Liquid-phase Microextraction Research Articles

Sustainable eutectic mixture-based ultrasound assisted multifaceted valorisation of pineapple waste for bromelain and bioethanol production

A large number of pineapple residues like peels, leaves and stems generated during processing remains underutilized. The current investigation provides one-pot task-specific valorisation of these residues by sequential extraction of bromelain and saccharification of cellulose residue for bioethanol production. Employing natural deep eutectic solvents (NADES) prepared by mixing ammonium salts with imidazole and glycerol has guaranteed sustainable extraction of bromelain. Ultrasound-assisted liquid phase microextraction (UA-LPME) was performed and NADES with moderate density (TBC:I:G/sodium sulphate) was observed to have a higher bromelain yield and purity. Response Surface Methodology-based optimization of UA-LPME was carried out and solid: liquid ratio (25 ml/g), ultrasound time (17.5 min) and ultrasound temperature (45 °C) were observed to be influential variables resulting in an optimal bromelain yield of (87%). Sequential fractionation of the enzyme concentrate with gel filtration chromatography and anion exchange chromatography has resulted in a corresponding purity fold of 89.27. The cellulose-rich residue remaining after bromelain extraction was enzymatically saccharified (Cellic CTec2) for bioethanol production (12.7 g/L). This novel approach guarantees sustainable valorisation of pineapple waste using NADES as a sustainable extraction medium.

Green electromembrane extraction procedure based on biodegradable chitosan films for determination of polyphenolic compounds in food samples: Greenness assessment of the sample preparation approach

A simple, rapid and environmentally friendly method for the electromembrane extraction of polyphenolic compounds has been developed using chitosan films (60% (w/w) chitosan, 40% (w/w)-Aliquat®336, 10–11 μm thickness) as biopolymeric membrane. In this work for the first time with this type of chitosan-based support, the use of organic solvents has been completely eliminated, which allows considering the proposed methodology as a green solvent-free procedure, as demonstrated by performing analytical greenness metric for sample preparation (AGREEprep). Under optimal experimental conditions (10 mL donor phase, pH 7; 50 μL acceptor phase, pH 9; 100 V applied voltage for 15 min) high enrichment factors (EF ≥ 60) were obtained for all the target analytes. Wide concentration ranges between 52.8 μg L−1 and 1000 μg L−1, good linearity (R2 ≥ 0.996), low limit of detection (15.9–37.1 μg L−1), and repeatability (relative standard deviation (RSD) values 4–10%) were achieved. Polyphenolic compounds have been successfully extracted from coffee- and tea-based dietary food supplements in different formats (pills and ampoules). For comparison purposes, target analytes have additionally been determined in green coffee beans and tea.

Combination of in-situ electro synthesized Zn–Al-LDH@ pencil graphite fiber and three phase hollow fiber LPME for microextraction of some antibiotics in urine samples and quantification via HPLC-UV

In the present study, a combination of two useful extraction techniques including fiber solid phase microextraction based on the new synthesized sorbent and the porous hollow fiber liquid phase microextraction is reported. The selective anion-exchangeable Zn–Al-layered double hydroxide as a fiber was electrodeposited on the surface of pencil graphite substrate through simple and cost-effective method. The prepared fiber was characterized and put into the lumen of the porous hollow fiber, which was filled by alkaline solution. The obtained optimum condition for the method was as follows: donor phase HCl concentration of 0.10 mM, acceptor phase NaOH concentration of 7.60 mM and extraction time of 16 min. It is necessary to adjust the concentration of the donor phase in order to extract acidic analytes from an aqueous sample into an organic phase. The method was used for the quantification of three antibiotics including amoxicillin, ciprofloxacin and cefixime. The extracted antibiotics were analyzed by high performance liquid chromatography-ultraviolet detection (HPLC-UV). In the optimal conditions, the linearity of the proposed method was in the range of 0.50–500.00 μg L−1 for selected analytes in water and urine matrices. All calibration curves showed determination of coefficient higher than 0.9958. The limits of detection and limits of quantification were calculated to be between 0.08 and 0.16 μg L−1 and 0.28–0.56 μg L−1, respectively. In order to define the precision of the method, the inter-day and intra-day relative standard deviations were determined between 3.25 and 5.73% in the three selected concentrations. The enrichment factors (EFs) were between 46.20 and 55.81 for selected drugs. Moreover, the calculated absolute recoveries were between 69.30 and 83.71%. The relative recoveries were obtained in the range of 93.00–105.00%. The proposed method was also employed for analysis of various urine samples containing the selected drugs. The obtained recoveries indicated that the method was useful and applicable in complicated biological samples.

