Microwave-assisted Micellar Extraction Research Articles

Simultaneous capture of hydrophilic and hydrophobic compounds from complex plants by biosurfactant-assisted mechanical amorphous dispersion extraction

A biosurfactant-assisted mechanical amorphous dispersion extraction (BA-MADE) procedure was established for the simultaneous capture of hydrophilic phenolic acids and hydrophobic tanshinones from Salvia miltiorrhiza. Single-factor experiments and the response surface methodology were used to optimize and analyze the crucial parameters for the method, such as the type and amount of amorphous-dispersion extractants, grinding time, extraction time and solid-to-liquid ratio. The optimized parameter values for the BA-MADE process were 407.02 mg of sodium chenodeoxycholate, a grinding time of 4.87 min, an extraction time of 4.92 min, and a solid-to-liquid ratio of 0.5:10 g/mL. The calibration curves of danshensu, rosmarinic acid, lithospermic acid, salvianolic acid B, salvianolic acid A, dihydrotanshinone I, cryptotanshinone, tanshinone I, and tanshinone II A exhibited good linearity in the range of 1–500 μg/mL (R2 ≥ 0.9990). The limits of detection of nine analytes ranged from 5.46 to 130 ng/mL, the relative standard deviations (RSDs) of intraday and interday precision were less than 1.95 and 3.56%, respectively, and the recoveries of the real sample were in the range of 85–113%, with RSD% below 3.21%. The BA-MADE method was compared with previously reported methods, such as heating reflux extraction, ultrasonic extraction and microwave-assisted micellar extraction, and the results demonstrated that the developed method has significant advantages in the simultaneous extraction of hydrophilic and hydrophobic active components from Salvia miltiorrhiza.

Ultrasonic microwave-assisted micellar extraction and purification of flavonoids from licorice by metal complex and antisolvent recrystallization

This study aims to extract and purify flavonoids from licorice by an efficient and environmentally friendly approach. The ultrasonic microwave-assisted micellar extraction (UMAME) method was used to extract licorice flavonoids (LFs). The optimal extraction parameters including lauryl sodium sulfate concentration, microwave power, solvent-material ratio and extraction time were investigated by a single factor method and response surface methodology. The extraction rate of LFs was up to 3.65% under the optimal conditions. The extraction solution was pretreated with ethyl acetate and the purity of raw LFs reached 36.47%. The purity of raw LFs was increased from 36.47% to 90.32% by metal complex method and antisolvent recrystallization method. The antioxidant test results showed that the finally purified LFs with an IC50 value of 3.519 μg/mL had a strong scavenging ability on DPPH free radical.

PREPARATION, CHARACTERIZATION, AND FORMULATION OF SOLID LIPID NANOPARTICLES LOTION FROM MULBERRY ROOTS (MORUS ALBA L.)

Objective: Tween 80 has been used as a solvent for the extraction of phenolic compounds because this surfactant has both hydrophilic and hydrophobicproperties. Solid lipid nanoparticles (SLNs) have been developed to improve penetration through the skin layer. We investigated the efficacy of usingthe microwave-assisted micellar extraction (MAME) approach for extracting oxyresveratrol from Morus alba roots and also to develop an SLN lotion.Methods: The M. alba roots were extracted with Tween 80 in a microwave for 18 min, and the extract was used to develop SLN with differentconcentrations of glyceryl monostearate. The SLNs from M. alba root extracts were prepared by a high-speed homogenization technique (25,000 rpmfor 15 min). The SLNs produced were characterized as per particle size, polydispersity index (PDI), and zeta potential. The SLNs with the bestcharacteristics were used to formulate a lotion using a high-pressure homogenizer.Results: Extraction using MAME showed improved extraction efficiency. The oxyresveratrol concentration from the extract was 2.77%. The SLN with2.5% glyceryl monostearate showed the optimum result, with a particle size of 130.20 nm, a PDI of 0.278, and a zeta potential of −21.8 mV. The SLNlotion exhibited a particle size of 285.9 nm and a PDI of 0.360. The SLN lotion also had good penetration, with a flux of 4.70 μg cm−2/h.Conclusion: MAME is an efficient method for extracting oxyresveratrol from M. alba roots. The SLN with 2.5% glyceryl monostearate exhibited theoptimum characteristics, and the SLN lotion showed good characteristics, including skin penetration.

