Carbon nanotube reinforced hollow fiber solid/liquid phase microextraction: A novel extraction technique for the measurement of caffeic acid in Echinacea purpurea herbal extracts combined with high-performance liquid chromatography

A new design of hollow fiber solid–liquid phase microextraction (HF-SLPME) was developed for the determination of caffeic acid in medicinal plants samples as Echinacea purpure. The membrane extraction with sorbent interface used in this research is a three-phase supported liquid membrane consisting of an aqueous (donor phase), organic solvent/nano sorbent (membrane) and aqueous (acceptor phase) system operated in direct immersion sampling mode. The multi-walled carbon nanotube dispersed in the organic solvent is held in the pores of a porous membrane supported by capillary forces and sonification. It is in contact with two aqueous phases: the donor phase, which is the aqueous sample, and the acceptor phase, usually an aqueous buffer. All microextraction experiments were supported using an Accurel Q3/2 polypropylene hollow fiber membrane (600 μm I.D., 200 μm wall thicknesses, and 0.2 μm pore size). The experimental setup is very simple and highly affordable. The hollow fiber is disposable, so single use of the fiber reduces the risk of cross-contamination and carry-over problems. The proposed method allows the very effective and enriched recuperation of an acidic analyte into one single extract. In order to obtain high enrichment and extraction efficiency of the analyte using this novel technique, the main parameters were optimized. Under the optimized extraction conditions, the method showed good linearity (0.0001–50 μg/L), repeatability, low limits of detection (0.00005 μg/L) and excellent enrichment (EF = 2108).     

Three-phase system in solvent bar microextraction: An approach for the sample preparation of ionizable organic compounds prior to liquid chromatography

In this article, a simple new solvent microextraction technique is described for the extraction of ionizable organic compounds. This involves performing simultaneous forward- and back-extraction across an organic film immobilized in the pores of a porous polypropylene hollow fiber. Four chlorophenoxyacetic acid herbicides were chosen as model compounds. The target compounds are extracted from the stirred acidic aqueous sample (adjusted to 0.5 M HCl; donor phase) through a thin film of an organic solvent residing in the pores of a polypropylene hollow fiber; they are then finally extracted into another alkaline aqueous phase (1 M NaOH; acceptor phase). Both ends of the fiber are pressure-sealed. The acceptor phase was analyzed by liquid chromatography (LC). This method gave good enrichment (by a factor of 438-553) of the analytes in 40 min extraction time with reasonably good reproducibility. The analytical potential of the method was demonstrated by applying the method to spiked river water sample.     

Carbon nanotube mediated microscale membrane extraction

We demonstrate that functionalized carbon nanotubes can be readily immobilized into the pore structure of a polymeric membrane, which can dramatically improve its performance in analytical scale membrane extraction. This was accomplished by injecting an aqueous dispersion of the nanotubes through a polypropylene hollow fiber under pressure. The nanotubes were trapped and held within the pores and served as sorbents facilitating solute exchange from the donor to the acceptor phase. The effectiveness of this carbon nanotube mediated process was studied by direct solvent enrichment of nonpolar organics, and also by selective extraction of organic acids via a supported liquid membrane. In both cases, the enrichment factor measured as the ratio of concentrations in the acceptor to the donor phases could be increased by more than 200%.     

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.     

Application of continual injection liquid‐phase microextraction method coupled with liquid chromatography to the analysis of organophosphorus pesticides

