Mixed Hemimicelles Solid-phase Extraction Research Articles

Magnetic solid phase extraction of Sunitinib malate in urine samples assisted with mixed hemimicelle and spectrophotometric detection

The mixed hemimicelle-based solid phase extraction method using the coated sodium dodecyl sulfate by magnetic iron oxide nanoparticles as adsorbent was developed for extraction and determination of Sunitinib malate in real samples prior to determination by UV–Visible spectrophotometry. For the characterization of synthesized nanoparticles, Fourier transform infrared spectroscopy, and scanning electron microscopy was used. The influences of different factors affecting the extraction efficiency of Sunitinib malate, including the pH, the adsorbent amount, the volume and eluent type, the amount of the surfactant, the ionic strength, extraction, and desorption time, were investigated. At the optimized conditions, a good linearity with correlation coefficients of 0.998 and 0.999 was obtained over the concentration ranges of 1–22 and 1–19 µg/mL for water and urine samples, in order. The good recoveries of 97% and 99% and also, the limits of detection equal with 0.9, and 0.8 µg/mL for water and urine samples were enhanced, respectively. These results demonstrate that mixed hemimicelle solid phase extraction is a fast, efficient, economical and selective sample preparation method for the extraction and determination of Sunitinib malate in different water and urine sample solutions.

Mixed Hemimicelles Solid phase Extraction of Atrazine and Simazine from Environmental Water Samples Using Alumina-Coated Magnetite Composite Material

Mixed Hemimicelles Solid phase Extraction of Atrazine and Simazine from Environmental Water Samples Using Alumina-Coated Magnetite Composite Material

Magnetic nano-carbon core shell as potent mixed hemimicelle solid phase extraction strategy for determination of acrylamide from potato chips coupled by high-performance liquid chromatography

Magnetic nano-carbon core shell was applied as mixed hemimicelle magnetic solid phase extraction adsorbent to introduce a novel sample preparation method for determination of acrylamide from potato chips. Acrylamide is identified as neurotoxic, a probable human carcinogen (group 2A) compound. Effective extraction parameters such as type and amount of extracting solvent, type and amount of adsorbent, time of extraction and desorption, the effect of pH, time of ionic liquid loading on the adsorbent and stirring rate (rpm) were studied and optimized. Under optimized extraction conditions, a good linearity was observed in the concentration range of 100–1500 ng/g. Limit of detection was observed as 30 ng/g. Application of the proposed method was surveyed by analysis of some potato chips brands available in the local supermarkets. The satisfactory results with the recovery of 95.58% revealed that the proposed method could be applied in food analysis laboratories.

Mixed hemimicelles solid phase extraction based on sodium dodecyl sulphate-coated nano-magnets Fe3O4 for the simultaneous separation and preconcentration of cobalt and nickel

A simple nano-sized magnetic particles solid phase extraction (MSPE) was developed for simultaneous extraction and preconcentration of cobalt and nickel in water and food samples prior to their determination by flame atomic absorption spectrometry. This method was based on the reaction of trace amounts of cobalt and nickel from aqueous solutions with 2-nitroso-1-naphthol and adsorption of formed complexes on sodium dodecyl sulphate-coated Fe3O4 nanoparticles (NPs). The crucial factors affecting the efficiency of the developed method such as pH and amount of surfactant were optimized. The detection limits of the developed method were 0.09 and 0.40 μg L−1 (300.0 mL of samples), for Ni(II) and Co(II), respectively. The relative standard deviations were 2.3 and 2.4% for six replicate measurements of Ni (10.0 μg L−1) and Co (5.0 μg L−1). The method was successfully applied for the determination of cobalt and nickel in spinach, tea and water samples.

Novel mixed hemimicelles based on nonionic surfactant-imidazolium ionic liquid and magnetic halloysite nanotubes as efficient approach for analytical determination.

