Ultrasound-assisted Solid-phase Extraction Research Articles

Solid phase extraction with rotating cigarette filter for determination of bisphenol A in source and drinking water: computational and analytical studies.

An ultrasound assisted solid phase extraction method using rotating cigarette filter is developed herein to preconcentrate and determine trace amount of bisphenol in source and drinking water. Qualitative and quantitative measurements were performed using high-performance liquid chromatography coupled with ultra violet detector. Sorbent-analyte interactions were thoroughly investigated computationally and experimentally using molecular dynamics simulations; and attenuated total reflectance Fourier transform infrared spectroscopy, and Raman spectroscopy, respectively. Various extraction parameters were investigated and optimized. Under the optimal conditions, the results were linear in a low scale range of 0.01-55ng/mL with correlation coefficient of 0.9941 and a low limit of detection (0.04ng/mL, signal/noise = 3:1). A good precision (intra-day relative standard deviation ≤ 6.05%, inter-day relative standard deviation ≤ 7.12%) and recovery (intra-day ≥ 98.41%, inter-day ≥ 98.04%)) are obtained. Finally, the proposed solid phase extraction method offered a low cost, simple, fast, and sensitive analytical method to determine trace amount of bisphenol A in source and drinking water samples with chromatographic detection.

Magnetic Graphene Oxide Modified with a Surface-Active Ionic Liquid for Ultrasound-Assisted Solid-Phase Extraction (UA-SPE) to Preconcentrate Lenalidomide from Human Plasma with Determination by High-Performance Liquid Chromatography with Ultraviolet Detection (HPLC-UV)

A new magnetic graphene oxide (MGO) composite was developed as an adsorbent for the preconcentration of lenalidomide (LND) by ultrasound-assisted solid-phase extraction (UA-SPE) prior to determination by high-performance liquid chromatography with ultraviolet detection (HPLC-UV). The adsorbent was fabricated through chemical functionalization of a new surface-active ionic liquid (SAIL), i.e. 1-methyl-3-(trimethoxysilyl propyl)-imidazolium dodecyl sulfate (TMES-Im-DS) on MGO. The synthesized material presented the benefits of excellent adsorption for LND. The characterization of the synthesized functionalized magnetic nanocomposite was performed by Fourier transform-infrared spectroscopy, field emission scanning electron microscopy, Brunauer–Emmett–Teller (BET), vibrating sample magnetometry, and energy-dispersive X-ray spectroscopy. After optimization of the parameters, the limits of detection (LOD) and limit of quantification (LOQ) were 0.2 and 0.8 µg L−1 and 0.6 and 2.5 µg L−1in water and plasma samples, respectively. The enrichment factors (EFs) were from 90 to 180 in the samples. The relative standard deviation (RSD%, n = 5) as intra- and inter-day precision were from 6.3% to 7.5% and 7.1% to 8.5% in water and plasma, respectively. Lastly, the developed method presented good results for the preconcentration of LND in plasma with satisfactory repeatability.

Ultrasound assisted solid phase extraction of methylene blue dye by MgSiO3 nanoparticles through central composite design

ABSTRACT Current study is based on the synthesis and characterisation of MgSiO3 nanoparticles (MgSiO3 NPs) and its application for ultrasound-assisted solid-phase extraction (UASPE) of methylene blue (MB) dye from water samples using UV-Vis spectrophotometry. The prepared MgSiO3 NPs were fully identified and characterised by different techniques such as Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Scanning electron microscope (SEM) and Energy-dispersive X-ray spectroscopy (EDS). The prepared nano sorbent had spherical shape with size diameter of 20 nm. Central composite design (CCD) optimisation approach as versatile tool was used for investigation and optimisation of the effective parameters. Using CCD method, the optimised conditions were achieved to be pH of 7.0, sorbent dosage of 29.80 mg, ultrasonic time of 10.34 min, and temperature of 25°C at 500 µl of dimethylformamide eluent using Triton X-100 surfactant. Under the optimised conditions, the proposed method is applicable for wide linear range with detection limit of 0.084 mg L−1, limit of quantification of 0.28 mg L−1. The prepared MgSiO3 NPs have exceptional properties in terms of porous and sheets structure and also high adsorption capacity. In addition, the applied method showed satisfactory figure of merits in terms of pre-concentration factor of 10, which make candidate the applied method and nano sorbent as an operative and ideal candidate for pre-concentration and determination trace level of MB from water samples.

