Dispersive Liquid-liquid Microextraction Method Research Articles

Phthalates in marine sediment, water and the cockle Anadara antiquata on the coast of Tanzania

Phthalates are a group of chemicals used as plasticisers, and are easily released into the environment, where they degrade over time. We investigated the concentrations of phthalates in sediments, seawater, and the cockle Anadara antiquata from beaches at Dar es Salaam, Mtwara, Tanga and Zanzibar in Tanzania. A dispersive liquid-liquid microextraction method was used to extract analytes from samples, whereafter they were analysed with a gas chromatograph coupled to a mass spectrophotometer. Concentrations of diisobutyl phthalate (DiBP), dibutyl phthalate (DBP) and Bis(2-ethylhexyl) phthalate (DEHP) were determined. DiBP concentrations were highest at Dar es Salaam (11.5 - 12.4 ng/mL in seawater; 11.5 - 13.6 ng/g dry weight in sediments), compared to the other three sites, where minimum and maximum concentrations in sediments were 3.5 ng/g dw (Mtwara) and 10.7 ng/g dw (Tanga). DBP concentrations were also highest at Dar es Salaam (12.4 - 20.6 ng/mL in seawater; 12.1 - 18.7 ng/g dw in sediments) compared to 2.7 (minimum, Mtwara) and 11.2 ng/g dw (maximum, Tanga). DEHP at Dar es Salaam ranged from un-detected to 12.6 ng/mL in seawater and to 12.6 ng/g dw in sediments. It was further revealed that A. antiquata from Kawe Beach (Dar es Salaam) had higher concentrations of DiBP, DBP, and DEHP compared to other sites. Monitoring of phthalate concentrations will indicate pollution hotspots and trends in the region.

A selective dispersive liquid-liquid micro-extraction technique for trace level pollutants enrichment of pharmaceutical residues from hospital wastewaters followed by liquid chromatographic analysis

In this study a dispersive liquid-liquid micro-extraction (DLLME) method was utilized for extraction of trace pharmaceuticals in wastewater samples. Factors influencing the extraction performances were tested and accordingly 900 µL dichloroethane as the extraction solvent, 1400 µL acetonitirle as dispersive solvent, 10 min extraction time at 4000 rpm centrifugation, and pH 5 were found optimum. Acetonitrile and 0.2% formic acid in water were used as eluent. The column temperature was maintained at 25 °C and the optimum detection wavelengths of 273 nm for sulfamethoxazole and 280 nm for ciprofloxacin were used. For both the analytes, the coefficients of determinations (r2) were found to vary from 0.9989 to 0.9997, confirming good linearity in the concentration range of 0.005-100 µg mL-1 for sulfamethoxazole and 0.01-100 µg mL-1 for ciprofloxacin. The LOD and LOQ were in the range of 0.78-1.58 ng mL-1 and 2.24-5.28 ng mL-1, respectively; the RSDs were 0.41-3.21% for intra-day precision and 0.37-6.44% for inter-day precision. The concentrations of the three pharmaceuticals determined ranged from 0.76-1.53 μg mL-1 in the wastewater samples collected from Black Lion Hospital. However, ciprofloxacin and doxycycline were not detected and only low concentration of sulfamethoxazole was detected in the wastewater samples collected from Menelik II Hospital.
 KEY WORDS: Antibiotics, DLLME, Dispersive solvent, Hospital wastewater
 Bull. Chem. Soc. Ethiop. 2024, 38(1), 27-42. DOI: https://dx.doi.org/10.4314/bcse.v38i1.3

Development of an analytical method for the determination of pesticides in tropical fruits by LC-QTOF-MS/MS after QuEChERS extraction sample cleanup and DLLME preconcentration

In this study, QuEChERS extraction was combined with dispersive liquid–liquid microextraction (DLLME) to extract pesticides from tropical fruits for determination by a highly accurate and sensitive liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF-MS/MS) system. The QuEChERS method served as a matrix clean-up tool and the DLLME method preconcentrated the analytes for their determination at trace levels. All parameter variables of the DLLME method were optimized to improve the extraction output and lower the limits of detection and quantification (LOD and LOQ) for all the analytes. Under the optimum experimental conditions, the LOD and LOQ values were found in the range of 0.004–0.013 and 0.27–0.61 μg l−1, respectively. The detection limits achieved by direct LC-QTOF-MS/MS analysis were increased by about 10–260 folds using the optimized DLLME method. To assess the accuracy and applicability of the developed method, spike recovery experiments on tropical fruits were carried out. The matrix matching calibration method was used to enhance the quantification accuracy of the analytes in kiwi, pineapple, and mango matrices, with percent recoveries ranging between 89 and 117%.