The co-adsorption of mixed nonionic surfactant and imidazolium-based ionic liquid, Triton X100 (TX100), with 1-cetyl-3-methylimidazolium bromide (C16mimBr) adsorbed onto the surface of magnetic halloysite nanotubes (MHNTs) was used as an efficient adsorbent for simultaneous determination of amlodipine and nimodipine in urine. The designed adsorbent was characterized by TEM, TGA, FTIR, and DLS analysis methods. All the parameters that influence the extraction efficiency are optimized with the aid of response surface methodology (RSM). The effects of nonionic surfactant TX100 with different structures of ionic-liquid-coated MHNTs were investigated. Under optimum conditions, extraction recoveries of amlodipine and nimodipine were in the range of 73.8-81.2 and 94.3-96.1%, with RSDs (n = 3) of 2.6-5.5% in spiked urine samples, respectively. The adsorption mechanism principal of mixed hemimicelles was discussed in this study. The limit of detection obtained for analytes was < 0.002μg·mL-1. To our knowledge, this was the first attempt using a mixed hemimicelle solid-phase extraction (SPE) based on MHNTs and nonionic surfactant and imidazolium-based ionic liquid for the simultaneous determination of amlodipine and nimodipine in biological samples. Graphical abstract ᅟ.

Mixed hemimicelle solid-phase extraction based on magnetic halloysite nanotubes and ionic liquids for the determination and extraction of azo dyes in environmental water samples

An effective and greener mixed hemimicelles magnetic solid phase extraction (MHMSPE) based on magnetic halloysite nanotubes (MHNTs) and ionic liquid (IL) is developed for the simultaneous enrichment and determination of anionic azo dyes in a spiked environmental water sample. In this MHMSPE, the formation of C16mimBr with mixed hemimicelles on the surface of MHNTs leads to the retention of analytes by strong hydrophobic, p-p and electrostatic interactions. This MHMSPE technique combines the advantages of MHNTs and mixed hemimicelles. Zeta potential data demonstrated that mixed hemimicelles were formed in [C16mimBr]/[MHNTs] ratios of the range from 0.15 to 1.33. Different important factors affecting the preconcentration of analytes were investigated and optimized by response surface methodology and one variable at a time. Under the optimum conditions, the limits of detection (LOD) for methyl red and methyl orange (MR and MO) were 0.042 and 0.050 μg L−1 in samples, respectively. The accuracy of the method was assessed by recovery measurements on a spiked sample, and good recoveries 85–87% for MR and 89–93% for MO, with preconcentration factors of 481 and 524, respectively. The low relative standard deviations from 1.6–3.1% for tap water and 2.5–5.4% for lake water was achieved. So far as we know, this is the first development of a mixed hemimicelles SPE based on MHNTs and IL for the extraction of trace anionic azo dyes in environment water samples.

Magnetic mixed hemimicelle solid-phase extraction based on mixed hemi-/ad-micelle SDS-coated magnetic nanoparticles Fe2-xAlxO3 (x = 0.4) for the fluorimetric determination of carvedilol in biological samples

Mixed hemi-/ad-micelle SDS-coated magnetic nanoparticles (Fe2-xAlxO3 (x = 0.4)) were used as an efficient adsorbent for the extraction and preconcentration of carvedilol (CVD) based on magnetic mixed hemimicelle solid-phase extraction. The Fe2-xAlxO3 magnetic nanoparticles not only have better stability and resistance to acidity, as well as alkalinity, but also are easy to prepare, inexpensive, and environmentally friendly. Several parameters that affected the extraction efficiency were investigated, including the type and volume of desorption solvent, extraction and desorption times, pH of the solution, zeta potential, and amounts of adsorbent and surfactant. Under the optimized extraction conditions, the developed method showed good linearity (R2 = 0.9998) within the range of 0.02–2.7 ng mL−1, and the limit of detection was 0.009 ng mL−1. The spiked recoveries of CVD in urine and plasma samples ranged from 101.50% to 111.00%. To the best of our knowledge, this is the first time that a mixed hemi-/ad-micelle solid-phase extraction method based on magnetic separation and nanoparticles has been used as a simple and sensitive method for the monitoring of CVD in biological samples.

Platform construction and extraction mechanism study of magnetic mixed hemimicelles solid-phase extraction.

Simple, accurate and high-throughput pretreatment method would facilitate large-scale studies of trace analysis in complex samples. Magnetic mixed hemimicelles solid-phase extraction has the power to become a key pretreatment method in biological, environmental and clinical research. However, lacking of experimental predictability and unsharpness of extraction mechanism limit the development of this promising method. Herein, this work tries to establish theoretical-based experimental designs for extraction of trace analytes from complex samples using magnetic mixed hemimicelles solid-phase extraction. We selected three categories and six sub-types of compounds for systematic comparative study of extraction mechanism, and comprehensively illustrated the roles of different force (hydrophobic interaction, π-π stacking interactions, hydrogen-bonding interaction, electrostatic interaction) for the first time. What’s more, the application guidelines for supporting materials, surfactants and sample matrix were also summarized. The extraction mechanism and platform established in the study render its future promising for foreseeable and efficient pretreatment under theoretical based experimental design for trace analytes from environmental, biological and clinical samples.

