Graphene oxide reinforced polymeric ionic liquid monolith solid‐phase microextraction sorbent for high‐performance liquid chromatography analysis of phenolic compounds in aqueous environmental samples

A graphene oxide reinforced polymeric ionic liquids monolith was obtained by copolymerization of graphene oxide doped 1‐(3‐aminopropyl)‐3‐(4‐vinylbenzyl)imidazolium 4‐styrenesulfonate monomer and 1,6‐di‐(3‐vinylimidazolium) hexane bihexafluorophosphate cross‐linking agent. Coupled to high‐performance liquid chromatography, the monolith was used as a solid‐phase microextraction sorbent to analyze several phenolic compounds in aqueous samples. Under the optimized extraction and desorption conditions, linear ranges were 5–400 μg/L for 3‐nitrophenol, 2‐nitrophenol, and 2,5‐dichlorophenol and 2–400 μg/L for 4‐chlorophenol, 2‐methylphenol, and 2,4,6‐trichlorophenol (R² = 0.9973–0.9988). The limits of detection were 0.5 μg/L for 3‐nitrophenol and 2‐nitrophenol and 0.2 μg/L for the rest of the analytes. The proposed method was used to determine target analytes in groundwater from an industrial park and river water. None of the analytes was detected. Relative recoveries were in the range of 75.5–113%.     

Matrix solid‐phase dispersion coupled with homogeneous ionic liquid microextraction for the determination of sulfonamides in animal tissues using high‐performance liquid chromatography

Matrix solid‐phase dispersion coupled with homogeneous ionic liquid microextraction was developed and applied to the extraction of some sulfonamides, including sulfamerazine, sulfamethazine, sulfathiazole, sulfachloropyridazine, sulfadoxine, sulfisoxazole, and sulfaphenazole, in animal tissues. High‐performance liquid chromatography was applied to the separation and determination of the target analytes. The solid sample was directly treated by matrix solid‐phase dispersion and the eluate obtained was treated by homogeneous ionic liquid microextraction. The ionic liquid was used as the extraction solvent in this method, which may result in the improvement of the recoveries of the target analytes. To avoid using organic solvent and reduce environmental pollution, water was used as the elution solvent of matrix solid‐phase dispersion. The effects of the experimental parameters on recoveries, including the type and volume of ionic liquid, type of dispersant, ratio of sample to dispersant, pH value of elution solvent, volume of elution solvent, amount of salt in eluate, amount of ion‐pairing agent (NH₄PF₆), and centrifuging time, were evaluated. When the present method was applied to the analysis of animal tissues, the recoveries of the analytes ranged from 85.4 to 118.0%, and the relative standard deviations were lower than 9.30%. The detection limits for the analytes were 4.3–13.4 μg/kg.     

Bis(trifluoromethylsulfonyl)imide‐based frozen ionic liquid for the hollow‐fiber solid‐phase microextraction of dichlorodiphenyltrichloroethane and its main metabolites

1‐Hexadecyl‐3‐methylimidazolium bis(trifluoromethylsulfonyl)imide is a solid‐phase ionic organic material under ambient temperature and is considered as a kind of “frozen” ionic liquid. Because of their solid‐state and ultra‐hydrophobicity, “frozen” ionic liquids are able to be confined in the pores of hollow fiber, based on which a simple method was developed for the hollow‐fiber solid‐phase microextraction of dichlorodiphenyltrichloroethane and its main metabolites. Under optimized conditions, the proposed method results in good linearity (R ² > 0.9965) over the range of 0.5−50 μg/L, with low limits of detection and quantification in the range of 0.33−0.38 and 1.00−1.25 μg/L, respectively. Intra‐ and interday precisions evaluated by relative standard deviation were 3−6 and 1−6%, respectively. The spiked recoveries of dichlorodiphenyltrichloroethane and its main metabolites from real water samples were in the range of 64−113 and 79−112%, respectively, at two different concentration levels. The results suggest that “frozen” ionic liquids are promising for use as a class of novel sorbents.     