A hybrid material composed of multiwalled carbon nanotubes and MoSe2 nanorods as a sorbent for ultrasound-assisted solid-phase extraction of lead(II) and copper(II).

A MWCNT@MoSe2 nanorod hybrid material was synthesized by a hydrothermal method and used as an adsorbent for trace levels of Pb(II) and Cu(II). The material was characterized by Raman spectroscopy, XRD, SEM, SEM-EDX, SEM-mapping and BET methods. The hybrid material is demonstrated to be a viable sorbent for ultrasound-assisted solid phase extraction of Pb(II) and Cu(II) at pH5.5. Following desorption with 3 M HNO3, the two elements were quantified by FAAS. Key parameters affecting the extraction efficiency, including eluent conditions, amount of adsorbent, sample volume were optimized. No significant interference by other ions is observed. The accuracy of the method was evaluated by the analysis of the certified reference materials TMDA-53.3 (lake water) and SPS-WW2 (waste water level 2). The recoveries were in good agreement with certified values. The method was successfully applied to the extraction/preconcentration of Pb(II) and Cu(II) in different real samples. Graphical abstract A hybrid material of type MWCNT@MoSe2 was synthesized, characterized, and used as adsorbent for Pb(II) and Cu(II). Key parameters affecting the extraction efficiency, including eluent conditions, amount of adsorbent, sample volume were optimized. The method was applied to the extraction of analytes in water samples.

Cu2O-CuO ball like/multiwalled carbon nanotube hybrid for fast and effective ultrasound-assisted solid phase extraction of uranium at ultra-trace level prior to ICP-MS detection

Multiwalled carbon nanotube/Cu2O-CuO ball like hybrid material (MWCNTs/Cu2O-CuO) synthesized using of a green hydrothermal process was evaluated as a new sorbent for solid phase extraction of uranium with inductively coupled plasma mass spectrometry (ICP-MS). According to our best knowledge, this new material was synthesized and used as solid phase extraction adsorbent for the first time in the literature. The characterization of new hybrid material was carried out using Raman spectroscopy, X-ray diffraction (XRD) and scanning electronic microscopy techniques (SEM, SEM-EDX and SEM-Mapping). The characterization results demonstrated that the new hybrid nanostructure was successfully obtained. The ultrasound-assisted solid phase extraction (UA-SPE) procedure was performed using 100 mg of new hybrid sorbent, 1000 μL of a 0.1% (w/v) solution of α-benzoin oxime and 2000 μL of phosphate buffer at pH 7.0 for separation and preconcentration of uranium. Uranium was eluted with 2 M HCl and the levels of uranium was measured by using ICP-MS. The linearity was observed between 2.5 and 100 ng mL−1 concentration range with a good correlation coefficient (r = 0.999, n = 7). The obtained limit of detection and quantitation values were 0.52 and 1.70 ng mL−1, respectively. Under optimum conditions, the preconcentration factor (PF) was calculated as 13.3. The accuracy of the developed method was assessed by analyzing of TMDA-62.2, TMDA-70.2 (Environment Canada) and GBW-07423 certified reference water and soil materials. The proposed UA-SPE-ICP-MS procedure developed with MWCNTs/Cu2O-CuO hybrid material was successfully applied to the analysis of uranium at ultra-traces levels in environmental water and geological rock samples.

Ultrasound-assisted solid-phase extraction of parabens from environmental and biological samples using magnetic hydroxyapatite nanoparticles as an efficient and regenerable nanosorbent.

