Vortex-assisted Solid-phase Extraction Research Articles

Metal organic framework composite (Ti3AlC2 @ZIF-67) for vortex assisted solid phase extraction of lead from water and food samples

A composite of Ti3AlC2 max phase and ZIF-67 metal-organic framework (Ti3AlC2 @ ZIF- 67) was synthesized by mixing Ti3AlC2 and ZIF-67 in dimethyl formamide and used for solid phase extraction of Pb(II). Fourier transformation infrared spectroscopy, scanning electron microscopy, x-ray diffraction, and energy dispersive x-ray were used to find functional group, surface morphology, surface area elemental composition, and crystalline structure of Ti3AlC2 @ ZIF-67. Factors like solution pH (7.0), adsorbent dose (10.0 mg), sample volume, eluent concentration and volume (0.5 M, 1.0 mL), and vortex time (1.0 min) were optimized. The effect of interfering ions has been checked to determine the method's selectivity. Analytical parameters such as limit of detection (LOD) 0.26 µg L−1, limit of quantification (LOQ) 0.86 µg L−1, preconcentration factor (PF) 21, enhancement factor (EF) 20 and relative standard deviation (RSD) 4.6% were calculated under optimized experimental condition. Certified reference materials TMDA-64.3 water samples and INCT-OBTL-5 tobacco leaves were used to validate the accuracy of the proposed method for trace metals detection. The technique was also used for lead determination in food and water samples with satisfactory recovery results.

Natural Luffa cylindrica sponge sorbent for the solid phase extraction of estrone, 17-β-estradiol, and testosterone in aquaculture water

The bare natural fibrous skeleton of Luffa cylindrica (LC) sponge gourd was simply prepared and used as a sorbent in the vortex-assisted solid phase extraction (VA-SPE) of three steroid hormones, estrone (E1), 17-β-estradiol (E2), and testosterone (T) from aquaculture water samples. The extracted compounds were analysed by high performance liquid chromatography with a diode array detector (HPLC-DAD). Extraction with the prepared sorbent was highly efficient, completing within 10 min. The developed method showed good linearity in a concentration range of 15–1000 μg L−1 for E1, E2, and T. The limits of detection (LODs) were 9.6 ± 0.1 μg L−1 for E1, 9.8 ± 0.1 μg L−1 for E2, and 9.7 ± 0.1 μgL−1 for T. The respective limits of quantitation (LOQs) were 32.1 ± 0.3 μg L−1, 32.7 ± 0.4 μg L−1, and 32.2 ± 0.5 μg L−1. Good reproducibility (RSD < 3.5%, n = 6), good precision (RSD < 6.8%, n = 6), and excellent reusability (n = 22, RSD < 8%) were achieved. Recoveries from real spiked samples ranged from 70.2 ± 0.1% to 98.9 ± 4.7% with RSDs lower than 6.0%. The proposed method is simple, fast, inexpensive, and eco-friendly, with potential applications in the trace analysis of steroid hormones. Novelty statementOnly a few studies have focused on sample preparation for the simultaneous determination of steroid hormones in aquaculture water. The authors believe that the use of unmodified naturally available Luffa cylindrica as a solid phase extraction (SPE) sorbent has not yet been reported. This work successfully developed, for the first time from the bare fibrous skeleton of Luffa cylindrica, a very simple and low-cost SPE sorbent to extract E1, E2, and T for simultaneous determination by HPLC.

Magnetic Adsorbent Decorated with Poly(N-Isopropylacrylamide) (PNIPAM) Brushes for the Vortex-Assisted Solid Phase Extraction (VASPE) of Lead in Water, Cigarettes and Soil with High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS) Detection

Here is reported the synthesis of a magnetic phosphorus-containing adsorbent decorated with poly(N-isopropylacrylamide) (PNIPAM) brushes via surface-initiated atom transfer radical polymerization (SI-ATRP) and its application for vortex assisted solid phase extraction of lead in water, cigarettes and soil. The adsorbent was characterized using Fourier-transform infrared spectroscopy (FT-IR) and energy dispersive x-ray (EDX) spectroscopy. A high-resolution continuum source flame atomic absorption spectrometer (HR-CS FAAS) was used for the quantification of lead. All factors affecting the extraction efficiency including the solution pH, adsorbent dose, sample volume, vortex time, and elution protocols were optimized. The limits of detection (LOD) and quantification (LOQ) were determined to be 0.05 µg L−1 and 0.18 µg L−1, respectively. The preconcentration and enhancement factors were 20 and 18. Validation was performed using TMDA 64.3 fortified water and INCT-OBTL-5 tobacco leaves certified reference materials with satisfactory recoveries. The method was shown to be sensitive, efficient and reproducible.