Polymeric ionic liquid modified stainless steel wire as a novel fiber for solid‐phase microextraction

A polymeric ionic liquid modified stainless steel wire for solid‐phase microextraction was reported. Mercaptopropyl‐functionalized stainless steel wire that was formed by co‐condensation of tetramethoxysilane and 3‐mercaptopropyltrimethoxysilane via a sol‐gel process, which is followed by in situ surface radical chain‐transfer polymerization of 1‐vinyl‐3‐octylimidazolium hexafluorophosphate to result in polymeric ionic liquid modified stainless steel wire. The fiber surface was characterized by field emission scanning electron microscope equipped with energy dispersive X‐ray analysis. Coupled with GC, extraction performance of the fiber was tested with phenols and polycyclic aromatic hydrocarbons as model analytes. Effects of extraction and desorption conditions were investigated systematically in our work. RSDs for single‐fiber repeatability and fiber‐to‐fiber reproducibility were less than 7.34 and 16.82%, respectively. The calibration curves were linear in a wide range for all analytes and the detection limits were in the range of 10–60 ng L^?1. Two real water samples from the Yellow River and local waterworks were applied to test the as‐established solid‐phase microextraction–GC method with the recoveries of samples spiked at 10 μg L^?1 ranged from 83.35 to 119.24%. The fiber not only exhibited excellent extraction efficiency, but also very good rigidity, stability and durability.     

Basalt fibers grafted with a poly(ionic liquids) coating for in‐tube solid‐phase microextraction

To improve the durability and extraction efficiency of an ionic liquid coating, 1‐dodecyl‐3‐vinylimidazolium bromide was polymerized and grafted onto basalt fibers for in‐tube solid‐phase microextraction. To develop an extraction tube, basalt fibers grafted with the poly(ionic liquids) coating were filled into a polyether ether ketone tube with a 0.75 mm inner diameter. The extraction tube was connected to high‐performance liquid chromatography system equipped with a sampling pump to build an online enrichment and analysis system. Using four common phthalates as model analytes, the extraction tube was investigated by the online analysis system. Good enrichment performance was exhibited by high enrichment factors ranging from 851 to 1858. Under the optimum conditions, an online analysis method was established, and good linearity (0.03–12 and 0.15–12 μg/L) and low limits of detection (0.01–0.05 μg/L) were achieved. This analysis method was applied to real samples including water in a disposable plastic box and the bottled water, some targets were detected but not quantified, and the relative recoveries spiked at 2, 5 and 10 μg/L were in the range of 86.4–119.5%.     

Matrix solid‐phase dispersion coupled with hollow fiber liquid phase microextraction for determination of triazine herbicides in peanuts

Two extraction procedures, matrix solid‐phase dispersion and hollow fiber liquid‐phase microextraction, were combined and applied to determine triazine herbicides in peanut samples. The results showed that the established method has high extraction efficiency and could greatly eliminate the interferences from complex matrix samples. A series of important experimental parameters were all investigated in detail. Under the optimal conditions, the developed method has the limits of detection for triazine herbicides in the range of 0.05 to 1.71 μg/kg. Moreover, it has the recovery in the range of 80.4–120.0% with relative standard deviations of equal or lower than 8.9%. The established method may have a great potential in separation, enrichment, and purification of triazines from complex fatty solid samples.     

Ionic liquid chemically bonded basalt fibers for in‐tube solid‐phase microextraction

Ionic liquids have been widely used in different fields by advantage of their specific properties. In this work, 1‐methyl‐3‐(3‐trimethoxysilyl propyl)imidazolium chloride was prepared and chemically bonded onto basalt fibers for in‐tube solid‐phase microextraction. Through combining in‐tube extraction device with high‐performance liquid chromatography equipped with a diode array detector, an online enrichment and analysis method for eight polycyclic aromatic hydrocarbons was established under the optimum conditions. A good enrichment factor (52–814), good linearity (0.10–15 and 0.20–15 μg/L), low limits of detection (0.03–0.05 μg/L), and low limits of quantitation (0.10–0.20 μg/L) were achieved using a sample volume of 50 mL. Analysis method was applied to the real samples including the groundwater and wastewater from a chemical industry park, some target analytes were detected and the relative recoveries were in the range of 80.4–116.8%.     

