Emulsification Microextraction Research Articles

Combination of Ultrasound-Assisted Extraction and Ultrasound-Assisted Emulsification Microextraction for Separation and Enrichment of Permethrin and Deltamethrin Residues in Spinach Samples

Combination of Ultrasound-Assisted Extraction and Ultrasound-Assisted Emulsification Microextraction for Separation and Enrichment of Permethrin and Deltamethrin Residues in Spinach Samples

Development of an Ultrasound-Assisted Emulsification Microextraction Method for the Determination of Volatile Compounds in Wines

A fast and simple method based on ultrasound-assisted emulsification microextraction (USAEME) was developed for the analysis of volatile compounds in wines. A full factorial 24 screening design was built to investigate the main factors affecting the extraction of volatile components, namely the volume of extraction solvent, sonication time, salt content, and pH. Then, the factors with significant effects were optimized using an I-optimal design. The optimal value for all the variables studied was reached under the following experimental conditions: volume of extraction solvent 200 μL and salt content 5% m/v. The suitability of the optimized method was evaluated, resulting in very good linearity with coefficients of determination (R2) higher than 0.995 in all cases, while repeatability was lower than 8.4% except for d-limonene and p-cymene. Recoveries higher than 82% were observed for the groups of ethyl esters, acetate esters, alcohols, and terpenoid alcohols (linalool, α-terpineol). The recovery of acids ranged from 70.5% to 88.9%, whereas the three monoterpenes studied (d-limonene, γ-terpinene, p-cymene) were not extracted satisfactorily. The proposed method was effectively applied for the analysis of volatile compounds in laboratory-scale fermentations with selected strains of Saccharomyces cerevisiae.

Trace-Level Detection of Cr(VI) and Cu(II) in Edible Vegetable Oils Using Dicationic Ionic Liquids and MFe2O4-Based Effervescence-Enhanced Emulsification Microextraction Followed by ICP-MS Analysis

Trace-Level Detection of Cr(VI) and Cu(II) in Edible Vegetable Oils Using Dicationic Ionic Liquids and MFe2O4-Based Effervescence-Enhanced Emulsification Microextraction Followed by ICP-MS Analysis

An effervescence-assisted microextraction for parabens in foodstuffs based on deep eutectic solvent composed of methyltrioctyl ammonium chloride and decanoic acid

An efficient and ecofriendly effervescence-assisted emulsification microextraction approach based on hydrophobic deep eutectic solvent (EA-EME-DES) was developed for the sensitive chromatographic determination of parabens (i.e., methyl-, ethyl-, propyl- and butylparaben) in foodstuffs. The DES extractant consisted of methyltrioctyl ammonium chloride (MTAC) and decanoic acid (DecA) (1:3, mol/mol), and had high hydrophobicity, solubility and stability. During the microextraction procedure, sodium carbonate was introduced to facilitate the dissolution of parabens in aqueous solution, DES dispersion and phase separation by enhancing solution pH and generating CO2 bubbles. The developed method exhibited satisfactory linearity (R2 ≥ 0.9986), detection limits (0.01–0.03 μg/g), quantitation limits (0.04–0.09 μg/g), recoveries (87.8% to 111%, with RSDs of 0.8% to 5%) and negligible matrix effects, hence it had remarkable effectiveness and applicability in determining parabens in complex foodstuffs.

A natural hydrophobic deep eutectic solvent-based microextraction method integrated with a spectrofluorimetric technique for the determination of daclatasvir as a direct-acting hepatitis C antiviral drug in plasma samples