Vortex-assisted solid phase extraction on MIL-101(Cr) of parabens in waters and cosmetics by HPLC–DAD

Vortex-assisted solid phase extraction on MIL-101(Cr) of parabens in waters and cosmetics by HPLC–DAD

A simple gelatin aerogel tablet sorbent for the effective vortex assisted solid phase extraction of polycyclic aromatic hydrocarbons from tea samples

A gelatin aerogel tablet was used as a vortex assisted solid phase extraction (VA-SPE) sorbent for the determination of polycyclic aromatic hydrocarbons (PAHs), benzo(a)anthracene (BaA), benzo(b)fluoranthene (BbF), and benzo(a)pyrene (BaP) in tea samples. They have been quantified by a high-performance liquid chromatography with a diode array detector (HPLC-DAD). The method shows good linearity (R2 = 0.999) at concentrations of 5.00–200 ng L−1, with the limits of detection of 1.65 ± 0.02, 1.81 ± 0.02, and 2.06 ± 0.03 ng L−1 for BaA, BbF, and BaP, respectively. Good reproducibility (RSDs < 0.24%, n = 6), good precision (RSDs < 6.3%), and excellent reusability (n = 40, RSDs < 0.17%) were achieved. The tablet can extract PAHs within 1.5 min with good recoveries (70.10 ± 0.74% – 119.3 ± 4.1%). This method, which is simple, rapid, ecofriendly, and inexpensive, requires low consumption of organic solvent, and has potential application in food safety.

Vortex-assisted solid-phase extraction based on metal-organic framework/chitosan-functionalized hydrophilic sponge column for determination of triazine herbicides in environmental water by liquid chromatography-tandem mass spectrometry

In the presented work, MIL-101(Cr) and chitosan were directly embedded on the skeleton of melamine sponge material using a simple and environmentally friendly method. Chitosan acts not only as an adhesive during the preparation of functionalized sponges, but also as an adsorption adjuvant in herbicide detection. Unlike other polymers, chitosan has excellent hydrophilicity and contains numerous adsorption sites; thus, it enables the sponge material to be used for determination of contaminants in an aqueous phase. Scanning electron microscopic (SEM) analysis showed that the coating material was uniformly distributed on the skeleton of melamine sponge. The prepared material was used as a sorbent in a vortex-assisted solid-phase extraction and combined with high performance liquid phase tandem mass spectrometry for the extraction and trace determination of six triazines in water samples (Atraton, Desmetryn, Prometon, Ametryn, Prometryn and Dimethametryn). Several parameters that affect the extraction efficiencies were investigated. Under the optimal conditions (MIL-101(Cr) loading, 150 mg; sample pH, 7; salt concentration, 0%; adsorption time, 3 min; desorption solvent, 1.5 mL acetonitrile; desorption time, 4 min), the proposed method was successfully used in the determination of trace triazines in five real water samples (drinking water, tap water, lake waters and river water), satisfactory recoveries were obtained in the range of 78.9%–118.6%. The limits of detection of the proposed method in detecting triazine herbicides in spiked water samples ranged from 0.014 to 0.045 ng mL−1.

One-step fabrication of hydrophilic MIL-68(Al)/Chitosan-coated melamine sponge for vortex-assisted solid-phase extraction of parabens in water samples

A novel vortex-assisted solid-phase extraction method based on MIL-68(Al)/Chitosan-melamine sponge column (or V-MIL-68(Al)/CS-SC-SPE) is presented in this paper. The MIL-68(Al)/Chitosan-sponge column was prepared by a simple infiltration method and a preparation process that does not consume organic solvents. Scanning electron microscopy was used to characterize the functionalized sponge columns, and the skeleton and pores of the melamine sponge were successfully modified with the coating material (MIL-68(Al) and chitosan). Chitosan was used successfully not only as an adsorption adjuvant material, but also as an adhesive in the preparation of MIL-68(Al)/CS coating sponge materials. The presented method was further combined with high performance liquid chromatography (HPLC) and used in the determination of trace parabens (including methyl-, ethyl-, propyl- and butyl-parabens) in environmental water samples. Several important factors that affect the extraction performance were investigated. Under the optimum conditions, the method was successfully used to detect the four kinds of parabens in different water samples (domestic water, lake water and river water). The limits of detection ranged between 0.21 and 0.50 ng/mL, and the relative standard deviations for all parabens were below 10.8%.