A study on the enrichment mechanism of three nitrophenol isomers in environmental water samples by charge transfer supramolecular-mediated hollow fiber liquid-phase microextraction.

To explore the mechanism of extraction and enrichment of three nitrophenol isomers by charge-transfer supramolecular synergistic three-phase microextraction system, a charge transfer supramolecular-mediated hollow fiber liquid-phase microextraction (CTSM-HF-LPME) combined with high-performance liquid chromatography-ultraviolet detector (HPLC-UV) method was established for the determination of real environmental water samples. In this study, the three nitrophenols (NPs) formed charge-transfer supramolecules with electron-rich hollow fibers, which promoted the transport of NPs in the three-phase extraction system and greatly increased the EFs of NPs. The relationships between the EFs of NPs and their solubility, pKa, apparent partition coefficient, equilibrium constant, and structural property parameters were investigated and discussed. At the same time, most of factors affecting the EFs of NPs were investigated and optimized, such as the type of extraction solvent, pH value of sample phase and acceptor phase, extraction time, and stirring speed. Under optimal conditions, the EFs of o-nitrophenol, m-nitrophenol, and p-nitrophenol were 163, 145, and 87, respectively. With good linearity in the range of 5 × 10-7 ~ 1µg/mL, and the limit of detection of 0.1pg/mL, the relative standard deviations of the method precision were lower than 7.4%, and the average recoveries were between 98.6 and 106.4%. This method had good selectivity and sensitivity, satisfactory precision, and accuracy and had been successfully applied to the trace detection of real water samples.

Programmable Millifluidic Platform Integrating Automatic Electromembrane Extraction Cleanup and In-Line Electrochemical Detection: A Proof of Concept.

A fully automatic millifluidic sensing platform coupling in-line nonsupported microelectromembrane extraction (μ-EME) with electrochemical detection (ECD) is herein proposed for the first time. Exploiting the features of the second generation of flow analysis, termed sequential injection (SI), the smart integration of SI and μ-EME-ECD enables (i) the repeatable formation of microvolumes of phases for the extraction step in a membrane-less (nonsupported) arrangement, (ii) diverting the acceptor plug to the ECD sensing device, (iii) in-line pH adjustment before the detection step, and (iv) washing of the platform for efficient removal of remnants of wetting film solvent, all entirely unsupervised. The real-life applicability of the miniaturized sensing system is studied for in-line sample cleanup and ECD of diclofenac as a model analyte after μ-EME of urine as a complex biological sample. A comprehensive study of the merits and the limitations of μ-EME solvents on ECD is presented. Under the optimal experimental conditions using 14 μL of unprocessed urine as the donor, 14 μL of 1-nonanol as the organic phase, and 14 μL of 25 mM NaOH as the acceptor in a 2.4 mm ID PTFE tubing, an extraction voltage of 250 V, and an extraction time of 10 min, an absolute (mass) extraction recovery of 48% of diclofenac in urine is obtained. The proposed flow-through system is proven to efficiently remove the interfering effect of predominantly occurring organic species in human urine on ECD with RSD% less than 8.6%.

Nylon Membrane-Based Electromembrane Extraction Coupled with Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry for the Determination of Insulin

A rapid and sensitive protein determination method that uses electromembrane extraction (EME) and is coupled with matrix-assisted laser desorption/ionization mass spectrometry (MALDI/MS) is developed. A flat nylon membrane is used to collect proteins from an aqueous solution and is directly analyzed by MALDI/MS after the addition of the MALDI matrix. Insulin is used as a model protein to investigate the optimum extraction of the parameters. The optimum EME conditions are obtained at 12 V of voltage, 10 min of extraction time, 12 mL sample volume, and 400 rpm agitation rate. The linear dynamic range (LDR) of insulin in an aqueous solution is in the range of 1.0–100.0 nM. The limit of detection (LOD) for insulin in an aqueous solution is 0.3 nM with 103-fold signal-to-noise (S/N) ratio enhancement. Furthermore, the applicability of this method to determine insulin in complicated sample matrices is also investigated. The LDR of insulin in human urine samples is in the range of 5.0–100.0 nM, and the LOD of insulin in urine samples is calculated to be 1.5 nM. The precision and accuracy of this method are evaluated at three different concentration levels, and the coefficient of variation (CV) and relative error are less than 6%. This approach is time-efficient and economical, as the flat membrane mode of EME coupled with MALDI/MS is suitable.