Rapid ultrasonic and microwave-assisted micellar extraction of zingiberone, shogaol and gingerols from gingers using biosurfactants

Two kinds of extraction methods ultrasonic-assisted micellar extraction (UAME) and microwave-assisted micellar extraction (MAME) coupled with ultra-high performance liquid chromatography with ultraviolet detector (UHPLC-UV) were developed and evaluated for extraction and determination of zingerone, 6-gingerol, 8-gingerol, 6-shogaol and 10-gingerol in Rhizoma Zingiberis and Rhizoma Zingiberis Preparata. A biosurfactant, hyodeoxycholic acid sodium salt, was used in micellar extraction. Several experimental parameters were studied separately by a univariate method. The result indicated that the MAME was more efficient than UAME. The optimal conditions of MAME were as follows: 100mM of hyodeoxycholic acid sodium salt was used as surfactant, the irradiation time was set at 10s and the extraction temperature was set at 60°C. The validation results indicated that the limits of detection were in the range of 3.80-8.11ng/mL. The average recoveries were in the range of 87.32-103.12% for the two samples at two spiking levels. Compared with other reported methods, the proposed MAME-UHPLC-UV method was more effective, quicker (10s) and more eco-friendly.

Analysis of sulfonamides in soil, sediment, and sludge based on dynamic microwave-assisted micellar extraction.

A green and high-throughput analytical method was described for the simultaneous determination of ten sulfonamides (SAs) from soil, sediment, and sludge in northeast China. None of potentially hazardous organic solvents was used in the whole sample preparation procedure, and the total preparation time of 15 samples was about 18min. The limits of detection for the SAs were in the range of 0.42-0.68ngg(-1). The intra-day and inter-day precisions, expressed by the relative standard deviation, were below 7%. Under the optimum conditions, the recoveries of ten SAs were between 69.7 and 102.7%. The proposed method was successfully applied to analyze the SAs residues in agricultural soils, river sediments, and sewage sludge. SAs were found at the levels of 1.40-2.31ngg(-1) and 3.77-29.29ngg(-1) in the sediments and sludge, respectively. The aging effect of spiked soil samples on the SAs recoveries was examined, and the results demonstrate that eight SAs could persist in five soils for 3months. Compared with the traditional method, the proposed method could reduce the consumption of the organic solvent, shorten the sample preparation time, and increase the sample throughput.

Determination of Ni, Cr, Cu, Pb and Cd on the Mediterranean endemic plant Posidonia oceanica using the green extraction method “Microwave Assisted Micellar Extraction” and GFAAS

An effort is currently being made to reduce the acid concentrations in traditional methodologies for the analysis of metals based on green chemistry. However, it becomes necessary to develop alternative extraction and analytical environmentally friendly methods that completely avoid the use of acids. In this sense, a Microwave Assisted Micellar Extraction (MAME) method was developed, which employs biodegradable surfactants as extractants. On the other hand, Posidonia oceanica has demonstrated its potential as a bioindicator for metal pollution in the marine environment. Therefore, a new green method has been tested for the extraction of heavy metals (Ni, Cr, Cu, Pb, Cd) from Posidonia oceanica, by using a mixture of biodegradable surfactants: Sodium Dodecyl Sulphate (SDS) and Triton X-100 as extractants and analysis by Graphite Furnace Atomic Absorption Spectrometry (GFAAS). The proposed method showed, in general, satisfactory recovery percentages, RSD below 7.29%, and LOD ranging from 0.04 to 0.22 μg g−1. On the other hand, the proposed method was applied to aged Posidonia oceanica as well as different macrophyte samples. The results obtained were compared to those from ISO 11047:1998.

Combination of microwave‐assisted micellar extraction with liquid chromatography tandem mass spectrometry for the determination of fluoroquinolone antibiotics in coastal marine sediments and sewage sludges samples

In this work, a method for the analysis of fluoroquinolone antibiotics using microwave-assisted micellar extraction combined with liquid chromatography-mass spectrometry detection has been developed. Different surfactants were tested for use as extractants in the isolation of the analytes from solid samples, and several experimental designs were evaluated for the determination and optimization of the variables that affect recovery from the matrix. Under optimal conditions, we obtained recoveries greater than 73% with relative standard deviations below 8%. Compounds were detected by liquid chromatography-electrospray ionization tandem mass spectrometry with detection limits between 0.15 and 0.55 ng g(-1) and quantification limits between 0.49 and 1.85 ng g(-1) . Finally, the optimized method was applied in the determination of antibiotics in real solid samples. Four fluoroquinolones (levofloxacin, norfloxacin, ciprofloxacin and enrofloxacin) were found in coastal marine sediments taken close to a marine outfall and in sewage sludge samples from a wastewater treatment plant. Concentrations ranged between 0.81 and 34.3 ng g(-1) in the sediments and 3.43 and 206.1 ng g(-1) in the sludge.