Ionic‐liquid‐modified magnetic nanoparticles as a solid‐phase extraction adsorbent coupled with high‐performance liquid chromatography for the determination of linear alkylbenzene sulfonates in water samples

Novel ionic‐liquid‐functionalized Fe₃O₄ magnetic nanoparticles were synthesized by the thiol‐ene click reaction. The prepared functionalized Fe₃O₄ nanoparticles possessed multiple interactions, such as electrostatic, hydrophobic, and π–π interactions. The functionalized Fe₃O₄ nanoparticles were characterized by using Fourier transform infrared spectroscopy, X‐ray diffraction, vibrating sample magnetometry, and transmission electron microscopy. Four kinds of linear alkylbenzene sulfonates, namely, sodium decylbenzenesulfonate, sodium undecylbenzene sulfonate, sodium dodecylbenzenesulfonate, and sodium tridecylbenzenesulfonate, were selected as model compounds to evaluate the applicability of adsorbents for extraction and subjected to high‐performance liquid chromatography analysis. In addition, the effects of various parameters, such as sorbent amount, pH value, ionic strength, sample volume, extraction time, and elution conditions on extraction efficiency were studied in detail. Under the optimum conditions, good linearities were attained, with correlation coefficients between 0.9912 and 0.9968. The proposed method exhibited limits of detection ranging from 0.061 to 0.099 μg/L for all the target analytes. The spiked recoveries of the target analytes in real water samples ranged from 86.3 to 107.5%, with relative standard deviations lower than 7.96%. The enrichment factors of the analytes ranged from 364 to 391, indicating that the obtained functionalized Fe₃O₄ nanoparticles can effectively extract trace target analytes from environmental 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%.     

Cotton thread modified with ionic liquid copolymerized polymer for online in‐tube solid‐phase microextraction and HPLC analysis of nonsteroidal anti‐inflammatory drugs

Cotton fiber is a biodegradable material that possesses properties such as high specific area, adjustable shape, and hygroscopicity. In this work, organic polymer was directly in situ grown on the surface of cotton thread and packed into a poly(ether ether ketone) tube for online in‐tube solid‐phase microextraction. The novel strategy solves the problems like high backpressure and tedious optimization process of normal monolithic polymer‐based in‐tube solid‐phase microextraction capillary. The quaternary ammonium typed ionic liquid of 1‐allyl‐methylimidazolium chloride, 4‐vinylbiphenyl, and ethylene dimethacrylate were co‐polymerized and in situ grown on the surface of cotton thread as extraction phase. The solid‐phase microextraction tube showed excellent performance for the extraction of three nonsteroidal anti‐inflammatory drugs including ketoprofen, naproxen, and flurbiprofen due to the strong ion exchange and hydrophobic interactions. After online coupling with a high‐performance liquid chromatography system by six‐port valve, the method was applied for the quantitative analysis of nonsteroidal anti‐inflammatory drugs in human plasma samples showing good enrichment performance (enrichment factor between 263 and 279), high sensitivity, good linearity, and good reproducibility.     

Coupling of solid‐phase microextraction with micellar desorption and high performance liquid chromatography for the determination of pharmaceutical residues in environmental liquid samples

A residue analytical method combining solid‐phase microextraction (SPME) with external micellar desorption (MD) and high‐performance liquid chromatography with diode array detector (HPLC‐DAD) has been developed and validated for the simultaneous determination of six pharmaceutical compounds, belonging to various therapeutic categories in water samples. Target compounds include antiinflamatory drugs (ibuprofen, ketoprofen and naproxen), an analgesic (phenazone), a lipid regulator (bezafibrate) and an antiepileptic (carbamazepine). A detailed study of the experimental conditions of extraction and desorption with different surfactants was performed in order to obtain the best results during instrumental analysis. Of the different fibers and surfactants investigated, 65 µm polydimethysiloxane‐divinilbenzene (PDMS‐DVB) fiber and polyoxyethylene 10 lauryl ether (POLE) and polyoxyethylene 6 lauryl ether (C₁₂E₆) as desorbing agents produced the optimal response to pharmaceutical residues. Recoveries obtained were generally higher than 80% and the variability of the method was below 16% for all compounds in both surfactants. Method detection limits were 0.05–12 ng mL^?1 for POLE and 0.1–5 ng mL^?1 for C₁₂E₆. The developed method was compared using external desorption with organic solvent and it was successfully applied to the determination of these pharmaceutical compounds in water samples from different origin. Solid‐phase microextraction with micellar desorption (SPME‐MD) represents a new approach for the extraction of different pharmaceutical compounds in natural waters because it combines shorter handling time, better efficiency, safety and more environmentally friendly process than the traditional methods. Copyright © 2009 John Wiley & Sons, Ltd.     