Determination of Three Pyrethroid Insecticides in Food by Magnetic Ionic Liquid-Based Dispersive Liquid Phase Microextraction (DLLME) with High-Performance Liquid-Chromatography (HPLC)

A simple, green, rapid, and efficient magnet ionic liquid (MIL) dispersive liquid–liquid microextraction (DLLME) method coupled with high-performance liquid chromatography (HPLC) was successfully developed for the determination of three trace pyrethroids (fenvalerate, beta-cypermethrin, and bifenthrin) in water and food samples. Tri-hexyl-tetradecyl-phosphonium tetra-chlorocobalt (II) [P6,6,6,14 +]2[CoCl4 2−] was explored as the extraction solvent due to its magnetic susceptibility, low ultraviolet absorbance, difficulty to hydrolyze in aqueous solution, and high extraction capacity. Important factors of extraction efficiency, such as the mass of MIL, pH, and ionic strength, were optimized. The spiked recoveries of the targets in water and food samples were from 96.3 to 103.8%. The detection limits were from 0.75 to 1.75 ng ml−1. The results indicated that the developed MIL-DLLME method based on [P6,6,6,14 +]2[CoCl4 2−] as the extraction solution has the advantages of rapid and high efficiency and was employed to determine pyrethroids in water and food samples.

Research Advances in the Analysis of Estrogenic Endocrine Disrupting Compounds in Milk and Dairy Products.

Milk and dairy products are sources of exposure to estrogenic endocrine disrupting compounds (e-EDCs). Estrogenic disruptors can accumulate in organisms through the food chain and may negatively affect ecosystems and organisms even at low concentrations. Therefore, the analysis of e-EDCs in dairy products is of practical significance. Continuous efforts have been made to establish effective methods to detect e-EDCs, using convenient sample pretreatments and simple steps. This review aims to summarize the recently reported pretreatment methods for estrogenic disruptors, such as solid-phase extraction (SPE) and liquid phase microextraction (LPME), determination methods including gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), Raman spectroscopy, and biosensors, to provide a reliable theoretical basis and operational method for e-EDC analysis in the future.

Preparation and further evaluation of l-menthol-based natural deep eutectic solvents as supported liquid membrane for the hollow fiber liquid-phase microextraction of sulfonamides from environmental waters

In this work, the use of a hydrophobic natural deep eutectic solvent (NADES) as supported liquid membrane (SLM) for hollow fiber liquid-phase microextraction (HF-LPME) of sulfonamides is proposed. Different NADES based on L-menthol and naturally occurring organic acids (citric acid, formic acid, acetic acid, decanoic acid, nonanoic acid, lactic acid, valeric acid, isobutyric acid, hexanoic acid, octanoic acid, and 2-methylbutyric acid) were prepared at different molar ratios. Important solvent properties to work as SLM were studied such as stability in the fiber and compatibility with HPLC. Then, the ability of the prepared NADES to extract 8 antibiotics of the family of sulfonamides (SAs) from water by HF-LPME was studied. From them, the combination of formic acid:L-menthol (1:1) was selected as optimum since it provided a better and more balanced extraction of SAs. The optimized HF-LPME procedure was applied to the analysis of an artificial water containing humic acids, tap and river water samples, showing a good clean-up ability for all the tested samples. Calibration curves showed good linearity for all the SAs and samples with linear regression coefficients (r 2 ) greater than 0.992. Relative recoveries ranged from 53 to 121%, with relative standard deviation values between 5 and 21%, depending upon the analyte and type of water sample. The limits of detection of the method varied from 0.63 to 2.85 µg/L for tap water, 0.70 to 3.23 µg/L for the Jarama river and 0.61 to 2.52 µg/L for the Manzanares river. Besides, the proposed method can be considered sustainable, according to AGREEprep tool, and greener than reported methods in the literature based in other microextraction techniques. Graphical Abstract .