A liquid‐phase microextraction coupled with LC method has been developed for the determination of organophosphorus pesticides (methidation, quinalphos and profenofos) in drinking water samples. In this method, a small amount (3 μL) of isooctane as the acceptor phase was introduced continually to fill‐up the channel of a 1.5 cm polypropylene hollow fiber using a microsyringe while the hollow fiber was immersed in an aqueous donor solution. A portion of the acceptor phase (ca. 0.4 μL) was first introduced into the hollow fiber and additional amounts (ca. 0.2 μL) of the acceptor phase were introduced to replenish at intervals of 3 min until set end of extraction (40 min). After extraction, the acceptor phase was withdrawn and transferred into a 2 mL vial for a drying step prior to injection into a LC system. Parameters that affect the extraction efficiency were studied including the organic solvent, length of fiber, volume of acceptor and donor phase, stirring rate, extraction time, and effect of salting out. The proposed method provided good enrichment factors of up to 189.50, with RSD ranging from 0.10 to 0.29%, analyte recoveries of over 79.80% and good linearity ranging from 10.0 to 1.25 mg/L. The LOD ranged from 2.86 to 82.66 μg/L. This method was applied successfully to the determination of organophosphorus pesticides in selected drinking water samples.     

A novel approach to automation of dynamic hollow fiber liquid-phase microextraction

An automated dynamic two-phase hollow fiber microextraction apparatus combined with high-performance liquid chromatography was developed for extraction and determination of chlorophenoxy acid (CPA) herbicides from environmental samples. The extraction device, called TT-extractor, consists of a polypropylene hollow fiber mounted inside a stainless steel tube by means of two tee-connectors in flow system. An organic solvent, which fills the lumen and the pores of the hydrophobic fiber, is pumped through the fiber repeatedly and the sample is pumped along the outer side of the fiber. The factors affecting the dynamic hollow fiber liquid-phase microextraction (DHF-LPME) of target analytes were investigated and the optimal extraction conditions were established. To test the applicability of the designed instrument, CPAs were extracted from environmental aqueous samples. The limits of detection (LODs) as low as 0.5 μg/L, linear dynamic range in the range of 1-100 μg/L and the relative standard deviations of <7% were obtained. The developed method can provide perconcentration factors as large as 230. A hollow fiber membrane can be used at least 20 times with neither loss in the efficiency nor carryover of the analytes between runs. The system is cheap and convenient and requires minimal manual handling.     

Liquid-liquid-liquid microextraction with automated movement of the acceptor and the donor phase for the extraction of phenoxyacetic acids prior to liquid chromatography detection

A simple liquid-liquid-liquid microextraction with automated movement of the acceptor and the donor phase (LLLME/AMADP) technique is described for the quantitative determination of five phenoxyacetic acids in water using a disposable and ready to use hollow fiber. The target compounds were extracted from the acidified sample solution (donor phase) into the organic solvent residing in the pores of the hollow fiber and then back extracted into the alkaline solution (acceptor phase) inside the lumen of the hollow fiber. The fiber was held by a conventional 10-microl syringe. The acceptor phase was sandwiched between the plunger and a small volume of the organic solvent (microcap). The acceptor solution was repeatedly moved in and out of the hollow fiber assisted by a programmable syringe pump. This repeated movement provides a fresh acceptor phase to come in-contact with the organic phase and thus enhancing extraction kinetics leading to high enrichment of the analytes. The microcap separates the aqueous acceptor phase and the donor phase in addition of being partially responsible for mass transfer of the analytes from donor solution (moving in and out of the hollow fiber from the open end of the fiber) to the acceptor solution. Separation and quantitative analyses were then performed using liquid chromatography (LC) with ultraviolet (UV) detection at 280 nm. Various parameters affecting the extraction efficiency viz. type of organic solvent used for immobilization in the pores of the hollow fiber, extraction time, stirring speed, effect of sodium chloride, and concentration of donor and acceptor phases were studied. Repeatability (RSD, 3.2-7.4%), correlation coefficient (0.996-0.999), detection limit (0.2-2.8 ng ml(-1)) and enrichment factors (129-240) were also investigated. Relative recovery (87-101%) and absolute recoveries (4.6-13%) have also been calculated. The developed method was applied for the analysis of river water.     