Preparation of monolithic fibers for the solid‐phase microextraction of chlorophenols in water samples

Monolithic fibers were synthesized and applied for the solid‐phase microextraction and determination of chlorophenols in environmental water samples by coupling with HPLC. The fibers were prepared by copolymerization of vinylimidazole and ethylene dimethacrylate as functional monomer and cross‐linker, respectively. The effect of the preparation conditions of monolithic fibers on the extraction efficiencies was investigated in detail. Several characteristic techniques, such as elemental analysis, infrared spectroscopy, mercury‐intrusion porosimetry, and SEM were used to characterize the monolithic material. The effect of the extraction parameters, including desorption solvent, extraction and desorption time, pH values, and ionic strength in sample matrix on the extraction performance was investigated thoroughly. Under the improved extraction conditions, the linear ranges of 2‐chlorophenol, 2,4‐dichlorophenol and pentachlorophenol were 1.0–200 μg/L and 2.0–200 μg/L for 2,4,6‐trichlorophenol. The detection limits (S/N = 3) were in the range of 0.16–0.45 μg/L, the RSDs for intraday and interday precisions were <7.0%. Finally, the proposed method was successfully used to detect different environmental water samples. The recoveries of spiked water samples were ranged from 90.0 to 115%. At the same time, satisfactory repeatability was achieved with RSDs < 9.0%.     

Determination of triazine herbicides in juice samples by microwave‐assisted ionic liquid/ionic liquid dispersive liquid–liquid microextraction coupled with high‐performance liquid chromatography

A novel microextraction method, termed microwave‐assisted ionic liquid/ionic liquid dispersive liquid–liquid microextraction, has been developed for the rapid enrichment and analysis of triazine herbicides in fruit juice samples by high‐performance liquid chromatography. Instead of using hazardous organic solvents, two kinds of ionic liquids, a hydrophobic ionic liquid (1‐hexyl‐3‐methylimidazolium hexafluorophosphate) and a hydrophilic ionic liquid (1‐butyl‐3‐methylimidazolium tetrafluoroborate), were used as the extraction solvent and dispersion agent, respectively, in this method. The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of 1‐hexyl‐3‐methylimidazolium hexafluorophosphate dispersed entirely into sample solution with the help of 1‐butyl‐3‐methylimidazolium tetrafluoroborate. In addition, an ion‐pairing agent (NH₄PF₆) was introduced to improve recoveries of the ionic liquid phase. Several experimental parameters that might affect the extraction efficiency were investigated. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 5.00–250.00 μg/L, with the correlation coefficients of 0.9982–0.9997. The practical application of this effective and green method is demonstrated by the successful analysis of triazine herbicides in four juice samples, with satisfactory recoveries (76.7–105.7%) and relative standard deviations (lower than 6.6%). In general, this method is fast, effective, and robust to determine triazine herbicides in juice samples.     

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.     

Ultrasensitive determination of highly polar trimethyl phosphate in environmental water by molecularly imprinted polymeric fiber headspace solid‐phase microextraction

A sensitive, accurate, and cost effective method for the quantification of trimethyl phosphate, which is highly polar and volatile, in environmental water is presented. Trimethyl phosphate was headspace solid‐phase microextracted on a molecularly imprinted polymeric fiber, and then the fiber was thermally desorbed in the gas chromatograph injector, and the compound was determined. The trimethyl phosphate imprinted polymeric fiber was prepared by copolymerization in a fused silica capillary tube and obtained by removal of the wall of fused silica capillary tube. The monolithic fiber displayed good selectivity toward trimethyl phosphate among its structural analogues. It was thermally stable up to 320°C so that it can withstand the high temperature of the gas chromatograph injector for desorption. The factors influencing the performance of its headspace solid‐phase microextraction were studied. Under the optimal conditions, the method for quantification of trimethyl phosphate in environmental water was well developed. It exhibited significant linearity, the lowest limit of quantification to date, and good recoveries. Using this method, trimethyl phosphate was detected in five out of seven environmental water samples at concentration levels from 0.28 to 1.22 μg/L, illustrating the heavy pollution of trimethyl phosphate in environmental water.     