Stir membrane liquid-phase microextraction based on milk fats hydrolysis and deep eutectic solvent formation: Determination of bisphenols

In this paper, a stir membrane liquid-phase microextraction approach based on milk fats hydrolysis and in situ deep eutectic solvent formation was developed for the first time. The approach was applied to clean-up and preconcentrate bisphenols from milk samples. The procedure assumed alkaline hydrolysis of samples fats to obtain water-soluble salts of fatty acids that acted as precursors for the deep eutectic solvent formation. A stir membrane disk impregnated with menthol was placed into the sample solution. The formation of microdroplets of the hydrophobic fatty acids was observed under sample acidification. Collection of the extract phase on the disk was based on deep eutectic solvent formation. Under optimal conditions, the RSD was < 6 %, limits of detection for bisphenols were 0.3–0.5 μg kg−1. The extraction recoveries were in the range of 95–97 %, which indicated the excellent capability of the developed approach to extract hydrophobic analytes from complex matrices.

Liquid-phase microextraction of ascorbic acid in food and pharmaceutical samples using ferrofluid-based on cobalt ferrite (CoFe2O4) nanoparticles

Quantitation of ascorbic acid is extremely desired in the food, cosmetic, and pharmaceutical samples. In this study, liquid-phase microextraction using ferrofluid (LPME-FF) based on the cobalt ferrite nanoparticles (CoFe2O4) coupled with a green, precise, accurate, and robust spectrofluorometric approach was used for extraction and determination of ascorbic acid. The procedure is based on the reaction between ascorbic acid (AA) and methylene blue (MB) as an inexpensive and readily available fluorescence quenching reagent. The native fluorescence intensity of MB was quenched using ascorbic acid. The CoFe2O4 magnetic nanoparticles were synthesized and confirmed by Fourier transform infrared (FT-IR) spectroscopy, vibrating sample magnetometer (VSM), field emission scanning electron microscopy (FE-SEM), and energy dispersive X-ray spectroscopy (EDXS). Three parameters of pH, ferrofluid volume, and ultrasonic time were selected as influential factors on the process and optimized by central composite design (CCD). Under optimal conditions, linear range, detection limit, and the relative standard deviation were obtained 0.26–5.70 μM, 0.074 μM and, 2.0 %, respectively. Finally, the proposed method was successfully employed for the quantification of ascorbic acid in real samples of lemon juice, orange juice, and vitamin C tablets.

Novel miniaturized passive sampling devices based on liquid phase microextraction equipped with cellulose-grafted membranes for the environmental monitoring of phthalic acid esters in natural waters

Phthalic acid esters (PAEs) are considered endocrine disruptors and potential carcinogens. Consequently, efficient and accurate environmental monitoring of trace levels of these organic pollutants is necessary to protect the population against their hazardous effects. Passive sampling techniques have gained notoriety for environmental monitoring and have been proven highly sensitive to temporal variations. This study developed a miniaturized passive sampling device (MPSD) based on hollow fiber liquid-phase microextraction (HF-LPME). The devices were calibrated in the laboratory using an automated calibration system. The results demonstrated the first-order uptake ranges for Diethyl phthalate (DEP), Diisobutyl phthalate (DiBP), Dibutyl phthalate (DBP), Benzyl butyl phthalate (BBP) and Bis(2-ethylhexyl phthalate) (DEHP) between 30 min and 24 h with sampling rates equivalent to 0.009; 0.021; 0.033; 0.085 and 0.003 mL h−1 respectively (R2 between 0.88 and 0.99). The calibrated devices were deployed in 12 marginal lagoons, stretching approximately 330 km along the main river. The extracts recovered from the devices were analyzed by gas chromatography (GC), resulting in the identification and quantification of DEP (0.697–13.7 ng L−1), DiBP (0.100–4.43 ng L−1), DBP (0.014–1.21 ng L−1), BBP (0.218–5.67 ng L−1), and DEHP (0.002–2.24 ng L−1). Despite being frequently identified, DEHP concentrations were well below the maximum established limits, revealing a good water quality in terms of the target PAEs. In contrast, screening the extracts using GCxGC was possible to detect other hazardous pollutants such as pesticides, drugs, and their metabolites. The described device was effective and reliable, providing accurate PAE measurements following short exposure periods. In this sense, its deployment during emergency operations, such as accidental discharges of industrial effluents into natural waters, could continuously and cost-effectively monitor water quality.