Determination of estrogens in wastewater using three-phase hollow fiber-mediated liquid-phase microextraction followed by HPLC

Three-phase hollow fiber-mediated liquid-phase microextraction followed by HPLC was used for the determination of three synthetic estrogens, namely diethylstilbestrol, dienestrol, and hexestrol, in wastewater. Extraction conditions including organic solvent, volume ratio between donor solution and acceptor phase, extraction time, stirring rate, donor phase and acceptor phase were optimized. The target compounds were extracted from a 10 mL aqueous sample at pH 1.5 (donor solution) through a 45 mm in length hollow polypropylene fiber that was immersed in 1-octanol in advance, and then the hollow fiber was filled with 10 microL 0.5 mol/L sodium hydroxide solution (acceptor phase). After a 40 min extraction, the acceptor phase was directly injected into an HPLC system for detection. Under the optimized extraction conditions, a large enrichment factor (more than 300-fold) was achieved for the three estrogens. The determination limit at an S/N of 3 ranged from 0.25 to 0.5 microg/L for the estrogens. The recovery ratio was more than 86% in the determination of these estrogens in wastewater.     

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.     

Dynamic hollow fiber protected liquid phase microextraction and quantification using gas chromatography combined with electron capture detection of organochlorine pesticides in green tea leaves and ready-to-drink tea

The dynamic hollow fiber protected liquid phase microextraction (DHFP-LPME) technique was evaluated for the extraction of organochlorine pesticides (OCPs) in green tea leaves and ready-to-drink tea prior to gas chromatography combined-electron capture detection (GC-ECD) analysis. A conventional microsyringe with a 1.5 cm length of hollow fiber attached to its needle was connected to a syringe pump to perform the extraction. The microsyringe was used as both the microextraction device and the sample introduction device for GC-ECD analysis. In this work, the organochlorine pesticides were extracted and condensed to a volume of 3 microl of organic extracting solvent (1-octanol) confined within a 1.5 cm length of hollow fiber. The effects of extraction solvent, extraction time, sample agitation, plunger speed, and extraction temperature and salt concentration content on the extraction performance were also investigated. Good enrichments were achieved (34-297-fold) with this method, and good repeatabilities of extraction were obtained, with full name (RSDs) below 12.57%. Detection limits were much below 1 microg l(-1) for ready-to-drink tea and much below 1 microg g(-1) for green tea leaves.     

Hollow fiber‐based liquid membrane microextraction combined with high‐performance liquid chromatography for extraction and determination of trimetazidine in human plasma

A hollow fiber‐based liquid phase microextraction strategy combined with high‐performance liquid chromatography was evaluated for the quantitative determination of trimetazidine in human plasma. Trimetazidine was extracted from a 2.1 mL basified plasma sample (donor phase) into the organic solvent (n‐octanol) impregnated in the pores of a hollow fiber and then extracted into an acidic solution (acceptor phase) inside the lumen of the hollow fiber. The result showed that transport of drugs from alkaline sample solution into 0.5 m HCl occurred efficiently when 25 μL of 250 mm sodium 1‐octanesulfonate was added into the donor phase. Several parameters influencing the efficiency of the method, such as the nature of organic solvent used to impregnate the membrane, compositions of donor phase and acceptor phase, type and concentration of carrier, extraction time, stirring rate and salt concentration, were investigated and optimized. Under the optimal conditions, the calibration curves were obtained in the range of 5–200 ng/mL with reasonable linearity (r > 0.9980). The method was successfully applied to determine the concentration of trimetazidine in human plasma. Copyright © 2012 John Wiley & Sons, Ltd.     

On‐line extraction and determination of two herbicides: Comparison between two modes of three‐phase hollow fiber microextraction