Magnetic hydrophobic deep eutectic solvents for orbital shaker-assisted dispersive liquid-liquid microextraction (MAGDES-OS-DLLME) - Determination of nickel and copper in food and water samples by FAAS

In this work, a cheap and widely applicable dispersive liquid-liquid microextraction (DLLME) method was developed for the extraction of Ni(II) and Cu(II) from water and food samples and analysis using flame atomic absorption spectrometry. DLLME was assisted by orbital shaker, while ferrofluid as an extractant was based on deep eutectic solvent (DES). This ferrofluid was made of hydrophobic DES (hDES), composed of lauric acid and menthol (molar ratio 1:2), and toner powder@aliquat 336 magnetic particles. The extraction procedure does not require any heating or centrifugation. The method limits of detection value were 0.15 µg L−1 and 0.03 µg L−1 for Ni(II) and Cu(II) respectively along with wide linearity range (0.4–250 µg L−1). The validation of the method was performed using certified reference materials (CRMs). The studies revealed excellent accuracy between results obtained by the developed method and expected values for all CRMs. The relative recoveries of Ni(II) and Cu(II) ions ranged from 92.8% to 98.6%. The developed method was further used for the determination of Ni(II) and Cu(II) in real water and food samples and provided quantitative recoveries.

Dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry (GC-MS) for the determination of soy sauce aroma compounds

In the present work, a dispersive liquid-liquid microextraction (DLLME) method combined with gas chromatography-mass spectrometry (GC-MS) was successfully developed for accurate determination of aroma-active components in soy sauce. Several key experimental parameters were optimized, including the type of dispersant, vortex time and the volume ratio of extractant and dispersant. The optimal conditions were 1200 μL acetone as dispersant, 800 μL dichloromethane as extractant and 3 min of vortex mixing. The proposed method was validated, achieving good linearities with R2 ≥ 0.9941, recoveries between 82 and 129% with 4-hydroxy-2,5-dimethyl-3(2H)-furanone (HDMF) and 4-hydroxy-2 (or 5)-ethly-5 (or 2)-methyl-3(2H)-furanone (HEMF) within 84–103%, relative standard deviations ranging from 0.02 to 8.60% with HDMF and HEMF between 0.26 and 1.44%, and limits of detection and limits of quantification in the range of 0.08–35.95 μg/L and 0.25–119.83 μg/L, respectively. The entire sample processing with DLLME was completed in roughly 15 min with a total consumption of 2 mL of organic solvent, and 93 volatiles identified in the obtained extracts, with 87.1% (81 volatiles) showing relative standard deviations lower than 10%. Compared to conventional liquid-liquid extraction (LLE), DLLME exhibited obvious advantages of simplicity, rapidity, stability and low solvent consumption, favouring the extraction of acids and ketones. This is the first application of the DLLME technique for the analysis of aroma compounds in soy sauce and is suitable for rapid determination of key aroma compounds like HDMF and HEMF, especially for routine detection and large batch analysis of soy sauce, which can provide reliable information for soy sauce flavour analysis.

Application of chemometric modeling for ionic liquid-based ultrasonic-assisted dispersive liquid-liquid microextraction: Analysis of fosetyl-aluminum in fruit and vegetable samples

This manuscript presents a new method for selective extraction and determination of fosetyl-aluminum in fruits and vegetable samples based on ultrasonic-assisted dispersive liquid-liquid microextraction method using ionic liquids (IL-UA-DLLME). A UV-Visible spectrophotometer was used for detection and quantification. Plants used for sample collection were grown under controlled conditions in a greenhouse. Central composite design (CCD)-response surface methodology (RSM) analysis was used for the optimization of significant factors (volume of IL, pH, ultrasonication time, and THF volume). Under optimal conditions, the limit of detection and limit of quantification of the IL-UA-DLLME procedure were 1.5 ng mL−1 and 5.0 ng mL−1 respectively with relative standard deviation 1.9–3.3%. The developed IL-UA-DLLME procedure demonstrated linearity within the concentration range of 5–600 ng mL−1 with an R2 value of 0.9914. The enrichment factor was 114 with a recovery% of 94.2–98.6% (n = 3) at optimal conditions. The IL-UA-DLLME assay was used for the analysis of fosetyl-aluminum in a variety of food samples and was found highly selective and efficient.