An ultrasound-assisted emulsification microextraction method based on a natural hydrophobic deep eutectic solvent (USAEME-HDES) was developed for extraction and preconcentration of daclatasvir, a hepatitis C virus inhibitor, from plasma samples prior to spectrofluorimetric measurement. To make the deep eutectic solvent (DES) compatible with the fluorescence device, fatty acids were used as components of DES that can simultaneously act as hydrogen bond donors (HBD) and hydrogen bond acceptors (HBA). Various parameters, such as the solvent effect on the fluorescence spectrum and the composition and ratio of DES, were investigated and optimized. Other parameters, including pH, DES volume, sonication time, and NaCl concentration, were investigated and optimized using the central composite design combined with the desirability function. Under optimal conditions, compared to other methods, this method had a wide linear range (5–600 ng/mL) with a good coefficient of determination (0.9985) and a low limit of detection (1.42 ng/mL). Drug analysis results in the plasma samples showed that the method has good accuracy. Finally, the Green Analytical Procedure Index (GAPI) tool was used to evaluate the greenness of the method, which demonstrates our method's superior eco-friendship in comparison to other reported methods.

The comparison of two microextraction methods for the determination of safranal from Iranian saffron

In this study, safranal as the main component of the pleasant aroma of saffron was extracted and analyzed by two liquid-phase microextraction based methods, namely ultrasound-assisted emulsification microextraction and solidified floating organic drop microextraction. These methods are fast, simple, low-cost, environmentally friendly and efficient procedures that have been developed for the determination of safranal from aqueous samples. Extracted safranal was determined by high pressure liquid chromatography and the performance of the above mentioned methods was compared accurately. A narrow neck glass tube was used for the simple and rapid collection of the low-density organic phase from the sample surface after its centrifugation. A dynamic range over 0.1 to 5 μg mL−1 of safranal and limit of detection of 20 ng mL−1 were obtained for ultrasound-assisted emulsification microextraction. In addition, the dynamic range for solidified floating organic drop microextraction was between 0.02 to 5 μg mL−1 as well as a limit of detection of 3 ng mL−1 was obtained. Furthermore, the enrichment factor and recovery percent were 38 and 101±4.6% in ultrasound-assisted emulsification microextraction besides 252 and 25.2 ± 5.8% in solidified floating organic drop microextraction. The applicability of the proposed methods was evaluated by the extraction and determination of safranal from different Iranian saffron samples and finally, the results were validated by the ISO 3632 procedure.

Ultrasound-assisted surfactant-enhanced emulsification microextraction and determination of caffeine and theophylline in human plasma and cocoa powder

Ultrasound-assisted surfactant-enhanced emulsification microextraction and determination of caffeine and theophylline in human plasma and cocoa powder

Ultrasound-assisted Emulsified Microextraction Followed by High Performance Liquid Chromatography for Permethrin

Ultrasound assisted emulsification microextraction (UAEME) as a new sample preparation method was optimized for the determination of permethrin in urine samples. Also, deep eutectic solvent was used as the extracting solvent instead of organic solvents in this method. In order to determine the optimal values, six main parameters were studied in different levels. Totally, 105 runs were performed using the one-variable-at-a-time method followed by high-performance liquid chromatography with a UV detector. Under the optimum conditions, the calibration curve for permethrin was linear in the concentration range of 5 to 500 μgL‑1 for urine samples. The accuracy and reproducibility of the introduced method were determined using the relative recovery (RR%) and relative standard deviation (RSD%) tests on the fortified urine samples. RR% and RSD% were found to be 96.3–101.7 % and 3.2–7.6 %, respectively. The limit of quantification and also the limit of detection were obtained 5 and 1 μg/L, respectively. In the present study, the DES-UA-EME technique was successfully developed for the extraction of permethrin from urine samples and subsequent quantification by high-performance liquid chromatography.In comparison to the other sample preparation methods, the proposed technique has the advantages of shorter extraction time, simplicity, and applicability in laboratories with less equipment

Ethyl salicylate and ethyl benzoate for vortex-assisted surfactant-enhanced emulsification microextraction of fungicides in water samples and analysis by high-performance liquid chromatography

ABSTRACT Ethyl salicylate (EtSA) and ethyl benzoate (EtBZ) as alternative extraction solvents have been evaluated for vortex-assisted surfactant-enhanced emulsification microextraction (VASEME) of target fungicides (e.g. carbendazim, thiabendazole, and fuberidazole) before the high-performance liquid chromatographic analysis. Under optimum conditions, the preconcentration factors about 16–28 (18–33) and limits of detection in the range of 0.01–0.1 µg/L were achieved for both extraction solvents. Good recoveries in the range of 76.2–118.4% (85.7–114.6%) with the acceptable relative standard deviation lower than 10.4 were obtained at the concentration evaluation of 20 µg/L and 50 µg/L each fungicide in different water sample matrices. As a result, the proposed extraction solvents can be used as an alternative to other related solvents like methyl salicylate (MeSA) and methyl benzoate (MeBZ) for the preconcentration of target fungicides.

