Dispersive Solid‐Phase Extraction

Socas‐Rodríguez, Bárbara; Herrera‐Herrera, Antonio V.; Asensio‐Ramos, María; Hernández‐Borges, Javier

doi:10.1002/9783527678129.assep056

Cited by 47 publications

(13 citation statements)

References 241 publications

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“…Since then, a variety of MOFs coming from the most widely known families have been tested so far in a number of analytical SPE applications [ 15 , 16 , 18 , 20 ] and even in chromatography [ 17 ]. The dispersive mode of the miniaturized solid-phase extraction method (D-μSPE) is a successful approach widely used in sample preparation given its simplicity [ 21 ]. It requires a strong dispersion of the sorbent (in an amount lower than 500 mg) into an aqueous sample containing analytes (i.e., with the aid of vortex or ultrasounds), followed by proper separation of the sorbent containing extracted analytes from the sample, and further elution/desorption of trapped analytes before the chromatographic determination [ 16 , 21 , 22 ].…”

Section: Introductionmentioning

confidence: 99%

Influence of Ligand Functionalization of UiO-66-Based Metal-Organic Frameworks When Used as Sorbents in Dispersive Solid-Phase Analytical Microextraction for Different Aqueous Organic Pollutants

et al. 2018

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Four metal-organic frameworks (MOFs), specifically UiO-66, UiO-66-NH2, UiO-66-NO2, and MIL-53(Al), were synthesized, characterized, and used as sorbents in a dispersive micro-solid phase extraction (D-µSPE) method for the determination of nine pollutants of different nature, including drugs, phenols, polycyclic aromatic hydrocarbons, and personal care products in environmental waters. The D-µSPE method, using these MOFs as sorbents and in combination with high-performance liquid chromatography (HPLC) and diode-array detection (DAD), was optimized. The optimization study pointed out to UiO-66-NO2 as the best MOF to use in the multi-component determination. Furthermore, the utilization of isoreticular MOFs based on UiO-66 with the same topology but different functional groups, and MIL-53(Al) to compare with, allowed us for the first time to evaluate the influence of such functionalization of the ligand with regards to the efficiency of the D-µSPE-HPLC-DAD method. Optimum conditions included: 20 mg of UiO-66-NO2 MOF in 20 mL of the aqueous sample, 3 min of agitation by vortex and 5 min of centrifugation, followed by the use of only 500 µL of acetonitrile as desorption solvent (once the MOF containing analytes was separated), 5 min of vortex and 5 min of centrifugation. The validation of the D-µSPE-HPLC-DAD method showed limits of detection down to 1.5 ng·L−1, average relative recoveries of 107% for a spiked level of 1.50 µg·L−1, and inter-day precision values with relative standard deviations lower than 14%, for the group of pollutants considered.

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Section: Introductionmentioning

confidence: 99%

Influence of Ligand Functionalization of UiO-66-Based Metal-Organic Frameworks When Used as Sorbents in Dispersive Solid-Phase Analytical Microextraction for Different Aqueous Organic Pollutants

et al. 2018

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“…SPE has become one of the main extraction techniques in sample preparation since its introduction in 1972 [ 49 ] due to its well-known advantages with respect to other solvent-based procedures. However, some drawbacks, such as the need for conditioning and sample loading steps, resulting in long extraction times; difficulties in performing more than one extraction at a time; and carry-over problems derived from the reusability of the sorbents or cartridges blocking caused by particles and microorganisms from the sample matrix, made necessary the introduction of sorbent-based extraction alternatives in order to solve those problems/drawbacks [ 50 ]. In this sense, multiple modifications of the original procedure have been proposed, including several miniaturized versions following the same concept, such as PT-SPE or spin column SPE, among others, as previously indicated [ 51 ].…”

Section: Cofs As Sorbents In Solid-phase Extractionmentioning

confidence: 99%

“…However, the dSPE version meant a revolution for this technique in terms of simplification and time savings, since the direct dispersion of the sorbent into the sample matrix allowed one to avoid conditioning and sample loading steps, considered as the bottlenecks of conventional SPE. At the same time, dSPE allows the analysis of complex matrices, such as environmental and food samples, without classical blocking problems [ 50 ]. Although dSPE was initially introduced as a clean-up procedure as part of the QuEChERS (quick, easy, cheap, effective, rugged and safe) method [ 52 ], it has shown a good performance when it is applied with extraction purposes.…”