Distance-based thread analytical devices coupled with dispersive liquid-liquid microextraction for melatonin detection

This article reports the first distance-based thread analytical devices (dTADs) coupled with a dispersive liquid-liquid microextraction (DLLME) method for quantitative monitoring of trace melatonin levels in human samples and dietary supplements. Detection is based on colorimetric reaction between melatonin and 2,3-naphthalenedialdehyde (2,3-Nda) carried out on a thread substrate. Herein, melatonin is preconcentrated and extracted to the organic phase of an extraction solvent utilizing the DLLME method. A little droplet of the extraction solvent was then introduced into the dTAD. The yellow-orange colored length is measured, which is proportional to the amount of melatonin level. We obtained a linear range from 15.0 to 45.0 pg mL−1 (R2 = 0.9949) and a detection limit (LOD) of 2.50 pg mL−1, resulting in the clinically relevant ranges for melatonin monitoring in human samples. This technique also exhibited remarkable reproducibility and selectivity. The proposed method is simple, inexpensive, and exhibits more sensitivity than other methods that request expensive reagents and instrumentation. Additionally, this assay constituted an accurate and precise device for concentration quantification in human control samples with recovery percentage ranging from 98.42% to 102.52%. Likewise, there was no significant difference in measured melatonin levels obtained from our method against the nutrition label obtained from melatonin dietary supplements by t-test validation. The combination of an economical dTAD with a simple microextraction method, the proposed device therefore has the advantage of simplicity, instrument-free convenience, and affordability for trace melatonin detection, making it suitable for point-of-care medical diagnostics and food analysis.

A new method based on dispersive liquid-liquid microextraction for fat-soluble vitamin determination in serum by LC-MS/MS.

A green and inexpensive pretreatment known as dispersive liquid-liquid microextraction (DLLME) was developed in this assay coupled with the LC-MS/MS method for routine analysis of fat soluble vitamins (FSVs). The technique was performed with methanol as the dispersive solvent and dichloromethane as the extraction solvent. The extraction phase containing FSVs was evaporated to dryness and reconstituted in a mixture of acetonitrile and water. The influence variables concerning the DLLME procedure were optimized. After that, the method was investigated for its applicability in LC-MS/MS analysis. As a result, the parameters were settled for the optimal conditions during the DLLME process. A cheap and lipid-free substance was found as an alternative to serum to eliminate the matrix effect while preparing the calibrators. The method validation indicated that it was suitable for determining FSVs in serum. Moreover, this method was applied successfully to determine serum samples, which was consistent with the literature. In summary, the DLLME method developed in this report was reliable and more cost-effective than the traditional LC-MS/MS method, and could be applied in the future.

Effervescence-assisted dispersive liquid-liquid microextraction for extraction and preconcentration of organochlorine pesticides in water samples

ABSTRACT. In this paper, effervescence-assisted dispersive liquid-liquid microextraction method has been developed for the extraction and preconcentration of organochlorine pesticides in water samples before their determination by gas chromatography-mass spectrometry. The method involves in-situ generation of CO2 bubbles to induce dispersion of the extraction solvent in the aqueous sample. Different parameters affecting the extraction efficiency of the method including the type and concentration of the effervescent agents as well as the type and volume of extraction solvent were optimized. Under optimum conditions, matrix matched calibration curves were constructed at eight concentrations ranging from 0.6–4.0 ng/mL showed good linearity with coefficient of determinations of ≥ 0.9961. The limits of detections and quantifications ranged from 0.2–0.4 and 0.6–1.0 ng/mL, respectively. The intra- and inter-day precisions studied at two concentration levels had below 5% relative standard deviation values. Similarly, recoveries investigated at two concentration levels ranged from 80.7–117.4%. The findings demonstrated that proposed method is simple, rapid, and efficient to be used as alternative method for analysis of organochlorine pesticides from environmental water and other similar matrices.
 
 KEY WORDS: Effervescence agents, CO2 bubbles, Organochlorine pesticides, Water samples, gas chromatography-mass spectroscopy
 
 Bull. Chem. Soc. Ethiop. 2023, 37(5), 1109-1122. 
 DOI: https://dx.doi.org/10.4314/bcse.v37i5.4

Trace nickel determination in seawater matrix using combination of dispersive liquid-liquid microextraction and triethylamine-assisted Mg(OH)2 method.