Three‐phase hollow fiber liquid‐phase microextraction based on a magnetofluid for the analysis of aristolochic acids in plasma by high‐performance liquid chromatography

A new and fast sample preparation technique based on three‐phase hollow fiber liquid‐phase microextraction with a magnetofluid was developed and successfully used to quantify the aristolochic acid I (AA‐I) and AA‐II in plasma after oral administration of Caulis akebiae extract. Analysis was accomplished by reversed‐phase high‐performance liquid chromatography with fluorescence detection. Parameters that affect the hollow fiber liquid‐phase microextraction processes, such as the solvent type, pH of donor and acceptor phases, content of magnetofluid, salt content, stirring speed, hollow fiber length, extraction temperature, and extraction time, were investigated and optimized. Under the optimized conditions, the preconcentration factors for AA‐I and AA‐II were >627. The calibration curve for two AAs was linear in the range of 0.1–10 ng/mL with the correlation coefficients >0.9997. The intraday and interday precision was <5.71% and the LODs were 11 pg/mL for AA‐I and 13 pg/mL for AA‐II (S/N = 3). The separation and determination of the two AAs in plasma after oral administration of C. akebiae extract were completed by the validated method.     

Development and validation of a magnetic solid‐phase extraction with high‐performance liquid chromatography method for the simultaneous determination of amphetamine and methadone in urine

The simultaneous determination of amphetamine and methadone was carried out by magnetic graphene oxide nanoparticles, a magnetic solid‐phase extraction adsorbent, as a new sample treatment technique. The main factors (the amounts of sample volume, amount of adsorbent, type and amount of extraction organic solvent, time of extraction and desorption, pH, the ionic strength of extraction medium, and agitation rate) influencing the extraction efficiency were investigated and optimized. Under the optimized conditions, good linearity was observed in the range of 100–1500 ng/mL for amphetamine and 100–1000 ng/mL for methadone. The method was evaluated for determination of AM and methadone in positive urine samples, satisfactory results were obtained, therefore magnetic solid‐phase extraction can be applied as a novel method for the determination of drugs of abuse in forensic laboratories.     

Nanostructured‐silver‐coated polyetheretherketone tube for online in‐tube solid‐phase microextraction coupled with high‐performance liquid chromatography

Polyetheretherketone tube is a better substrate for in‐tube solid‐phase microextraction than fused‐silica capillary and metal tube because of its resistance to high pressure and good flexibility. It was modified with a nanostructured silver coating, and characterized by scanning electron microscopy and energy dispersive X‐ray spectroscopy. It was connected into high‐performance liquid chromatography equipment to build the online analysis system by replacing the sample loop of a six‐port injection valve. To get the highest extraction capacity, the preparation conditions of the coating was investigated. Important extraction conditions including length of tube, sample volume, and desorption time were optimized using eight polycyclic aromatic hydrocarbons as model analytes. The tube exhibits excellent extraction efficiency toward them, with enrichment factors from 52 to 363. The online analysis method provides good linearity (0.5–100 or 1.0–100 μg/L) and low detection limits (0.15–0.30 μg/L). It has been used to determine polycyclic aromatic hydrocarbons in water samples, with relative recoveries in the range of 92.3–120%. The tube showed highest extraction ability for polycyclic aromatic hydrocarbons, higher extraction ability for hydrophobic phthalates and anilines, and almost no extraction ability for low hydrophobic phenols, due to the possible extraction mechanism including hydrophobic and electron‐rich element‐metal interactions.     

Introduction of a coiled solid‐phase microextraction fiber based on a coating of animal bone waste for chromatographic analysis

We attempt to introduce animal bone waste as a coating material with an organic−inorganic structure for the fabrication of a coiled solid‐phase microextraction fiber for the first time. The coiled fiber was simply prepared with the use of copper wire and coated with bone waste suspension through the dip‐coating method. The bone waste coating was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and X‐ray diffraction analysis. It was applied as new type of solid‐phase microextraction fiber for preconcentration of polycyclic aromatic hydrocarbons before determination by high‐performance liquid chromatography with UV detection. A wide linear range 0.01–99.0 μg/L and limits of detection in the range 3.0–11.1 ng/L were obtained at optimized conditions. The bone waste coated coiled solid‐phase microextraction fiber has promise in sample preparation techniques because it is cost effective, available, stable in aqueous and organic solutions, environmentally friendly, and easy to fabricate and operate.     

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.