Combination of Microwave Assisted Micellar Extraction and Liquid Chromatography for Determination of Cryptotanshinone, Tanshinone I, and Tanshinone IIA in Salvia Miltiorrhiza Bunge

A new method based on the microwave assisted micellar extraction technique (MAME) has been optimized for the extraction of tanshinones from the traditional Chinese medicine-Salvia miltiorrhiza Bunge. Non-ionic surfactant Genapol X-080 solution was employed as extractant. Under optimum conditions, i.e., 10% Genapol X-080 (w/v), liquid/solid ratio 80:1 (mL · g−1), microwave assisted extraction time 7 min (4 min + 3 min), microwave power 260 W, particle size of Salvia miltiorrhiza Bunge <105 µm, the extraction efficiency of tanshinones reached the highest value. Compared with static extraction and ultrasonic assisted extraction techniques, MAME has the highest extraction yield of tanshinones and shortest extraction time. Furthermore, MAME has similar extraction efficiency with the heating reflux method recommended by Chinese Pharmacopoeia.

Microwave‐assisted micellar extraction coupled with solid‐phase extraction for preconcentration of pharmaceuticals in molluscs prior to determination by HPLC

A simple and specific analytical method was developed and tested for the determination of pharmaceuticals in mollusc samples. A combination of microwave-assisted micellar extraction (MAME) and solid-phase extraction (SPE) using a non-ionic surfactant, polyoxyethylene 10 lauryl ether, was examined to extract and determine simultaneously a group of pharmaceuticals such as carbamazepine, clorfibric acid, ketoprofen, naproxen, bezafibrate and ibuprofen by liquid chromatography using UV-diode array detector. The MAME extraction performance was evaluated by studying various parameters such as the volume and concentration of surfactant and microwave conditions. Finally, an OASIS HLB cartridge was used as an optimum SPE sorbent to clean up the extracts and preconcentrate the selected analytes. The proposed method showed satisfactory linearity and reproducibility (between 3 and 15%), as well as detection limits ranging from 30 to 220 ng/g. Finally, the method was successfully applied to the determination of the target pharmaceuticals in various kinds of mollusc samples. This study has demonstrated that microwave-assisted micellar extraction with solid-phase extraction may be used as a viable alternative to conventional methods for the extraction of pharmaceuticals in this type of matrices.

Application of microwave-assisted micellar extraction combined with solid-phase microextraction and high-performance liquid chromatography with UV detection for the determination of organochlorine pesticides in different mud samples

An analytical method combining microwave assisted micellar extraction (MAME) followed by solid-phase microextraction (SPME) and high-performance liquid chromatography–ultraviolet high-performance liquid chromatography with UV detection–detection is implemented for the determination of six organochlorine pesticides in different mud samples collected on Gran Canaria Island (Spain). This method allows detection limits to be reduced with respect to MAME extraction and also enables target organochlorine pesticides to be determined in complex matrices due to the clean-up procedure. Several new variables that affect the MAME–SPME process were introduced and optimized. A non-ionic surfactant, polyoxyethylene 10 lauryl ether, and a 60 µm polydimethylsiloxane-divinylbenzene fibre were used for this approach. After systematic investigations, the optimum experimental parameters were fixed. The optimized method provided satisfactory precision (relative standard deviation less than 10%), good recoveries (79.78–117.70%) and detection limits ranging between 28 and 136 ng g−1 for the pesticides studied. The proposed method was successfully applied to the determination of target organochlorine pesticides in several kinds of mud samples of different physico-chemical characteristics and areas. The MAME–SPME method was also validated and applied to a certified reference material.

Analysis of Organochlorine Pesticides in Mollusc Samples by HPLC after Microwave Assisted Micellar Extraction Coupled with Solid Phase Extraction

A mixture of six organochlorine pesticides were determined by HPLC in different types of molluscs after their extraction by microwave assisted micellar extraction (MAME) coupled with a clean‐up and preconcentration step by solid phase extraction (SPE). A non‐ionic surfactant (Polyoxyethylene 10 lauryl ether, POLE) was used in MAME followed by SPE for cleaning and preconcentration of the samples. The extracts were determined by HPLC‐UV. With the optimum experimental variables established, the analytical parameters of the method were determined with satisfactory results (relative standard desviation values between 3.9 and 9.3% and detection limits between 6 and 38 ng · g−1). The method was validated using the conventional Soxhlet extraction method.