Magnetic hydroxyapatite nanoparticles (γ-Fe2O3@HAP) are shown to be a viable sorbent for the preconcentration and adsorption of parabens (specifically of methyl-, ethyl-, propyl-, butyl-, pentyl-, phenyl- and benzylparaben). The average diameter of the magnetic γ-Fe2O3@HAP nanoadsorbents is 25nm. The effects of amount of nanoadsorbent, pH value and time of adsorption on the adsorption efficiency were studied by chemometry and optimized using a Box-Behnken design, and the respective response surface equations were derived. The loaded magnetic nanoadsorbent can be removed from the aqueous sample by applying an external magnetic field. Following extraction with acetonitrile, the parabens were quantified by gas chromatography with mass spectrometric detection. Under optimum condition, the limit of detection (LOD) and adsorption efficiencies of the method are in the range from 5 to 10μgL-1 and 95-106%, respectively. The preconcentration factors range from 320 to 350. The results demonstrate that this nanoadsorbent can be applied to the removal of parabens from different water, soil, beverage and urine samples. Graphical abstract Schematic representation of ultrasound-assisted solid-phase extraction of parabens from environmental and biological samples by γ-Fe2O3@HAP nanoadsorbent as a new and effective method with high reproducibility and reusability.

Development and application of metal organic framework/chitosan foams based on ultrasound-assisted solid-phase extraction coupling to UPLC-MS/MS for the determination of five parabens in water.

In this work, a variety of highly porous metal organic framework/chitosan (MOF/CS) foams (MIL-53(Al)/CS, MIL-53(Fe)/CS, MIL-101(Cr)/CS, MIL-101(Fe)/CS, UiO-66(Zr)/CS, and MIL-100(Fe)/CS) were designed and prepared by an ice-templating process. The introduction of MOFs made these foams achieve excellent inherent characters in terms of strength, stability, and adsorption ability. The MOFs incorporated in the foams retained their unique properties. Additionally, the foams were durable and their adsorption abilities had only a little loss after being recycled several times. MIL-53(Al)/CS foam was selected as an adsorbent candidate to develop an ultrasound-assisted solid-phase extraction (UA-SPE) method for the first time, owing to its particularly noteworthy performance among the prepared MOF/CS foams. The method was then successfully applied to extract trace amount of five parabens (methylparaben, ethylparaben, propylparaben, butylparaben, benzylparaben) in water samples, followed by ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) detection. Several experimental parameters were investigated. Under the optimal conditions, the linear ranges were 0.5-200μg/L with regression coefficients (r2) from 0.9948 to 0.9983. The method detection limits were between 0.09 and 0.45μg/L. The recoveries ranged from 78.75 to 102.1% with relative standard deviations (RSDs) < 7.4%. Furthermore, the molecular interactions and free binding energies between MOFs and parabens were calculated by means of molecular docking to explain the adsorption mechanism deeply. The novel method proposed in this work exhibited many benefits such as easy operation, high enrichment efficiency, less solvent consuming, and higher sensitivity. Such a strategy would expand the application prospect of MOFs in sample pretreatment. Graphical abstract ᅟ.

Ultra-trace determination of thallium(I) using a nanocomposite consisting of magnetite, halloysite nanotubes and dibenzo-18-crown-6 for preconcentration prior to its quantitation by ET-AAS

A nanocomposite modified with dibenzo-18-crown-6 was synthesized and applied as a new sorbent for the preconcentration of thallium(I) via ultrasound assisted-solid phase extraction. This extraction step was combined with electrothermal atomic absorption spectrometry to determine ultra-trace amounts of thallium(I). The nanocomposite was characterized by Fourier transform infrared spectroscopy, X-ray diffraction spectrometry, field emission scanning electron microscopy and transmission electron microscopy. Under the optimized conditions, a dynamic linear range from 7.0 to 435 ng L−1, a detection limit of 1.8 ng L−1 and a quantification limit of 6.0 ng L−1 were obtained. Also, the intra- and inter-day relative standard deviations for 20.0 ng mL−1 Tl(I) were calculated as ±4.8% and ±5.1%, respectively. The adsorbent was applied to the determination of thallium(I) in the environmental, biological and standard samples with satisfactory results.

Determination of ionic liquid cations in soil samples by ultrasound-assisted solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry

Liquid chromatography-tandem mass spectrometry coupled with an ultrasonic-assisted extraction and solid phase extraction procedure has been investigated for the separation and detection of ionic liquid cations in soil samples.