Determination of rhodamine B in water and cosmetics by switchable solvent-based liquid phase microextraction with spectrophotometric determination

A microextraction method has been developed for the determination of rhodamine B (Rh-B) in water and cosmetics by separation and preconcentration with liquid microextraction based upon a switchable hydrophilic solvent and determination by spectrophotometry. The analyte was extracted into the triethylamine (TEA) phase using sodium hydroxide (NaOH) to convert protonated triethylamine carbonate (P-TEA-C) to triethylamine. Various analytical parameters such as the pH of the sample solution, extraction solvent volume, and sample volumes affecting the quantitative recovery values of rhodamine B were optimized. The limit of detection (LOD) and limit of quantification (LOQ) were 2.96 and 9.88 ng/mL, respectively. The developed method was successfully applied to the determination of rhodamine B and satisfactory recovery values were obtained. The developed approach is fairly fast and an environmentally friendly alternative for the separation and preconcentration of rhodamine B water and cosmetic samples.

Microwave-Assisted Dispersive Liquid-Liquid Microextraction Combined with HPLC for the Determination of Three Biogenic Amines in Beverages.

Microwave-assisted dispersive liquid-liquid microextraction (MADLLME) coupled with high-performance liquid chromatography (HPLC) with diode array detector was used for the extraction and determination of three biogenic amines (BAs), including tryptamine, histamine and phenylethylamine in beverages (beer, cherry juice and white spirit). Compared with solid-phase extraction, solid-phase microextraction and liquid-phase microextraction, which is more solvent use with lower extraction efficiency, this MADLLME method obviously shortened analytical time, the rapid heating of aqueous samples with non-ionizing electromagnetic radiation, a lower solvent use and enhanced extraction efficiency. Because of good extraction for three BAs, [3C6PC14][FeCl4] was used as an extraction solvent. We showed a tunable selectivity of magnetic ionic liquids (MILs) toward extracting BAs by changing anion or cation due to the modification of the interaction between the MIL and the BAs. Extraction conditions including the type and volume of extraction solvent, microwave power, microwave-assisted extraction time, sample pH, disperser and interference experiment were investigated. Under the optimal conditions, a good linear relationship was found in the concentration range of 100-2,000ngmL-1 for three BAs with correlation coefficient (R2) of 0.995-0.999. The limit of detections (S/N = 3) and limit of quantitations (S/N = 10) were in the range of 3.46-4.96ngmL-1 and 10.44-14.88ngmL-1, respectively. The recoveries of three targets were in the range of 84.3-108.5%, and the relative standard deviations based on the peak areas for six replicate analyses of beverages spiked with 10, 50 and 100ngmL-1 of each biogenic amine were lower than 7.9%. This method has also been successfully applied to analyze the real samples at three different spiked concentrations, and excellent results have been obtained.

Electromembrane extraction of clenbuterol from swine urine for monitoring illegal use in livestock.

The illegal use of clenbuterol seriously endangers food safety and human health. Accurate monitoring of the illegal use of clenbuterol in livestock can efficiently prevent the clenbuterol residue pork products from entering the consumer market. Thus, in this study, a simple, rapid, and sensitive method for the determination of clenbuterol in swine urine was developed using electromembrane extraction combined with liquid chromatography-tandem mass spectrometry. It should be noted that the electromembrane extraction method presented many advantages of simple operation, fast mass transfer rate, good sample clean-up capability, and less organic solvent consumption. The effect of important factors on the extraction efficiency of clenbuterol was investigated. Under the optimal conditions, good linearity was achieved for clenbuterol over the range of 1-1000ng/ml (linear correlation [R2 ] =0.9996). The recoveries of clenbuterol in swine urine at three spiked levels ranged from 83.7% to 110.0% with relative standard deviation values lower than 9.7% (n=4). The limits of detection and quantification for clenbuterol were 0.07 and 0.25ng/ml, respectively. These results suggested that the proposed method has great potential for the extraction and determination of trace analyte in a complex sample matrix for monitoring illegal use in livestock.

Hydrophobic microporous extraction on polyurethane sponges for convenient and sensitive analysis of organic molecules in water.