In order to eliminate the effects of seawater matrix on the precise/accurate determination of elements, new and efficient analytical procedure requires. In this study, co-precipitation method based on the triethylamine (TEA)-assisted Mg(OH)2 was performed to eliminate side-effects of seawater medium on the determination with flame atomic absorption spectrometry (FAAS) prior to the preconcentration of nickel by an optimized dispersive liquid-liquid microextraction (DLLME) method. Under the optimum conditions of the presented method, the limit of detection and quantification (LOD, LOQ) values obtained for nickel were found as 16.1 and 53.8μgkg-1, respectively. Seawater samples collected from West Antarctic region were used for real sample applications to check the accuracy and applicability of developed method, and satisfying recovery results (86-97%) were obtained. In addition to this, the digital image-based colorimetric detection system and the UV-Vis system were applied to confirm the applicability of the developed DLLME-FAAS method in other analytical systems.

Pesticide residues in herbs and their transfer for infusions.

In this work, a cost-effective gas chromatography-mass spectrometry method was validated for the analysis of twenty-five pesticide residues in herbs and infusions using a quick, easy, cheap, effective, rugged, and safe procedure or a dispersive liquid-liquid microextraction method, respectively. Figures of merit of the method showed good accordance with current guidelines. From the 58 herb samples studied (pertaining to 20 different species), 80% presented at least one detectable pesticide, with 62% of them above the maximum residual level. Results showed that pesticide residues from naturally contaminated herbs were not transferred at a significant rate to the herbal infusions. When a control assay was conducted by spiking a blank herb sample with a large amount of each pesticide (7mg/L) 15 analytes were detected below the limit of quantification in the infusion.

An effective dispersive liquid-liquid microextraction method for pharmaceutical extraction: Optimization via central composite design

An effective dispersive liquid-liquid microextraction method for pharmaceutical extraction: Optimization via central composite design

Dispersion liquid microextraction of fluoroquinolones

The dispersive liquid-liquid microextraction method of norfloxacin, ciprofloxacin and enrofloxacin with chromatographic detection was developed. The optimization of dispersive microextraction was carried out, and the optimal parameters were determined as follows: 5 ml of aqueous solution; 70 l of chloroform; 500 l of isopropanol; extraction time of 5 min; centrifugation time of 5 min; and pH 7.0–9.0. The concentration range was 4.0–100 g/ml, and the limit of detection was not exceeded 1.5 g/ml. The microextraction method was tested on mineral water samples by the standard addition method. The obtained results indicate sufficient accuracy and reproducibility of the developed method. The relative standard deviation does not exceed 2%.

Development of dispersive liquid-liquid microextraction with solid-phase evaporation as a novel hyphenated method prior to ion mobility spectrometry and its application for trace analysis of fluoxetine.

For the hyphenating of dispersive liquid-liquid microextraction (DLLME) with nano mesoporous solid-phase evaporation (SPEV) as a novel method, MCM-41@SiO2 was synthesized and used as a nano mesoporous adsorbent for coating on the solid-phase fiber, preconcentration of fluoxetine antidepressant drug (as a model compound), and total evaporation of the extraction solvents obtained by the DLLME method. To detect the analyte molecules, a corona discharge ionization-ion mobility spectrometer (CD-IMS) was applied. In order to increase the extraction efficiency and the IMS signal of the fluoxetine drug, some variables including extraction solvent and its volume, disperser solvents and its volume, sample solution pH, desorption temperature, and evaporation time of the solvent from the solid-phase fiber were chosen and optimized. Some analytical parameters including limit of detection (LOD), limit of quantification (LOQ), linear dynamic range (LDR) with determination coefficient, and relative standard deviations (RSDs) were calculated under the optimized conditions. LOD (S/N = 3), 3ngmL-1; LOQ (S/N = 10), 10ngmL-1; LDR, 10-200ngmL-1; and intra- and inter-day RSDs (n = 3), 2.5% and 9.6% for 10ngmL-1, and 1.8% and 7.7% for 150ngmL-1, respectively. To investigate the ability of the hyphenated method to determine fluoxetine in real samples, fluoxetine tablets, and some biological samples such as human urine and blood plasma were selected and the relative recovery values were calculated to be 85-110%. The accuracy of the proposed method was compared with that of the HPLC standard method.