Two different modes of three‐phase hollow fiber liquid‐phase microextraction were studied for the extraction of two herbicides, bensulfuron‐methyl and linuron. In these two modes, the acceptor phases in the lumen of the hollow fiber were aqueous and organic solvents. The extraction and determination were performed using an automated hollow fiber microextraction instrument followed by high‐performance liquid chromatography. For both three‐phase hollow fiber liquid‐phase microextraction modes, the effect of the main parameters on the extraction efficiency were investigated and optimized by central composite design. Under optimal conditions, both modes showed good linearity and repeatability, but the three‐phase hollow fiber liquid‐phase microextraction based on two immiscible organic solvents has a better extraction efficiency and figures of merit. The calibration curves for three‐phase hollow fiber liquid‐phase microextraction with an organic acceptor phase were linear in the range of 0.3–200 and 0.1–150 μg/L and the limits of detection were 0.1 and 0.06 μg/L for bensulfuron‐methyl and linuron, respectively. For the conventional three‐phase hollow fiber liquid‐phase microextraction, the calibration curves were linear in the range of 3.0–250 and 15–400 μg/L and LODs were 1.0 and 5.0 μg/L for bensulfuron‐methyl and linuron, respectively. The real sample analysis was carried out by three‐phase hollow fiber liquid phase microextraction based on two immiscible organic solvents because of its more favorable characteristics.     

Liquid-liquid-liquid microextraction of nitrophenols with a hollow fiber membrane prior to capillary liquid chromatography

A simple liquid-liquid-liquid microextraction device utilizing a 2 cm x 0.6 mm I.D. hollow fiber membrane was used to preconcentrate nitrophenols from water sample prior to capillary liquid chromatography (cLC) analysis. The extraction procedure was induced by the pH difference inside and outside the hollow fiber. The donor phase outside the hollow fiber was adjusted to pH approximately 1 with HCl; the acceptor phase was NaOH solution used at various concentrations. Organic solvent was immobilized into the pores of the hollow fiber. With stirring, the neutral nitrophenols outside the fiber were extracted into the organic solvent, then back extracted into 2 microl of basic acceptor solution inside the fiber. The acceptor phase was then withdrawn into a microsyringe and injected into the cLC system directly. This technique used a low-cost disposable extraction "device" and is very convenient to operate. Up to 380-fold enrichment of analytes could be achieved. This procedure could also serve as a sample clean-up step because large molecules and basic compounds were not extracted into the acceptor phase. The RSD (n=6) was less than 6.2%, while the linear calibration range was from 1 to 200 microg/ml with r>0.998. The procedure was applied to the analysis of seawater.     

Liquid–liquid–solid microextraction based on membrane-protected molecularly imprinted polymer fiber for trace analysis of triazines in complex aqueous samples

A novel liquid–liquid–solid microextraction (LLSME) technique based on porous membrane-protected molecularly imprinted polymer (MIP)-coated silica fiber has been developed. In this technique, a MIP-coated silica fiber was protected with a length of porous polypropylene hollow fiber membrane which was filled with water-immiscible organic phase. Subsequently the whole device was immersed into aqueous sample for extraction. The LLSME technique was a three-phase microextraction approach. The target analytes were firstly extracted from the aqueous sample through a few microliters of organic phase residing in the pores and lumen of the membrane, and were then finally extracted onto the MIP fiber. A terbutylazine MIP-coated silica fiber was adopted as an example to demonstrate the feasibility of the novel LLSME method. The extraction parameters such as the organic solvent, extraction and desorption time were investigated. Comparison of the LLSME technique was made with molecularly imprinted polymer based solid-phase microextraction (MIP-SPME) and hollow fiber membrane-based liquid-phase microextraction (HF-LPME), respectively. The LLSME, integrating the advantages of high selectivity of MIP-SPME and enrichment and sample cleanup capability of the HF-LPME into a single device, is a promising sample preparation method for complex samples. Moreover, the new technique overcomes the problem of disturbance from water when the MIP-SPME fiber was exposed directly to aqueous samples. Applications to analysis of triazine herbicides in sludge water, watermelon, milk and urine samples were evaluated to access the real sample application of the LLSME method by coupling with high-performance liquid chromatography (HPLC). Low limits of detection (0.006–0.02 μg L⁻¹), satisfactory recoveries and good repeatability for real sample (RSD 1.2–9.6%, n = 5) were obtained. The method was demonstrated to be a fast, selective and sensitive pretreatment method for trace analysis of triazines in complex aqueous samples.     