Preconcentration of pharmaceuticals residues in sediment samples using microwave assisted micellar extraction coupled with solid phase extraction and their determination by HPLC–UV

An analytical method combining microwave assisted micellar extraction (MAME) and solid phase extraction (SPE) has been developed to extract and preconcentrate a selected group of eight pharmaceutical compounds in sediment samples prior to their determination using liquid chromatography with an UV–DAD detector. A non-ionic surfactant, Polyoxyethylene 10 lauryl ether (POLE) was used for the MAME extraction and the different parameters for the optimization process were studied. Then, SPE was used to clean-up and preconcentrate the target analytes in the extract, prior to their determination using HPLC–UV. The method was applied to the determination of the selected pharmaceuticals compounds in several kinds of sediment samples with different characteristics. Relative recoveries for spiked sediment samples were over 70% and relative standard deviations (RSDs) were under 11% for all recoveries tested. Detection limits between 4 and 167 ng g −1 were obtained. The method was validated using Soxhlet extraction procedure.

Microwave-assisted Micellar Extraction and Determination of Glycyrrhizic Acid and Liquiritin in Licorice Root by HPLC

Abstract The feasibility of employing non-ionic surfactant (Triton X-100) as an alternative and effective solvent for the microwave-assisted extraction of glycyrrhizic acid (GA) and liquiritin (LQ) from licorice root was studied. The optimal extraction parameters based on the microwave-assisted micellar extraction technique were determined. Under the optimal conditions, i.e. 5% (by volume) Triton X-100, microwave-assisted extraction for 3—5min at 373K, the percentage extraction of active ingredients reached the highest value. The preconcentration factor for GA and LQ (about 13.5) and the extraction efficiency for these two ingredients approached 100% showed the coupling of microwave-assisted extraction and cloud-point extraction could be employed as a new and effective technique for the rapid extraction and preconcentration of pharmacologically active ingredients from medicinal plants such as licorice root without disturbing chromatographic analysis.

SPME and SPE comparative study for coupling with microwave-assisted micellar extraction in the analysis of organochlorine pesticides residues in seaweed samples

Solid-phase microextraction (SPME) and solid-phase extraction (SPE) procedures were coupling with microwave-assisted micellar extraction for organochlorine pesticides residues determination in seaweed samples. They were optimized, compared and discussed. Preliminary experiments were performed in order to study experimental conditions for the extraction of pesticides from spiked seaweed samples with microwave-assisted micellar extraction (MAME) using a non-ionic surfactant (Polyoxyethylene 10 Lauryl Ether). After that, SPME and SPE were used to clean-up and preconcentrate MAME extract prior the analysis by liquid chromatography with photodiode array (PDA) detection. Excellent results were obtained for both procedures. Average pesticide recoveries between 80.5 and 104.3% for MAME-SPME and between 73.9 and 111.5% for MAME-SPE were obtained. Relative standard deviations (RSDs) were lower than 10.3% and 5.3% respectively for all recoveries tested, and LOD between 138–348 ng g − 1 for MAME-SPME and 2–38 ng g − 1 for MAME-SPE were obtained. The method was validated using Soxhlet extraction procedure. Both methods were applied to analyse target organochlorine pesticides in several seaweed samples and results were compared. These results show the great possibilities of combining MAME-SPE-HPLC-UV for the analysis of seaweed samples, improving the selectivity and sensitivity in the determination of organochlorine pesticides analysis for this kind of samples.

Focused microwave-assisted micellar extraction combined with solid-phase microextraction—gas chromatography/mass spectrometry to determine chlorophenols in wood samples

This work describes the utilization of the focused microwave-assisted micellar extraction in combination with the solid-phase microextraction (SPME) to determine chlorophenols in wood samples. The influence of the nature of the surfactant in the extraction process, the optimization of the variables of the focused-microwave system, and the effect of the ageing time of the samples in the extraction efficiency of the method, have been assessed in this study. The overall method using the non-ionic surfactant POLE as extracting medium allows us to determine chlorophenols in wood samples achieving an average extraction efficiency of 104.1%, limits of detection ranging from 2 to 120 ng g −1, and intermediate precision values ranging between 3.5 and 13.2%. The proposed method is also characterized by short analysis times (around 5 min for the microwaves extraction step) and by avoiding the use of organic solvents.