Simultaneous Determination of Azaperone and Azaperol in Swine Adipose Samples Using Switchable Fatty Acid–Based CO2-Effervescence–Ameliorated Emulsification Microextraction

Simultaneous Determination of Azaperone and Azaperol in Swine Adipose Samples Using Switchable Fatty Acid–Based CO2-Effervescence–Ameliorated Emulsification Microextraction

Simultaneous determination of low molecule benzotriazoles and benzotriazole UV stabilizers in wastewater by ultrasound-assisted emulsification microextraction followed by GC\u2013MS detection

A rapid, sensitive, economically and ecologically friendly method based on one-step ultrasound-assisted emulsification microextraction and in situ derivatization followed by gas chromatography–mass spectrometry for simultaneous determination of low molecular benzotriazoles and benzotriazole-based ultraviolet filters was developed. The optimized method allows quantification of benzotriazole, 4-methylbenzotriazole, 5-methylbenzotriazole; 5-chlorobenzotriazole, 2-(2′-hydroxy-3′-tert-butyl-5′-methylphenyl)-5-chlorobenzortriazole and 2-(2′-hydroxy-5′-(1,1,3,3-tetramethylbutyl)phenyl)benzotriazole in municipal and industrial (dairy) wastewater. The method was validated using real influent and effluent wastewater and samples at various stages of the purification process. Relative recoveries obtained using wastewater as sample matrix were between 77 and 137%, method limits of detection from 0.001 to 0.035 µg/L, method limits of quantification from 0.003 to 0.116 µg/L, the repeatability expressed by the coefficient of variation did not exceed 12%. The use of the method for the determination of tested compounds in municipal and industrial wastewater showed their presence in most of the tested samples, in concentrations from LoD to 6.110 µg/L. The conducted studies of samples from municipal wastewater treatment plant located in north-east Poland showed that the effectiveness of benzotriazole removal by this plant wasfrom 29 to 84%. The load of tested compounds released into the environment by this facility ranges from 2 to 269 mg/day/1000 inhabitants.

Deep eutectic solvent based ultrasound assisted emulsification microextraction for preconcentration and voltammetric determination of aflatoxin B1 in cereal samples.

A new and simple deep eutectic solvent based ultrasound-assisted emulsification microextraction (DES-UAEME) procedure has been developed for preconcentration and voltammetric determination of aflatoxin B1 (AFB1) in cereal products. The method is based on the acetonitrile-based extraction of AFB1 from homogenized cereal samples followed by a DES-UAEME procedure for subsequent differential pulse voltammetry (DPV) determination in a microcell. A DES composed of choline chloride and urea (ChCl-Ur) was used as the extraction solvent and electrolyte for DPV detection. Various parameters affecting the extraction efficiency of AFB1 were evaluated and optimized. Under optimum conditions the calibration graph was linear in the range of 0.2-80.0 μg L-1 (R2 = 0.9966) and the limit of detection (3Sb) was estimated to be 0.05 μg L-1. The intra-day and inter-day precision (RSD%) for determination of 5.0 μg L-1 AFB1 were 3.4% and 3.9%, respectively. The proposed method was also successfully applied for preconcentration and determination of AFB1 in different cereal samples and good relative recoveries were obtained over a range of 94 to 104%.