Mixed hemimicelles solid-phase extraction of cephalosporins in biological samples with ionic liquid-coated magnetic graphene oxide nanoparticles coupled with high-performance liquid chromatographic analysis

A novel mixed hemimicelles solid phase extraction based on magnetic graphene oxide (Fe3O4/GO) and ionic liquid (IL) was developed for the simultaneous extraction and determination of trace cephalosporins in spiked human urine. The high surface area and excellent adsorption capacity of the graphene oxide after modification with1-hexadecyl-3-methylmidazoliumbromide(C16mimBr) were utilized adequately in the solid phase extraction(SPE) process. A comprehensive study of the parameters affecting the extraction recovery, such as the zeta-potential of magnetic graphene oxide, amounts of magnetic graphene oxide and surfactant, pH of solution, ionic strength, extraction time, and desorption condition were optimized. A comparative study on the use of different surfacant-coated Fe3O4/GO NPs as sorbents was presented. Good linearity (R2>0.9987) for all calibration curves was obtained. The LODs were ranged between 0.6 and 1.9ng mL−1 for the cephalosporins and the LOQs were 1.5 to 5.5, respectively. Satisfactory recoveries(84.3% to 101.7%)and low relative standard deviations from 1.7% to 6.3% in biological matrices were achieved. The mixed hemimicelles magnetic SPE (MSPE) method based on ILs and Fe3O4/GO NPs magnetic separation has ever been successfully used for pretreatment of complex biological samples.

Simultaneous determination of trace amounts of anti-hypertensive drugs in urine using magnetic mixed hemimicelles solid-phase extraction combined with HPLC-UV

Hypertension is the leading cause of morbidity and mortality in developed and developing countries. The combination of amlodipine and carvedilol is very effective for reducing blood pressure and improving treatment compliance. Determination of drugs in biological fluids is vital in therapeutic efficacy. In the present study, a simple, rapid and efficient magnetic solid phase extraction procedure based on mixed hemimicelles is described and validated for the simultaneous determination of trace amounts of anti-hypertensive drugs in urine samples using sodium dodecyl sulfate-coated magnetite nanoparticles as extractant. Various factors, which could affect the extraction efficiency were investigated and optimized. Under the optimum conditions, the limits of detection (S/N = 3) for amlodipine and carvedilol were 5 and 2 ng/mL, respectively. The relative standard deviation for six measurements of 50 ng/mL of amlodipine and carvedilol were 4.7 and 5.2%, respectively. The developed method was applied to the analysis of patients' urine samples, and satisfactory results were obtained in the range between 81.6 and 92.7%.

Mixed hemimicelles solid-phase extraction based on sodium dodecyl sulfate-coated nano-magnets for selective adsorption and enrichment of illegal cationic dyes in food matrices prior to high-performance liquid chromatography-diode array detection detection

In this study, mixed hemimicelles solid-phase extraction (MHSPE) based on sodium dodecyl sulfate (SDS) coated nano-magnets Fe3O4 was investigated as a novel method for the extraction and separation of four banned cationic dyes, Auramine O, Rhodamine B, Basic orange 21 and Basic orange 22, in condiments prior to HPLC detection. The main factors affecting the extraction of analysts, such as pH, surfactant and adsorbent concentrations and zeta potential were studied and optimized. Under optimized conditions, the proposed method was successful applied for the analysis of banned cationic dyes in food samples such as chili sauce, soybean paste and tomato sauce. Validation data showed the good recoveries in the range of 70.1–104.5%, with relative standard deviations less than 15%. The method limits of determination/quantification were in the range of 0.2–0.9 and 0.7–3μgkg−1, respectively. The selective adsorption and enrichment of cationic dyes were achieved by the synergistic effects of hydrophobic interactions and electrostatic attraction between mixed hemimicelles and the cationic dyes, which also resulted in the removal of natural pigments interferences from sample extracts. When applied to real samples, RB was detected in several positive samples (chili powders) within the range from 0.042 to 0.177mgkg−1. These results indicate that magnetic MHSPE is an efficient and selective sample preparation technique for the extraction of banned cationic dyes in a complex matrix.