Sample Extraction Method Combining Micellar Extraction−SPME and HPLC for the Determination of Organochlorine Pesticides in Agricultural Soils

A method for the determination of organochlorine pesticides in soil samples combining microwave assisted micellar extraction (MAME) with solid-phase microextraction (SPME) and high-performance liquid chromatography-UV has been developed. A mixture of two nonionic surfactants (polyoxyethylene 10 lauryl ether and polyoxyethylene 10 stearyl ether) was used for the extraction of pesticides from agricultural soils, and different types of SPME fibers were compared. The different parameters which affect extraction efficiency in the SPME procedure were optimized such as extraction time and temperature. The method developed involves extraction and preconcentration for the target analytes in soil samples. The analytical parameters were also studied and good recoveries obtained, RSD being lower than 10% and detection limits ranging between 36 and 164 ng g(-1) for the pesticides studied. The proposed method was successfully applied to the determination of some organochlorine pesticides in several kinds of agricultural soil samples with different characteristics.

Determination of Benzimidazole Fungicides in Soil Samples Using Microwave-Assisted Micellar Extraction and Liquid Chromatography with Fluorescence Detection

A simple and fast analytical method was developed for the determination of benzimidazole fungicides (benomyl, carbendazim, thiabendazole, and fuberidazole) in soil samples. The analytes were extracted from the soil samples by means of conventional microwave-assisted extraction, using the non-ionic surfactants polyoxyethylene 10 lauryl ether (POLE) and oligoethylene glycol monooalkyl ether (Genapol X-080) as extractants. Determinations were made by using liquid chromatography with direct fluorescence detection. The use of an analytical column Symmetry C-18 offered short retention times of analytes without the need of any pH regulators with mobile phase methanol-water (50 + 50, v/v). The best results were obtained using 5% (v/v) POLE as extractant with recoveries of the fungicides in spiked soil samples between 71 and 105%. The results were compared with those obtained when Soxhlet extraction was applied to the same soil samples.

Microwave assisted micellar extraction coupled with solid phase microextraction for the determination of organochlorine pesticides in soil samples

Microwave assisted micellar extraction (MAME) coupled with solid phase microextraction (SPME) and HPLC-UV determination have been used for the determination of five organochlorine pesticides from agricultural soil samples. A non-ionic surfactant, Polyoxyethlylene 10 Lauryl Ether was used, and the different variables for the optimization of MAME and SPME procedures were studied. This method was applied successfully to the determination of these pesticides in several kinds of agricultural soil samples with different characteristics. Most of the compounds studied can be recovered in good yields with R.S.D. lower than 9% and detection limit ranged between 56–96 ng g −1 for the pesticides studied.

An Approach to the Application of Microwave-Assisted Micellar Extraction and Liquid Chromatography with Ultraviolet Detection to the Extraction and Determination of Organophosphorus Pesticides in Tomato Samples

Microwave-assisted micellar extraction methodology was applied to extract a mixture of 8 organophosphorus pesticides from the cuticle of tomato samples prior to analysis by liquid chromatography with ultraviolet detection. This technique provided very good results and was simple, fast, and environmentally friendly. The pesticides under study were extracted using the nonionic surfactants polyoxyethylene 10 lauryl ether (POLE) and oligoethylene glycol monoalkyl ether (Genapol X-080). The optimal extraction variables to be applied were determined for each surfactant and then compared. POLE proved to be the most suitable for the extraction, with recoveries over 70% in the majority and relative standard deviation values under 4.8%. After validation using a tomato sample enriched with a certified mixture, the proposed method was applied to the analysis of organophosphorus pesticides in lettuce and pepper samples.

A New and Fast Extraction Method for the Determination of Priority Phenols from Marine Sediments by Liquid Chromatography

A new and fast method for the determination of priority phenols in marine sediment samples by high-performance liquid chromatography using microwave-assisted micellar extraction is optimized. This study is carried out using the nonionic surfactants polyoxyethylene 9 lauryl ether (polidocanol) and genapol X-080 as extractants. Parameters studied include surfactant concentration, solution pH, extraction time, and power. Once the method is optimized, it is applied to different spiked marine sediments from of the Canary Islands coastlines (Spain). The results obtained indicate that a power irradiation of 500 W for 2 min achieved the best extraction efficiency (approximately 100% recovery) and less than 10% relative standard deviation. Detection limits are obtained in the 2-20 microg/g range for the phenols studied. Finally, the proposed method provides a simple, fast, and organic solvent-free procedure to analyze phenols from marine sediment samples.