Ultrasound-assisted solid phase extraction of nitro- and chloro-(phenols) using magnetic iron oxide nanoparticles and Aliquat 336 ionic liquid

A novel and sensitive ultrasound-assisted solid phase extraction (UASPE) method for pre-concentration and determination of ultra-trace amounts of nitrophenols and chlorophenols in water samples was demonstrated. Four hazardous phenolic compounds in water samples were extracted and monitored by high performance liquid chromatography. The results demonstrated that in the presence of Aliquat 336 (ALQ), magnetic iron oxide nanoparticles (MIONPs) were quite efficient in the adsorption and pre-concentration of traces of analytes. MIONPs were synthesized and characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The important parameters influencing the extraction efficiency were studied and optimized. The separation and pre-concentration steps were fast and completed in 10min. Acetonitrile was used for the desorption of target analytes. Under optimum adsorption conditions, a linear range between 0.015 and 100μgL−1 (R2≥0.997), and limits of detections (LODs) ranging from 0.005 to 0.041μgL−1 were obtained. Enrichment factors in the range of 76–195 were achieved and relative standard deviations (%RSDs) were less than 10.0 (n=3) for the target analytes. The analytical method was successfully applied for environmental water samples such as tap water and river water. The recoveries varied within the range of 70–119% confirming the good performance of the method in various water samples. The results showed that the proposed method is a rapid, convenient and feasible technique for the determination of nitrophenols and chlorophenols in aqueous samples.

Determination of Zn(II) in rock and vegetable samples after acidic digestion followed by ultrasound-assisted solid-phase extraction with reduced graphene oxide as novel sorbent, in combination with flame atomic absorption spectrometry

Graphene, a novel class of carbon nanostructures, has great promise for use as sorbent materials because of its ultrahigh specific surface area. A new method using reduced graphene oxide (RGO) as sorbent was developed for the preconcentration of trace amounts of zinc (Zn) to its determination by flame atomic absorption spectrometry. Zinc could be adsorbed quantitatively on RGO in the pH range of 1–9, and then eluted completely with 0.5 mL of 0.1 mol L−1 HCl. Some effective parameters on the extraction were selected and optimized. Under optimum conditions, the calibration graph was linear in the concentration range of 0.2–15 μg L−1 with a detection limit of 0.14 μg L−1 with an enrichment factor of 100.12. The relative standard deviation for ten replicate measurements of 10 μg L−1 of Zn was 0.58 %, respectively. The proposed method was successfully applied in the analysis of rock and vegetable samples. Good spiked recoveries over the range of 99.9–100 % were obtained. This work not only proposes a useful method for sample preconcentration, but also reveals the great potential of graphene as an excellent sorbent material in analytical processes.

Ultrasound-assisted solid-phase extraction using multiwalled carbon nanotubes for determination of cadmium by flame atomic absorption spectrometry

Ultrasound-assisted solid-phase extraction (SPE) with multiwalled carbon nanotubes (MWCNTs) as a solid sorbent and 1-(2-pyridylazo)-2-naphthol (PAN) as a chelating agent was developed for the determination of trace and ultratrace amounts of Cd(II) ions in aqueous samples. The solution containing Cd(II) complexed with PAN was passed through the syringe filter with a PVDF membrane loaded with 25 mg of MWCNTs. The elution process was performed with 2.0 mL of 2.0 mol L−1 HNO3 with assistance of sonication. In order to obtain the high recovery of the Cd(II) ions, the proposed procedure was optimized for various analytical parameters such as pH, amounts of PAN, sample volume, and elution conditions such as volume and concentration of eluent and influence of sonication and temperature. The investigation shows that sonication considerably improves the recovery, whereas temperature does not influence the elution process. Under optimized conditions Cd(II) ions can be determined with very good recovery (99 ± 3%), precision (RSD = 3.2%) and detection limit (0.3 ng mL−1) for an enrichment factor of 50. The effect of common coexisting ions was also investigated. Cd(II) can be determined in the presence of heavy metal ions and alkali metals. The proposed ultrasound-assisted SPE was applied for the determination of Cd(II) in water samples and biological samples (Lobster Hepatopancreas).