Mixed-Hemimicelle Solid Phase Extraction Followed by Dispersive Liquid-Liquid Microextraction of Amphetamines from Biological Samples

In this work, the synthesized Fe3O4 nanoparticles was coated by sodium dodecyl sulfate and then it was used as a sorbent in mixed-hemimicelle solid phase extraction of some amphetamines, as psychoactive drugs, from biological samples. This extraction method was combined with dispersive liquid-liquid microextraction to enhance enrichment factors of targeted analytes. Effect of different parameters influencing the hybrid extraction performance, such as sodium dodecyl sulfate amount and sample pH, were investigated. The method showed linearity in the range of 1.0-250 and 2.0-250 µg L-1 for the most of analytes in urine and plasma samples, respectively. The limits of detection, based on signal to noise of 3, were found 0.1-0.2 and 0.3-0.5 µg L-1 in urine and plasma samples, respectively. The results of the intra-day and inter-day precision were less than 13.5% for all amphetamines. The amounts of relative recoveries in spiked urine and plasma samples were found in the range of 90-96 and 87-93%, respectively.

Mixed hemi/ad-micelle SDS-coated magnetic Fe2−xAlxO3 (x = 0.4) nanoparticles for the capture of gatifloxacin and prulifloxacin coupled with fluorimetric determination

A mixed hemimicelle solid-phase extraction technique coupled with fluorescence for the extraction of prulifloxacin and gatifloxacin was developed. This method has promising clinical and therapeutic drug monitoring applications.

Development of a novel mixed hemimicelles dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene for the separation and preconcentration of fluoxetine in different matrices before its determination by fiber optic linear array spectrophotometry and mode-mismatched thermal lens spectroscopy

This study aims at developing a novel, sensitive, fast, simple and convenient method for separation and preconcentration of trace amounts of fluoxetine before its spectrophotometric determination. The method is based on combination of magnetic mixed hemimicelles solid phase extraction and dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene as a sorbent. The magnetic graphene was synthesized by a simple coprecipitation method and characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). The retained analyte was eluted using a 100 μL mixture of methanol/acetic acid (9:1) and converted into fluoxetine-β-cyclodextrin inclusion complex. The analyte was then quantified by fiber optic linear array spectrophotometry as well as mode-mismatched thermal lens spectroscopy (TLS). The factors affecting the separation, preconcentration and determination of fluoxetine were investigated and optimized. With a 50 mL sample and under optimized conditions using the spectrophotometry technique, the method exhibited a linear dynamic range of 0.4–60.0 μg L−1, a detection limit of 0.21 μg L−1, an enrichment factor of 167, and a relative standard deviation of 2.1% and 3.8% (n = 6) at 60 μg L−1 level of fluoxetine for intra- and inter-day analyses, respectively. However, with thermal lens spectrometry and a sample volume of 10 mL, the method exhibited a linear dynamic range of 0.05–300 μg L−1, a detection limit of 0.016 μg L−1 and a relative standard deviation of 3.8% and 5.6% (n = 6) at 60 μg L−1 level of fluoxetine for intra- and inter-day analyses, respectively. The method was successfully applied to determine fluoxetine in pharmaceutical formulation, human urine and environmental water samples.

Superparamagnetic Fe3O4@SiO2core-shell composite nanoparticles for the mixed hemimicelle solid-phase extraction of benzodiazepines from hair and wastewater samples before high-performance liquid chromatography analysis

Magnetic Fe3 O4 /SiO2 composite core-shell nanoparticles were synthesized, characterized, and applied for the surfactant-assisted solid-phase extraction of five benzodiazepines diazepam, oxazepam, clonazepam, alprazolam, and midazolam, from human hair and wastewater samples before high-performance liquid chromatography with diode array detection. The nanocomposite was synthesized in two steps. First, Fe3 O4 nanoparticles were prepared by the chemical co-precipitation method of Fe(III) and Fe(II) as reaction substrates and NH3 /H2 O as precipitant. Second, the surface of Fe3 O4 nanoparticles was modified with shell silica by Stober method using tetraethylorthosilicate. The Fe3 O4 /SiO2 composite were characterized by X-ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, and vibrating sample magnetometry. To enhance their adsorptive tendency toward benzodiazepines, cetyltrimethylammonium bromide was added, which was adsorbed on the surface of the Fe3 O4 /SiO2 nanoparticles and formed mixed hemimicelles. The main parameters affecting the efficiency of the method were thoroughly investigated. Under optimum conditions, the calibration curves were linear in the range of 0.10-15 μgmL(-1) . The relative standard deviations ranged from 2.73 to 7.07%. The correlation coefficients varied from 0.9930 to 0.9996.