Section: Cofs As Sorbents In Solid-phase Extractionmentioning

confidence: 99%

Covalent Organic Frameworks in Sample Preparation

et al. 2020

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Covalent organic frameworks (COFs) can be classified as emerging porous crystalline polymers with extremely high porosity and surface area size, and good thermal stability. These properties have awakened the interests of many areas, opening new horizons of research and applications. In the Analytical Chemistry field, COFs have found an important application in sample preparation approaches since their inherent properties clearly match, in a good number of cases, with the ideal characteristics of any extraction or clean-up sorbent. The review article is meant to provide a detailed overview of the different COFs that have been used up to now for sample preparation (i.e., solid-phase extraction in its most relevant operational modes—conventional, dispersive, magnetic/solid-phase microextraction and stir-bar sorptive extraction); the extraction devices/formats in which they have been applied; and their performances and suitability for this task.

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“…SPME utilizes a very small amount of solid for extraction (i.e., of the order of µg) and therefore minimizes the consumption of adsorbent and can lead to a faster extraction process compared to the traditional SPE. Nowadays, there is a wide diversity of possible SPME configurations, such as Stir Bar Sorptive Extraction (SBSE), Dispersive micro Solid-Phase Extraction (DµSPE) or Thin-Film Microextraction (TFME), among others [14][15][16]. Moreover, there is also a wide variety of materials that can be used as solid adsorbents; from the classical activated carbon or silica-gel to the most modern nanomaterials, such as ordered mesoporous silica, silica nanoparticles, carbon nanotubes, graphene or metal-organic frameworks (MOFs), among others [16,17].…”

Section: Introductionmentioning

confidence: 99%

Dispersive micro solid-phase extraction (DµSPE) with graphene oxide as adsorbent for sensitive elemental analysis of aqueous samples by laser induced breakdown spectroscopy (LIBS)

Ruíz

Ripoll

Hidalgo

et al. 2019

Talanta

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In this work, the combination of dispersive micro solid-phase extraction (DµSPE) with laser-induced breakdown spectroscopy (LIBS) was evaluated for simultaneous preconcentration and detection of Zn, Cd, Mn, Ni, Cr and Pb in aqueous samples. Two adsorbent materials were tested in the microextraction step, namely graphene oxide and activated carbon. In both cases, the microextraction process consisted in the dispersion of a small quantity of adsorbent in the sample solution containing the analytes. However, while the use of activated carbon required a previous chelation of the metals, this step was avoided with the use of graphene oxide. After extraction, the analytes retained in the adsorbents were analysed by LIBS. Several experimental factors affecting the extraction of the metals (adsorbent amount, pH and extraction time) were optimized by means of the traditional univariate approach. Under optimum microextraction conditions, the analytical features of the proposed DµSPE-LIBS methods were assessed, leading to limits of detection below 100 µg kg and 50 µg kg with the use of activated carbon and graphene oxide, respectively, as adsorbents in the DµSPE process. Trueness evaluation of the most sensitive procedure was carried out by spike and recovery experiments in a real sample of tap water, leading to recovery values in the range 98-110%.

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Dispersive Solid‐Phase Extraction

Cited by 47 publications

References 241 publications

Influence of Ligand Functionalization of UiO-66-Based Metal-Organic Frameworks When Used as Sorbents in Dispersive Solid-Phase Analytical Microextraction for Different Aqueous Organic Pollutants

Influence of Ligand Functionalization of UiO-66-Based Metal-Organic Frameworks When Used as Sorbents in Dispersive Solid-Phase Analytical Microextraction for Different Aqueous Organic Pollutants

Covalent Organic Frameworks in Sample Preparation

Dispersive micro solid-phase extraction (DµSPE) with graphene oxide as adsorbent for sensitive elemental analysis of aqueous samples by laser induced breakdown spectroscopy (LIBS)

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