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Separations
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Advanced Separation Strategies and High Throughput in Analytical Sample Preparation
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Advanced Separation Strategies and High Throughput in Analytical Sample Preparation

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Materials in Separation Science".

Deadline for manuscript submissions: closed (10 March 2023) | Viewed by 7935

Special Issue Editors

Dr. María José Trujillo-Rodríguez

E-Mail Website
Guest Editor
Departamento de Química (Unidad Departamental de Química Analítica), Universidad de La Laguna (ULL), La Laguna, 38206 Tenerife, Spain
Interests: ionic liquids; polymers; polymeric ionic liquids; analytical sample preparation; solid-phase microextraction; liquid-phase microextraction; chromatography; green analytical methods; environmental analysis; bioanalysis; food analysis
Prof. Dr. Verónica Pino

E-Mail Website
Guest Editor
Laboratorio de Materiales para Análisis Químicos (MAT4LL), Departamento de Química, Unidad Departamental de Química Analítica, Facultad de Ciencias, Universidad de La Laguna, Avda. Astrofísico Francisco Sánchez s/n, 38200 La Laguna, Tenerife, Spain
Interests: microextraction methods; miniaturized analytical sample preparation; ionic liquids and derivatives; metal-organic frameworks; environmental analysis
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Analytical applications often require different steps of separation, purification, extraction, clean-up, and/or preconcentration prior the analytical determination. These protocols are mandatory to ensure adequate sensitivity, interference elimination, and even compatibility with the subsequent analytical technique selected. Traditional analytical sample preparation approaches are time consuming, indeed being considered the bottleneck of the analytical method. This aspect is detrimental for their implementation in environmental quality, food technologies, and bioclinical laboratories, where a fast result is required for taking decisions/actions related to the sample analyzed. Apart of these significant drawbacks, these traditional approaches require highly specialized personnel and consume high amounts of solvents.

This Special Issue aims to highlight innovative and smarter analytical sample preparation strategies developed to be cost-effective, simpler, and more sustainable alternatives than conventional approaches. In particular, the issue focuses on microextraction and miniaturized methods using new extraction materials, greener strategies, parallel extraction, flow injection, or automation.

This Special Issue will significantly impact the research community and encourage colleagues to contribute with original research articles or reviews.

Dr. María José Trujillo-Rodríguez
Dr. Verónica Pino
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Separations is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2600 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • ionic liquids
  • polymers
  • nanomaterials
  • metal–organic frameworks
  • novel solvents
  • microextraction
  • miniaturization
  • green methods
  • automation
  • parallel extraction

Published Papers (4 papers)