Mixed hemimicelles solid-phase extraction based on sodium dodecyl sulfate (SDS)-coated nano-magnets for the spectrophotometric determination of Fingolomid in biological fluids

In this study, mixed hemimicelles solid-phase extraction (SPE) based on sodium dodecyl sulfate (SDS)-coated nano-magnets Fe3O4 was investigated as a novel method for the separation and determination of Fingolimod (FLM) in water, urine and plasma samples prior to spectrophotometeric determination. Due to the high surface area of these new sorbents and the excellent adsorption capacity after surface modification by SDS, satisfactory extraction recoveries can be produced. The main factors affecting the adsolubilization of analysts, such as pH, surfactant and adsorbent amounts, ionic strength, extraction time and desorption conditions were studied and optimized. Under the selected conditions, FLM has been quantitatively extracted. The accuracy of the method was evaluated by recovery measurements on spiked samples, and good recoveries of 96%, 95% and 88% were observed for water, urine and plasma respectively. Proper linear behaviors over the investigated concentration ranges of 2–26, 2–17 and 2–13mg/L with good coefficients of determination, 0.998, 0.997 and 0.995 were achieved for water, urine and plasma samples, respectively. To the best of our knowledge, this is the first time that a mixed hemimicelles SPE method based on magnetic separation and nanoparticles has been used as a simple and sensitive method for monitoring of FLM in water and biological samples.

Magnetic mixed hemimicelles solid‐phase extraction coupled with high‐performance liquid chromatography for the extraction and rapid determination of six fluoroquinolones in environmental water samples

In this study, a mixed hemimicelle solid-phase extraction method based on Fe3 O4 nanoparticles coated with sodium dodecyl sulfate was applied for the preconcentration and fast isolation of six fluoroquinolones in environmental water samples before high-performance liquid chromatography determination. The main factors affecting the extraction efficiency of the analytes, such as amount of surfactant, amount of Fe3 O4 nanoparticles, extraction time, sample volume, sample pH, ionic strength, and desorption conditions, were investigated and optimized. The method has detection limits from 0.05 to 0.1 ng/mL and good linearity (r ≥ 09948) in the range 0.1-200 ng/mL depending on the fluoroquinolone. The enrichment factor is ∼200. The recoveries (at spiked levels of 1, 5, and 50 ng/mL) are in the range of 79-120%.

Preparation of barium sulfate-coated magnetite particles for the extraction of trimethoprim from environmental water samples based on mixed hemimicelles solid-phase extraction

In this study, barium sulfate-coated magnetite particles (Fe3O4/BaSO4) for mixed hemimicelles solid-phase extraction, have been successfully synthesized by a chemical coprecipitation method.

Mixed hemimicelle solid-phase extraction based on magnetic carbon nanotubes and ionic liquids for the determination of flavonoids

A novel mixed hemimicelles solid phase extraction (SPE) based on magnetic carbon nanotubes (MCNTs) and ionic liquid (IL) is developed for the simultaneous extraction and determination of trace flavonoids in spiked human urine. In this novel SPE, the formation of C16mimBr with mixed hemimicelles on the surface of MCNTs@SiO2 nanoparticles (NPs) causes retention of analytes by strong hydrophobic, π–π and electrostatic interactions. This SPE technique combines the advantages of mixed hemimicelles and MCNTs. In order to establish the guidelines for the preparation of mixed hemimicelles on composite materials, different main factors affecting the preconcentration of analytes, such as material type, amount of surfactant, pH of solution, ionic strength, extraction time, desorption condition and regeneration property, were investigated and optimized. Under the selected conditions, the accuracy of the method was evaluated by recovery measurements on spiked samples, and good recoveries with low relative standard deviations from 3.5% to 4.9% were achieved. No interferences were caused by endogenous compounds in human urine. For our knowledge, this is the first development of a mixed hemimicelles SPE based on MCNTs and IL for the extraction of trace analytes in complex biological samples.

Magnetically mixed hemimicelles solid-phase extraction based on ionic liquid-coated Fe3O4 nanoparticles for the analysis of trace organic contaminants in water

Magnetically mixed hemimicelles formed by ionic liquid-coated Fe3O4 magnetic nanoparticles (IL-coated Fe3O4 NPs) as an adsorbent of solid-phase extraction are proposed for the preconcentration of five organic contaminants.