Ultrasound-Assisted Emulsified Microextraction Based on Deep Eutectic Solvent for Trace Residue Analysis of Metribuzin in Urine Samples

Deep eutectic solvent was used as extraction solvent to develop and optimize a new sample preparation method for the determination of metribuzin in urine samples. In order to determine the optimal values of the effective factors in the deep eutectic solvent-based ultrasound assisted emulsification microextraction method, six effective parameters were selected. The design of experiments was performed using the onevariable- at-a-time method. Totally, 96 experimental runs were performed, and the samples were analyzed using high-performance liquid chromatography with a UV detector. Under the optimum conditions, the calibration curve for metribuzin was linear in the concentration range of 5 to 500 μg L-1 for urine samples. The accuracy and reproducibility of the introduced method were determined using the relative recovery (RR %) and relative standard deviation (RSD %) tests on the fortified urine samples. RR % and RSD % were found to be 96.3 – 101.7 % and 3.2 – 7.6 %, respectively. The limit of quantification and the limit of detection were obtained 5 and 0.8 μg L-1, respectively.

Front Cover: Simultaneous determination of paracetamol and caffeine in aqueous samples by ultrasound‐assisted emulsification microextraction coupled with high‐performance liquid chromatography

Front Cover: Simultaneous determination of paracetamol and caffeine in aqueous samples by ultrasound‐assisted emulsification microextraction coupled with high‐performance liquid chromatography

Simultaneous determination of paracetamol and caffeine in aqueous samples by ultrasound‐assisted emulsification microextraction coupled with high‐performance liquid chromatography

AbstractToday, due to the growth of the pharmaceutical industry and the high consumption of drugs, monitoring of drug residues in environmental samples because of their destructive effects on the environment and humans is essential. In the present work, ultrasound‐assisted emulsification‐microextraction coupled with high‐performance liquid chromatography as a simple and fast method was applied for simultaneous determination of paracetamol and caffeine in the aqueous samples. Effective parameters on the extraction efficiencies of these analytes such as type and volume of extraction solvent, pH of sample solution, salt concentration, sonication, and centrifuging times were studied and optimized. Under the optimum conditions, the calibration graphs were linear in the range of 30.0–1100.0 ng/mL for paracetamol and 50.0–400.0 ng/mL for caffeine. The limits of detection were 9.7 and 15.2 ng/mL for paracetamol and caffeine, respectively. The proposed method was successfully applied for the determination of these drugs in different aqueous samples.

Vortex and Ultrasound-Assisted Surfactant-Enhanced Emulsification Microextraction for the Determination of Pesticide Residues in Honey using Gas Chromatography–Mass Spectrometry

A novel sample pre-treatment technique based on vortex and ultrasound-assisted surfactant-enhanced emulsification microextraction followed by gas chromatographic–mass spectrometric detection has been developed to determine the selected pesticide residues in honey samples. The key parameters which have affected extraction efficiency were investigated and optimized. Under optimal conditions, the extraction recovery was 90–101% and the enrichment factors were 173–191. The concentration ranges of detection and quantification limits were from 0.03 to 0.9 ng/g and from 0.1 to 3 ng/g, respectively, in honey samples. The relative standard deviation was <5% for intra-day (n = 6) and <8% for inter-day precision (n = 4). Target pesticides were observed in 25% of the samples. The results of this study showed that the residues of such pesticides as bifenthrin, fenpyroximate and thiamethoxam were more than the maximum amount in some honey samples, which causes serious harm to human health.

Microextraction and gas chromatography–flame ionization determination of five antiepileptic drugs in biological samples using amino acid-based deep eutectic ionic liquids