Multivariate optimization of dispersive liquid-liquid microextraction using ionic liquid for the analysis of ultraviolet filters in natural waters

In this work, a vortex-assisted dispersive liquid-liquid microextraction method, using an ionic liquid as the extracting solvent was developed, for the simultaneous analysis of three UV filters in different water samples. The extracting and dispersive solvents were selected in a univariate way. Then, the parameters such as the volume of the extracting and dispersive solvents, pH and ionic strength were evaluated using a full experimental design 24, followed by Doehlert matrix. The optimized method consisted of 50 μL of extracting solvent (1-octyl-3-methylimidazolium hexafluorophosphate), 700 μL of dispersive solvent (acetonitrile) and pH of 4.5. When combined with high-performance liquid chromatography, the method limit of detection ranged from 0.3 to 0.6 μg L−1, enrichment factors between 81 and 101%, and the relative standard deviation between 5.8 and 10.0%. The developed method demonstrated effectiveness in concentrating UV filters in both river and seawater samples, being a simple and efficient option for this type of analysis.

Different Extraction Approaches for the Analysis of Melatonin from Cabernet Sauvignon and Feteasca Neagra Wines Using a Validated HPLC-FL Method

In recent years, the wine industry has shown a considerable degree of interest in the occurrence of melatonin in wines. Sample pretreatment may be the most important step in trace analysis. Since wine is a complex matrix and melatonin is present in low amounts (ppb), an adequate extraction technique is required. In this study, the effect of several extraction methods, such as solid phase extraction (SPE), Quick, Easy, Cheap, Effective, Rugged, and Safe extraction (QuEChERS), and dispersive liquid-liquid micro-extraction (DLLME) was studied and the variable parameters that can arise throughout the extraction process were optimized to obtain the best results. A high-performance liquid chromatography with fluorescence detector (HPLC-FL) method was adapted and validated, including measurement uncertainty, for the analysis of melatonin in wines and to assess the efficiency of the extraction yield. After comparing the acquired results, the DLLME method was optimized. Extraction recoveries values ranging from 95 to 104% demonstrated that the approach may be successfully applied for the extraction and concentration (enrichment factor of almost eight) of melatonin in wine samples prior to HPLC-FL analysis. The first report of melatonin levels in Feteasca Neagra wines has been made. The data obtained for Cabernet Sauvignon revealed that the final levels of melatonin in the wines are dependent on the winemaking process.

Development of an efficient dispersive liquid-liquid microextraction approach combined with spectrophotometry for determination of antiviral drug, valacyclovir HCl in pharmaceutical formulations

ABSTRACT. A new, fast, sensitive, simple, and green dispersive liquid–liquid microextraction (DLLME)-based spectrophotometric method for the determination of valacyclovir HCl (VAL) in pure form and pharmaceutical formulations has been developed and validated. The developed method is based on the formation of a coloured product through the reaction of VAL and 1,2-naphthoquine-4-sulfonate (NQS) at pH = 9. The important experimental parameters affecting the extraction efficiency were investigated and optimized. The tiny organic droplets had a wavelength of l = 505 nm. At the optimum conditions, linearity ranged from 0.06 to 2.0 μg/mL, with a linear correlation coefficient of 0.9995. The limits of detection and quantification were 0.02, and 0.06 μg/mL, respectively. The enhancement factor was 36.87. Good recovery as accuracy (99.50%) and relative standard deviation (RSD) as precision were 1.20%, respectively. The developed DLLME method was successfully applied to the determination of VAL in pharmaceutical formulations, and the validity was assessed by applying the standard addition technique. The results obtained by the proposed method for the pure VAL and commercial tablets agreed well with those obtained by the official method.
 
 KEY WORDS: Valacyclovir HCl, Spectrophotometry, 1-2-Naphthoquine-4-sulfonate, Dispersive liquid–liquid microextraction, Pharmaceutical formulations
 
 Bull. Chem. Soc. Ethiop. 2023, 37(3), 579-592. 
 DOI: https://dx.doi.org/10.4314/bcse.v37i3.4

Determination of Ultra-Trace Amounts of Copper in Environmental Water Samples by Dispersive Liquid-Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry

A new method of dispersive liquid-liquid microextraction (DLLME) combined with graphite furnace atomic absorption spectrometry (GFAAS) was proposed for the determination of ultra-trace copper. It was based on the reaction of Cu(II) with the laboratory-prepared chelating agent 2-(5-bromo-2-pyridylazo)-5-dimethylaminoaniline (5-Br-PADMA) in a HAc-NaAc buffer solution at pH 5.0 to form stable hydrophobic chelates, which were separated and enriched by DLLME with chlorobenzene (C6H5Cl) and acetonitrile (CH3CN) as extraction and disperser solvents, respectively. The sedimented phase containing the chelates was then determined with GFAAS. Various operating variables that may be affected by the extraction process such as the pH of the solution, the concentration of the chelating agent 5-Br-PADMA, the types and volumes of extraction and disperser solvents, the extraction time, and the centrifugation time were investigated. Under optimum conditions, the calibration curve was linear in the range from 0.02 ng/mL to 0.16 ng/mL of copper with a correlation coefficient of r = 0.9961, and the detection limit was 0.01 ng/mL based on 3Sb. The relative standard deviation for six replicate measurements of 0.05 ng /mL of copper was 3.9%. An enrichment factor (EF) of 110 was obtained. The method has the advantages of low detection limit, high sensitivity, simple operation, less consumption of organic solvents, higher enrichment factor, and environmental friendliness and was applied to the determination of trace copper in environmental water samples with satisfactory results.

Monitoring the level of urinary metabolites of toluene and xylene in pregnant women in Isfahan and Khansar and their relationship with demographic factors and air quality index

Aim: In this study, the levels of urinary metabolites of toluene and xylene isomers in pregnant women in Isfahan and Khansar cities and their associations with air quality index (AQI) and demographic factors were investigated. Materials and Methods: Depending on the population, 55 pregnant women from Isfahan and 15 pregnant women from Khansar, a total of 70 people were enrolled in the study and 140 urine samples were collected during their 1st and 3rd trimesters of pregnancy (autumn and spring). Urinary metabolites of hippuric acid (HA), ortho-, meta-, and para-methyl HA (o-m-p-MHA) were extracted by dispersive liquid-liquid microextraction method, derivatized and analyzed using gas chromatography/mass spectrometer. The results were statistically correlated with AQI level and demographic factors using appropriate statistical methods. Results: Mean urinary concentrations of HA, o-m-p-MHA in the 1st trimester of pregnancy were 371.2, 1.14, 2.48, and 1.97 mg/g cr, and those in the 3rd trimester were 582.1, 3.54, 6.93, and 2.43 mg/g cr, respectively. In the 1st trimester, the mean urinary level of ortho-MHA was significantly associated with the outdoor exposure time on workdays and fragrances use (P < 0.05). In the 3rd trimester, the mean concentration of HA was significantly correlated to age and outdoor exposure time on workdays (P < 0.05). Conclusion: The mean urinary concentrations of HA and MHA isomers in the 1st trimester of pregnancy in Isfahan were more than those in Khansar. Because the level of air pollution in Isfahan was higher than Khansar and that in autumn was higher than spring. In the 3rd trimester of pregnancy, the mean levels of MHA isomers in Isfahan were more than those in Khansar. Only the amount of p-MHA was significantly associated with AQI in the 1st trimester of pregnancy. Thus, women who lived in high-traffic urban areas with high AQI were more exposed to toluene and xylene compounds.

Multi-magnetic center ionic liquids for dispersive liquid-liquid microextraction coupled with in-situ decomposition based back-extraction for the enrichment of parabens in beverage samples

In this paper, several new multi-magnetic center magnetic ionic liquids (MMILs) were prepared with paramagnetic component simultaneously contained in both the cation and anion and used as extractants to establish a dispersive liquid-liquid microextraction (DLLME) approach followed by in-situ MMIL decomposition based back-extraction for the enrichment and determination of four parabens in beverages. The appropriate MMIL was selected by investigating the extraction performances of the obtained MMILs combined with high performance liquid chromatography-ultraviolet detection (HPLC-UV), and some other experimental factors were explored. Under the optimized DLLME conditions, the four parabens exhibited coefficients of determination (R2) above 0.9987 in the linear range of 0.1-500 ng·mL−1 for ethylparaben, propylparaben and butylparaben and 0.2-500 ng·mL−1 for methylparaben. The limits of detection (LODs) and limits of quantification (LOQs) were respectively within 0.03-0.06 ng·mL−1 and 0.1-0.2 ng·mL−1, and the relative standard deviations (RSDs) for intra-day and inter-day precision were below 10.8%. Moreover, the application of the developed MMIL-based DLLME method in beverage samples exhibited recoveries within 81.3%-112.1% with RSDs of 0.3%-13.1% at three different spiked levels.