Extraction of hydroxyaromatic compounds in river water by liquid-liquid-liquid microextraction with automated movement of the acceptor and the donor phase

Liquid-liquid-liquid microextraction with automated movement of the acceptor and the donor phase technique is described for the extraction of six hydroxyaromatic compounds in river water using a disposable and ready to use hollow fiber. Separation and quantitative analyses were performed using LC with UV detection at 254 nm. Analytes were extracted from the acidified sample solution (donor phase) into the organic solvent impregnated in the pores of the hollow fiber and then back extracted into the alkaline solution (acceptor phase) inside the lumen of the hollow fiber. The fiber was held by a conventional 10 microL LC syringe. The acceptor phase was sandwitched between the plunger and a small volume of the organic solvent (microcap). The acceptor solution was repeatedly moved in and out of the hollow fiber using a syringe pump. This movement provides a fresh acceptor phase to come in contact with the organic phase and thus enhancing extraction kinetics thereby leading to the improvement in enrichment of the analytes. The microcap separates the acceptor phase and the donor phase in addition to being partially responsible for mass transfer of the analytes from the donor solution to the acceptor solution. Under stirring, a fresh donor phase will enter through the open end of the fiber that will also contribute to the mass transfer. Various parameters affecting the extraction efficiency viz type of organic solvent, extraction time, stirring speed, effect of sodium chloride, and concentration of donor and acceptor phases were studied. RSD (3.9-5.6%), correlation coefficient (0.995-0.997), detection limit (2.0-51.2 ng/mL), enrichment factor (339-630), relative recovery (93.2-97.9%), and absolute recovery (33.9-63.0%) have also been investigated. The developed method was applied for the analysis of river water.     

Dynamic three-phase hollow fiber microextraction based on two immiscible organic solvents with automated movement of the acceptor phase

Dynamic three-phase hollow fiber liquid-liquid-liquid microextraction (HF-LLLME) based on two immiscible organic solvents, with automated movement of organic acceptor phase to facilitate mass transfer was introduced for the first time. Polycyclic aromatic hydrocarbons were used as model compounds and extracted from water and soil samples. The extraction involved filling an 8 cm length of hollow fiber with 25 μL of organic acceptor solvent using a microsyringe, followed by impregnation of the pores in the fiber wall with n-dodecane. The fiber was then immersed in 20 mL of aqueous sample solution. During extraction, the organic acceptor phase was repeatedly moved in the lumen of the hollow fiber by movement of the syringe plunger controlled by programmable syringe pump. Following this microextraction, 2 μL of organic acceptor phase was injected into gas chromatography-flame ionization detector. This new technique provided up to 554-fold preconcentration of the analytes under the optimized conditions. Good repeatabilities (with RSDs ≤8.4%) were obtained. Detection limits were in the range of 0.2-0.5 μg/L. The utilization of the proposed method for extraction of the polycyclic aromatic hydrocarbons from different real samples (such as water and soil samples) also gave good precision and recovery.     

Preconcentration and determination of naproxen in water samples by functionalized multi-walled carbon nanotubes hollow fiber solid phase microextraction—HPLC

A simple, sensitive and selective solid phase microextraction with hollow fiber-supported multi-walled carbon nanotube functionalization reinforced sol–gel combined HPLC method was proposed for the determination of naproxen in tap, well and river water samples. In this method, functionalized multi-walled carbon nanotubes (MWCNTs) were prepared and held in pores of hollow fiber with sol–gel technology by immersion of polypropylene hollow fiber segment into the sol of the functionalized MWCNTs/silica composite and ultrasonically treated at room temperature. Effect of main parameters such as volume of donor phase, pH, extraction time, desorption time, type of desorption solvent, sample ionic strength and stirring rate were studied. Under optimum conditions, linearity was observed in the range of 0.03–500 ng/mL, with correlation coefficients of 0.997. The relative standard deviation for three replicate determinations of 50 ng/mL of naproxen was 4.3%. Limit of detection and pre-concentration factor were 0.008 ng/mL and 198, respectively. In order to check the applicability of the proposed method, it was used to determine trace levels of naproxen in different water samples.     