This study investigated the use of amino acid-based deep eutectic solvents (AADESs) in the ultrasound assisted reverse-phase emulsification microextraction (UARPEME) of five antiepileptic drugs (AEDs) from biological samples. The extraction was performed by dispersing the AADES into the sample solution using ultrasonic irradiation. After completing extraction, the sample solution was centrifuged. Then, the pre-concentrated AEDs in the AADES (upper phase) were derivatized by adding phenyltrimethylammonium hydroxide solution to it. The derivatized analytes were then eluted with n-hexane and it was injected directly into the gas chromatography–flame ionization detection (GC–FID) system to determine target analytes after the methylation reaction inside the injection chamber. The effective parameters of the proposed AADES–UARPEME method that comprises three consecutive extraction, derivatization and elution steps, were optimized using one Taguchi orthogonal array design and two central composite designs and evaluated by analysis of variance. The optimized method was successfully implemented to analyze AEDs in the human biological samples (serum, urine, breast-milk and hair) and acceptable results were obtained. The resultant calibration curves were linear over the concentration range of 0.5–850 μg/L (R2 > 0.998). The estimated limits of detection and quantification were lower than 0.5 μg/L and the improvement factors were between 1378 and 1409. The intra- and inter-day repeatability values varied below 5.3% (n = 5) and the relative recovery values were calculated between 90 and 110% for all samples.

Deep eutectic solvent-based ultrasound-assisted emulsification microextraction for the rapid determination of benzotriazole and benzothiazole derivatives in surface water samples

This work describes a simple and environmental-friendly method for the simultaneous determination of five benzotriazole derivatives (BTRs) and four benzothiazole derivatives (BTs) that are frequently found in surface water. The target analytes were efficiently extracted from water samples using a “green” deep eutectic solvent (DES) as the extraction solvent based- ultrasound-assisted emulsification microextraction (DES-USAEME), and their determination were performed by ultrahigh-performance liquid chromatography and electrospray ionization (+)-quadrupole time-of-flight mass spectrometry (UHPLC-ESI(+)-QToF-MS). The DES was composed of a mixture of choline chloride and phenol (molar ratio 1:2). The DES-USAEME factors were optimized by a Box-Behnken Design coupled response surface methodology. The developed method was validated, providing limits of quantitation (LOQs; 02 μg L−1), high precisions (1–8%), and satisfactory mean spiked recoveries (72–104 %). Relatively high total concentrations of the target analytes were found in samples collected from a reservoir (47.2–101.3 μg L−1), which may have been released from tire-wear particles and scrap tires from buses and old tires that were strung alongside the shuttle boats to prevent the boats from coming into contact with each other or from impacting against the dock during docking. This is the first study on the occurrence of BTRs and BTs in reservoir samples.

Simple Emulsification Microextraction for the Preconcentration of Palladium in Water Samples by Flame Atomic Absorption Spectrometry

A simple and selective emulsification microextraction (EME) method in conjunction with flame atomic absorption spectrometry (FAAS) is reported for the preconcentration of palladium ions in aqueous solution. In this approach, N-(3-chloro-4-fluorophenyl)-N-phenylthiourea (CFPT) was synthesized for the first time for the complexation of metal ions including manganese, nickel, cadmium, cobalt, copper, gold, lead, palladium, iron, zinc, aluminum, and chromium and platinum with the microextraction method. The new CFPT ligand provided excellent selectivity toward Pd2+ ions in highly acidic conditions. The formation of a palladium hydrophobic compound with the new synthesized ligand was extracted into chloroform by shaking a model solution for a few seconds. The cloudy solution was centrifuged and the organic phase containing Pd2+ was diluted with nitric acid and transferred for the monitoring of the palladium absorbance by FAAS. Under the optimum conditions, the linearity (R 2 = 0.9986) was in the range from 10 to 1000 µg L−1 and the limit of detection was 2.28 µg L−1 for Pd2+. The developed EME-FAAS method was successfully applied for preconcentration and determination of Pd2+ in spiked samples such as well, stream, tap and sea water with good recoveries.

Erratum to: Modified Vortex-Assisted Surfactant-Enhanced Emulsification Microextraction Using Methyl Benzoate for the Preconcentration of Fungicides in Fruit Juice Samples and Analysis by High-Performance Liquid Chromatography

Erratum to: Modified Vortex-Assisted Surfactant-Enhanced Emulsification Microextraction Using Methyl Benzoate for the Preconcentration of Fungicides in Fruit Juice Samples and Analysis by High-Performance Liquid Chromatography