eluted from the column with methanol aqueous solution as eluent. Finally, the eluate collected was analyzed by ion chromatography. The separation and direct conductivity detection of these pyrrolidinium cations by ion‐exchange column using 1.0 mM methanesulfonic acid (in water)/acetonitrile (97:3, v:v) as mobile phase was achieved within 10 min. By using this method, pyrrolidinium cations in Songhua River and Hulan River were successfully extracted with the recoveries ranging from 74.2 to 97.1% and the enrichment factor assessed as 60. Pyrrolidinium cations with the concentration of 0.001?0.03 mg/L can be enriched and detected in the water samples. The developed method for the determination of pyrrolidinium ionic liquid cations in water samples is simple and reliable, which provides a reference for the study of the potential impact of ionic liquids on the environment.     

Hollow‐fiber‐supported liquid membrane microextraction of amlodipine and atorvastatin

A simple, environmentally friendly, and efficient method, based on hollow‐fiber‐supported liquid membrane microextraction, followed by high‐performance liquid chromatography has been developed for the extraction and determination of amlodipine (AML) and atorvastatin (ATO) in water and urine samples. The AML in two‐phase hollow‐fiber liquid microextraction is extracted from 24.0 mL of the aqueous sample into an organic phase with microliter volume located inside the pores and lumen of a polypropylene hollow fiber as acceptor phase, but the ATO in three‐phase hollow‐fiber liquid microextraction is extracted from aqueous donor phase to organic phase and then back‐extracted to the aqueous acceptor phase, which can be directly injected into the high‐performance liquid chromatograph for analysis. The preconcentration factors in a range of 34–135 were obtained under the optimum conditions. The calibration curves were linear (R² ≥ 0.990) in the concentration range of 2.0–200 μg/L for AML and 5.0–200 μg/L for ATO. The limits of detection for AML and ATO were 0.5 and 2.0 μg/L, respectively. Tap water and human urine samples were successfully analyzed for the existence of AML and ATO using the proposed methods.     

Dispersive solid‐phase extraction combined with dispersive liquid‐liquid microextraction for simultaneous determination of seven succinate dehydrogenase inhibitor fungicides in watermelon by ultra high performance liquid chromatography with tandem mass spectrometry

In this study, a simple and accurate sample preparation method based on dispersive solid‐phase extraction and dispersive liquid‐liquid microextraction has been developed for the determination of seven novel succinate dehydrogenase inhibitor fungicides (isopyrazam, fluopyram, pydiflumetofen, boscalid, penthiopyrad, fluxapyroxad, and thifluzamide) in watermelon. The watermelon samples were extracted with acetonitrile, cleaned up by dispersive solid‐phase extraction procedure using primary secondary amine, extracted and concentrated by the dispersive liquid‐liquid microextraction procedure with 1,1,2,2‐tetrachloroethane, and then analyzed by ultra high performance liquid chromatography with tandem mass spectrometry. The main experimental factors affecting the performance of dispersive solid‐phase extraction and dispersive liquid‐liquid microextraction procedure on extraction efficiency were investigated. The proposed method had a good linearity in the range of 0.1–100 µg/kg with correlation coefficients (r) of 0.9979–0.9999. The limit of quantification of seven fungicides was 0.1 µg/kg in the method. The fortified recoveries of seven succinate dehydrogenase inhibitor fungicides at three levels ranged from 72.0 to 111.6% with relative standard deviations of 3.4–14.1% (n = 5). The proposed method was successfully used for the rapid determination of seven succinate dehydrogenase inhibitor fungicides in watermelon.     

Rapid pretreatment and determination of bisphenol A in water samples based on vortex‐assisted liquid–liquid microextraction followed by high‐performance liquid chromatography with fluorescence detection

A method for the rapid pretreatment and determination of bisphenol A in water samples based on vortex‐assisted liquid–liquid microextraction followed by high‐performance liquid chromatography with fluorescence detection was proposed in this paper. A simple apparatus consisting of a test tube and a cut‐glass dropper was designed and applied to collect the floating extraction drop in liquid–liquid microextraction when low‐density organic solvent was used as the extraction solvent. Solidification and melting steps that were tedious but necessary once the low‐density organic solvent used as extraction solvent could be avoided by using this apparatus. Bisphenol A was selected as model pollutant and vortex‐assisted liquid–liquid microextraction was employed to investigate the usefulness of the apparatus. High‐performance liquid chromatography with fluorescence detection was selected as the analytical tool for the detection of bisphenol A. The linear dynamic range was from 0.10 to 100 μg/L for bisphenol A, with good squared regression coefficient (r² = 0.9990). The relative standard deviation (n = 7) was 4.7% and the limit of detection was 0.02 μg/L. The proposed method had been applied to the determination of bisphenol A in natural water samples and was shown to be economical, fast, and convenient.     

Simultaneous dispersive liquid–liquid microextraction based on a low‐density solvent and derivatization followed by gas chromatography for the simultaneous determination of chloroanisoles and the precursor 2,4,6‐trichlorophenol in water samples

Chloroanisoles, particularly 2,4,6‐trichloroanisole, are commonly identified as major taste and odor compounds in water. In the present study, a simple and efficient method was established for the simultaneous determination of chloroanisoles and the precursor 2,4,6‐trichlorophenol in water by using low‐density‐solvent‐based simultaneous dispersive liquid–liquid microextraction and derivatization followed by gas chromatography with electron capture detection. 2,4‐Dichloroanisole, 2,6‐dichloroanisole, 2,4,6‐trichloroanisole, 2,3,4‐trichloroanisole, and 2,3,6‐trichloroanisole were the chloroanisoles evaluated. Several important parameters of the extraction‐derivatization procedures, including the types and volumes of extraction solvent and disperser solvent, concentrations of derivatization agent and base, salt addition, extraction‐derivatization time, and temperature were optimized. Under the optimized conditions (80 μL of isooctane as extraction solvent, 500 μL of methanol as disperser solvent, 60 μL of acetic anhydride as derivatization agent, 0.75% of Na₂CO₃ addition w/v, extraction‐derivatization temperature of 25°C, without salt addition), a good linearity of the calibration curve was observed by the square of correlation coefficients (R²) ranging from 0.9936 to 0.9992. Repeatability and reproducibility of the method were < 4.5% and <7.3%, respectively. Recovery rates ranged from 85.2 to 101.4%, and limits of detection ranged from 3.0 to 8.7 ng/L. The proposed method was applied successfully for the determination of chloroanisoles and 2,4,6‐trichlorophenol in water samples.