Development and application of microporous hollow fiber protected liquid-phase microextraction via gaseous diffusion to the determination of phenols in water

A new organic solvent-free microextraction technique termed liquid-gas-liquid microextraction (LGLME) was developed. In this technique, a small amount (6 microl) of aqueous acceptor solution (0.5M NaOH) is introduced into the channel of a 2.65 cm polypropylene hollow fiber. The hollow fiber is then immersed in an aqueous sample donor solution. The aqueous acceptor phase in the channel of the hollow fiber is separated from the sample solution by the hydrophobic microporous hollow fiber wall with air inside its pores. The analytes (phenols) passed through the microporous hollow fiber membrane by gas diffusion and were then trapped by the basic acceptor solution. After extraction, the acceptor solution was withdrawn into a microsyringe and injected into a capillary electrophoresis sample vial for subsequent analysis. Limits of detection of between 0.5 and 10 microg/l for eight phenols could be achieved. The relative standard deviations (n=6) of this technique between 2.7 and 7.6%. The technique also provides good enrichment factors for all the eight analytes.     

Analysis of trace amounts of chlorobenzenes in water samples: An approach towards the automation of dynamic hollow fiber liquid-phase microextraction

We have combined dynamic hollow fiber liquid-phase microextraction with GC and electron capture detection for the quantitative determination of five chlorobenzenes in water samples. Extraction is based on an automated dynamic extraction device called TT-tube extractor which consists of a polypropylene hollow fiber mounted inside a stainless steel tube. Toluene is used as the extraction solvent that fills the lumen and pores of the hydrophobic fiber and flows through the lumen of the fiber using a programmable syringe pump. The type of organic solvent, ionic strength, diameter of the TT-tube, sample volume, and the times for extraction and dwelling were optimized. Under optimum conditions, the method gives limits of detection as low as 10–100?ng?L^?1, a linear dynamic range of 0.05–100?μg?L^?1, and relative standard deviations of <7% (n?=?6). The preconcentration factor can be as large as 562–973. In an example for a practical application, the chlorobenzenes were successfully determined in environmental aqueous samples. The hollow fiber membrane can be used at least 20 times without any carry-over or loss in extraction efficiency. The system is inexpensive and convenient, and requires minimal manual handling.

Ionic liquid based three-phase liquid-liquid-liquid solvent bar microextraction for the determination of phenols in seawater samples

For the first time, an ionic liquid based three-phase liquid-liquid-liquid solvent bar microextraction (IL-LLL-SBME) was developed for the analysis of phenols in seawater samples. The ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([BMIM][PF(6)]), was used as the intermediary solvent for LLL-SBME, enhancing the extraction efficiency for polar analytes. In the procedure, the analytes were extracted from the aqueous sample into the ionic liquid intermediary and finally, back-extracted into an aqueous acceptor solution in the lumen of the hollow fiber. The porous polypropylene membrane acted as a filter to prevent potential interfering materials from being extracted, and no additional cleanup was required. After extraction, the acceptor solution could be directly injected into a high-performance liquid chromatographic system for analysis. Six phenols, 2-nitrophenol, 4-chlorophenol, 2,3-dichlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol were selected here as model compounds for developing and evaluating the method. The most influential extraction parameters were evaluated, including the ionic liquid, the composition of donor solution and acceptor solution, the extraction time and the extraction temperature, the effect of ionic strength, and the agitation speed. Under the most favorable extraction parameters, the method showed good linearity (from 0.05-50 to 0.5-50 μg/L, depending on the analytes) and repeatability of extractions (RSD below 8.3%, n=5). The proposed method was compared to conventional three-phase LLL-SBME and ionic liquid supported hollow fiber protected three-phase liquid-liquid-liquid microextraction, and showed higher extraction efficiency. The proposed method was demonstrated to be a simple, fast, and efficient method for the analysis of phenols from environmental water samples.