Application of vortex-assisted solid-phase extraction for the simultaneous preconcentration of Cd(ii) and Pb(ii) by nano clinoptilolite modified with 5(p-dimethylaminobenzylidene) rhodanine

Herein, a simple, fast and reliable method based on vortex-assisted solid-phase extraction (VA-SPE) followed by flame atomic absorption spectrometry was developed for the simultaneous preconcentration and trace detection of cadmium and lead.

Vortex assisted solid-phase extraction of lead(II) using orthorhombic nanosized Bi2WO6 as a sorbent.

Nanosized single crystal orthorhombic Bi2WO6 was synthesized by a hydrothermal method and used as a sorbent for vortex assisted solid phase extraction of lead(II). The crystal and molecular structure of the sorbent was examined using XRD, Raman, SEM and SEM-EDX analysis. Various parameters affecting extraction efficiency were optimized by using multivariate design. The effect of diverse ions on the extraction also was studied. Lead was quantified by flame atomic absorption spectrometry (FAAS). The recoveries of lead(II) from spiked samples (at a typical spiking level of 200-400ng·mL-1) are >95%. Other figures of merit includes (a) a detection limit of 6ng·mL-1, (b) a preconcentration factor of 50, (c) a relative standard deviation of 1.6%, and (d) and adsorption capacity of 6.6mg·g-1. The procedure was successfully applied to accurate determination of lead in (spiked) pomegranate and water samples. Graphical abstract Nanosized single crystal orthorhombic Bi2WO6 was synthesized and characterized by a hydrothermal method and used as a sorbent for vortex assisted solid phase extraction of lead(II). The procedure was successfully applied to accurate determination of lead in (spiked) pomegranate and water samples.

Nanosized spongelike Mn3O4 as an adsorbent for preconcentration by vortex assisted solid phase extraction of copper and lead in various food and herb samples

In this paper, a nanosized spongelike Mn3O4 was synthesized and used for the first time as an effective adsorbent for vortex-assisted separation and preconcentration of lead and copper from various food samples. Copper and lead were determined by flame atomic absorption spectrometry. The characterization of the nanosized spongelike Mn3O4 was performed by X-ray diffraction, scanning electron microscopy, Raman spectroscopy, Brunauer, Emmett and Teller surface area and zeta potential measurement. The contact times for both adsorption and elution were only 3min. Under the optimized conditions, detection limits for copper and lead were found to be 2.6μgL−1 and 3.0μgL−1, respectively. The relative standard deviations were found to be ⩽3.2%. The accuracy of the method was confirmed by analyzing the standard reference materials (BCR-482 Licken and SRM 1573a Tomato Leaves) and spiked real food and herb samples.

Spectrophotometric determination of basic fuchsin from various water samples after vortex assisted solid phase extraction using reduced graphene oxide as an adsorbent

In this study, a fast and simple vortex assisted solid phase extraction method was developed for the separation/preconcentration of basic fuchsin in various water samples. The determination of basic fuchsin was carried out at a wavelength of 554nm by spectrophotometry. Reduced graphene oxide which was used as a solid phase extractor was synthesized and characterized by X-ray diffraction, scanning electron microscopy and the Brunauer, Emmett and Teller. The optimum conditions are as follows: pH 2, contact times for adsorption and elution of 30s and 90s, respectively, 10mg adsorbent, and eluent (ethanol) volume of 1mL. The effects of some interfering ions and dyes were investigated. The method was linear in the concentration range of 50–250μgL−1. The adsorption capacity was 34.1mgg−1. The preconcentration factor, limit of detection and precision (RSD, %) of the method were found to be 400, 0.07μgL−1 and 1.2%, respectively. The described method was validated by analyzing basic fuchsin spiked certified reference material (SPS-WW1 Batch 114-Wastewater) and spiked real water samples.