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Research

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12 pages, 1248 KiB  
Article
Hydrophobic Natural Eutectic Solvents for the Gas Chromatographic Determination of Suspected Allergens in Fragrances by Dispersive Liquid-Liquid Microextraction
by Gaia Bechis, Giulia Mastellone, Arianna Marengo, Barbara Sgorbini, Cecilia Cagliero and Patrizia Rubiolo
Separations 2022, 9(10), 318; https://doi.org/10.3390/separations9100318 - 19 Oct 2022
Viewed by 1406
Abstract
The fragrance industry plays a key role in the global economy, producing a wide range of personal care and household products. However, some fragrance ingredients have been linked to allergic reactions in sensitive people, and their concentrations are regulated at the European level. [...] Read more.
The fragrance industry plays a key role in the global economy, producing a wide range of personal care and household products. However, some fragrance ingredients have been linked to allergic reactions in sensitive people, and their concentrations are regulated at the European level. For this reason, reliable, rapid, and sustainable analytical methods are needed to rapidly detect and quantify these compounds. Recently, a new class of hydrophobic eutectic solvents (HES) has been introduced; they consist of natural terpenoids or phenolic compounds that can be used as hydrogen bond donors (HBD) and acceptors (HBA), and they are more suitable for GC applications due to their higher volatility. In this study, a dispersive liquid–liquid microextraction (DLLME) approach is proposed for the analysis and quantification of a range of allergens in hydroalcoholic perfumes. The optimized method requires only 50 µL of a natural HES (thymol–eugenol), which is readily dispersed by vortexing in 2 mL of sample. After centrifugation, the HES rich phase is diluted in 400 µL EtOH and directly injected into the GC-FID system. The proposed method has been successfully applied in the analysis and quantification of commercial fragrances, demonstrating good enrichment of target allergens and suitability for aqueous matrices analysis. Full article
(This article belongs to the Special Issue Advanced Separation Strategies and High Throughput in Analytical Sample Preparation)
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12 pages, 1425 KiB  
Article
Disposable Pipette Extraction (DPX) Coupled to HPLC-DAD as an Alternative for the Determination of Phthalic Monoesters in Urine Samples
by Heloisa Comelli, Camila Will, Lucas Morés, Gabrieli Bernardi and Eduardo Carasek
Separations 2022, 9(10), 294; https://doi.org/10.3390/separations9100294 - 07 Oct 2022
Cited by 1 | Viewed by 1243
Abstract
Phthalates are widely used in industry, but adverse effects on human health have been reported due to exposure to these chemicals. In the human body, they are metabolized into phthalic monoesters, which are used to monitor human exposure and assess risk. Urine is [...] Read more.
Phthalates are widely used in industry, but adverse effects on human health have been reported due to exposure to these chemicals. In the human body, they are metabolized into phthalic monoesters, which are used to monitor human exposure and assess risk. Urine is one of the main biological samples used, due to its easy access and collection, and also being the main elimination pathway for phthalates. Urine samples are complex; therefore, sample preparation is a critical step. Disposable pipette extraction (DPX) has not previously been reported for quantifying phthalates in urine and is here presented as a fast and low sample consumption method. A fully optimized RP-DPX method was developed for determination of free monomethyl phthalate, monobutyl phthalate, monobenzyl phthalate, and monoethylhexyl phthalate from urine samples. Analytical parameters of merit were obtained. The values of R2 were ≥0.9832, and the LOD and LOQ varied from 3.0 to 7.6 μg L−1 and 10 to 25 μg L−1, respectively. Intraday (n = 3) and interday (n = 9) precision were ≤13.6 and 15.6%. The accuracy, as relative recovery, presented a range from 83 to 120%. The method was robust after performing the Youden test. Compared to other methods, this work stands out due to its short extraction time and sample consumption. Full article
(This article belongs to the Special Issue Advanced Separation Strategies and High Throughput in Analytical Sample Preparation)
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14 pages, 2641 KiB  
Article
Validation of an Analytical Method for the Determination of Manganese and Lead in Human Hair and Nails Using Graphite Furnace Atomic Absorption Spectrometry
by José Ricardo Forero-Mendieta, Juan David Varón-Calderón, Diana Angelica Varela-Martínez, Diego Alejandro Riaño-Herrera, Rubén Darío Acosta-Velásquez and John Alexander Benavides-Piracón
Separations 2022, 9(7), 158; https://doi.org/10.3390/separations9070158 - 23 Jun 2022
Cited by 4 | Viewed by 2969
Abstract
This article describes the validation of analytical methods for the determination of Manganese (Mn) and lead (Pb) by graphite furnace atomic absorption spectrometry (GFAAS) in human hair and nail samples. Method validation parameters such as linearity, repeatability, reproducibility, and precision were determined. In [...] Read more.
This article describes the validation of analytical methods for the determination of Manganese (Mn) and lead (Pb) by graphite furnace atomic absorption spectrometry (GFAAS) in human hair and nail samples. Method validation parameters such as linearity, repeatability, reproducibility, and precision were determined. In addition, the limit of detection (LOD), the limit of quantification (LOQ), and measurement uncertainty were calculated. The developed method was linear in the concentration ranges of 0.001–0.015 and 0.002–0.020 µg·L−1 of Mn and Pb, respectively. The determination coefficients obtained were greater than 0.995. The recoveries obtained after the addition of the standard concentration for the metals ranged from 84.80–107.98%, with a precision not exceeding 12.97% relative standard deviation. The calculated LOD and LOQ for Mn and Pb are within the ranges established by Commission Regulation (EU) No. 836/2011. The expanded uncertainty was estimated to be less than 9.93–6.59% for Mn and Pb. Matrix effects were also studied, finding a smooth effect in both matrices. The analysis of 30 samples of each type revealed the presence of Mn in 30 and Pb in 13 samples. Overall, the proposed validation method was considered optimal for the determination of Mn and Pb. Full article
(This article belongs to the Special Issue Advanced Separation Strategies and High Throughput in Analytical Sample Preparation)
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Review

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19 pages, 2628 KiB  
Review
In-Tube Solid-Phase Microextraction Directly Coupled to Mass Spectrometric Systems: A Review
by Caroline Fernandes Grecco, Israel Donizeti de Souza, Igor Gustavo Carvalho Oliveira and Maria Eugênia Costa Queiroz
Separations 2022, 9(12), 394; https://doi.org/10.3390/separations9120394 - 26 Nov 2022
Cited by 6 | Viewed by 1532
Abstract
Since it was introduced in 1997, in-tube solid-phase microextraction (in-tube SPME), which uses a capillary column as extraction device, has been continuously developed as online microextraction coupled to LC systems (in-tube SPME-LC). In the last decade, new couplings have been evaluated on the [...] Read more.
Since it was introduced in 1997, in-tube solid-phase microextraction (in-tube SPME), which uses a capillary column as extraction device, has been continuously developed as online microextraction coupled to LC systems (in-tube SPME-LC). In the last decade, new couplings have been evaluated on the basis of state-of-the-art LC instruments, including direct coupling of in-tube SPME to MS/MS systems, without chromatographic separation, for high-throughput analysis. In-tube SPME coupling to MS/MS has been possible thanks to the selectivity of capillary column coatings and MS/MS systems (SRM mode). Different types of capillary columns (wall-coated open-tubular, porous-layer open-tubular, sorbent-packed, porous monolithic rods, or fiber-packed) with selective stationary phases have been developed to increase the sorption capacity and selectivity of in-tube SPME. This review focuses on the in-tube SPME principle, extraction configurations, current advances in direct coupling to MS/MS systems, experimental parameters, coatings, and applications in different areas (food, biological, clinical, and environmental areas) over the last years. Full article
(This article belongs to the Special Issue Advanced Separation Strategies and High Throughput in Analytical Sample Preparation)
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