Various solvent supports have been developed to overcome solvent instability during liquid-phase microextraction. The hydrophobic polyurethane sponge (PS) possesses numerous cross-linked internal microchannels and terminal micropores that can facilitate steady solvent storage capacity, high extraction efficiency, extractant loading, and recycling convenience. In this study, an easy, convenient, and efficient PS-supported liquid-phase microextraction (PS-LPME) coupled with gas chromatography-mass spectrometry (GC-MS) method was developed for the trace analysis of different organic compounds in aqueous solutions. Different extraction solvents, PS dosages, stirring speeds, and extraction times were first investigated by extracting eight polycyclic aromatic hydrocarbons (PAHs: naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, and pyrene), and then applied for the analysis of triazines, amides, chloroacetamides, and organophosphorus compounds. High enrichment factors (approximately 208-439) were observed for the monitored PAHs. Good linearities, with determination coefficients (r2 ) greater than 0.9992, were achieved in the concentration range of 0.01-50 μg L-1 . Low limits of detection and quantification were found in the ranges of 0.3-3ng L-1 and 1-10ng L-1 , respectively. At three spiked concentrations (0.1, 1, and 10μg L-1 ), good recoveries were obtained in the range of 91.6-118.5% with intra- and inter-day relative standard deviations of less than 6.4% and 11.7%, respectively. The developed PS-LPME method coupled with GC-MS was successfully applied in the analysis of different organic compounds in aqueous solutions and has shown great convenience and satisfactory enrichment performance in microextraction analysis.

Hollow-Fiber Liquid-Phase Micro-Extraction Method for the Simultaneous Derivatization, Extraction, and Pre-concentration of Organotin Compounds from Packed Fruit Juices

Organotin compounds are widely employed as pesticides and fungicides in agriculture and as stabilizers for the industrial manufacture of polyvinyl chloride and other polymers. Accordingly, these endocrine disruptors can be found in a variety of foods and beverages. In the present study, we describe the optimization of a hollow-fiber liquid-phase micro-extraction approach for the simultaneous derivatization, extraction, and pre-concentration of butyltin species from commercial fruit juices with the aim of investigating their migration from the packaging. The best extraction efficiencies were achieved by using hexane as the acceptor solvent and a polypropylene fiber length of 2 cm, whereas the agitation speed, extraction temperature, and total extraction time were set at 1100 rpm, 25 ºC, and 10 min, respectively. Using these optimal conditions, the method was satisfactorily validated in terms of linearity (5–1000 µg L−1), limits of detection (0.8–1.8 µg L−1), recovery (80.5–92.1%), intraday precision (10.2–13.1%), inter-day precision (11.0–15.5%), matrix effect (83.2–91.8%), accuracy (85.2–95.2%), specificity, and carryover. The application of this technique to commercial samples obtained from a local market demonstrated that levels of organotin species in packed fruit juices are negligible, in agreement with the limits established by the European Food Safety Authority (0.14 mg of total organotin compounds per kg of food).

Amine-based vortex-assisted liquid-phase microextraction procedure for traces of tartrazine (E102) in food and water samples

Amine-based vortex-assisted liquid-phase microextraction procedure for traces of tartrazine (E102) in food and water samples

Application of carbon nanotubes assisted electromembrane extraction technique followed with capillary electrophoresis for sensitive determination of cocaine in wastewater and biological samples

Application of carbon nanotubes assisted electromembrane extraction technique followed with capillary electrophoresis for sensitive determination of cocaine in wastewater and biological samples

Alkyl polyglucoside-based supramolecular solvent formation in liquid-phase microextraction

The phenomenon of alkyl polyglucoside-based supramolecular solvent formation in the presence of alkyl carboxylic acid acted as coacervation agent was described for the first time. Various alkyl polyglucosides and carboxylic acids were studied as the amphiphiles and coacervation agents, respectively. A possible mechanism of the new supramolecular solvent formation was presented. The physico-chemical properties of the developed alkyl polyglucoside-based supramolecular solvents were investigated. The green liquid-phase microextraction approach with the use of alkyl polyglucoside-based supramolecular solvent was developed and applied to epinephrine (hormone and biomarker for the diagnosis of adrenal glands neoplastic diseases) separation and preconcentration from human urine samples prior to its chromatographic determination. Caprylyl/capryl glucoside was found to be the most effective supramolecular solvent precursor for microextraction of the epinephrine (extraction recovery 95%). The microliter amount of the heptanoic acid was required to induce coacervation process and phase separation. The reduced fluidity of alkyl polyglucoside-based supramolecular solvent under cooling was used to simplify the collection of the extract phase by decantation. The green supramolecular solvent obtained was less viscous then known nonionic surfactant-based solvents and as result more compatible with the high-performance liquid chromatography with fluorometric detection.