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Separations
Special Issues
Sample Preparation and Chromatographic Analysis of Environmental Samples
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Sample Preparation and Chromatographic Analysis of Environmental Samples

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Chromatographic Separations".

Deadline for manuscript submissions: 10 April 2026 | Viewed by 6243

Special Issue Editors

Dr. Rosangela Elliani

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Guest Editor
Dipartimento di Chimica e Tecnologie Chimiche, Università della Calabria, Via P. Bucci Cubo 12/C, I-87030 Arcavacata di Rende, Italy
Interests: analytical methods development; sample preparation; microextraction techniques (SPME, MEPS, DPX); gas chromatography; mass spectrometry (MS and MS/MS); environmental and biological matrices; method validation; experimental design; green sample preparation
Special Issues, Collections and Topics in MDPI journals
Prof. Dr. Antonio Tagarelli

E-Mail Website
Guest Editor
Department of Chemistry and Chemical Technologies, University of Calabria, Arcavacata, Italy
Interests: sample preparation; microextraction techniques; gas chromatography; mass spectrometry; chemometrics; experimental design; derivatization; environmental analysis; analytical clinical chemistry
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

The introduction of innovative analytical techniques in the field of environmental science presents a significant challenge to the scientific community. The exposure of humans to organic compounds, as well as the quality of air and water, can be evaluated through the implementation of sensitive analytical protocols. Analytes of interest may include those used as plasticisers, flame retardants, or those originating from traffic emissions or the combustion of organic material.

As is well known, the development of analytical protocols is a process involving numerous steps. Among these, sample preparation represents a pivotal phase, as it directly impacts the overall efficacy and reliability of the method. The latest developments in analytical chemistry are focused on achieving reliable results, reducing sample handling, increasing productivity, eliminating or reducing the use of organic solvents, and automating processes.

The present Special Issue invites scientists to share their results, presented in the form of either a research article or a review, in the field of analytical method development. We particularly welcome protocols based on innovative sample preparation and chromatographic techniques for the assessment of several organic compounds in environmental samples. Moreover, other analytical methods with relevant impacts for the entire scientific community will be considered.

Dr. Rosangela Elliani
Prof. Dr. Antonio Tagarelli
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 250 words) can be sent to the Editorial Office for assessment.

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

  • assessment of several organic compounds
  • chromatography analysis
  • analytical parameters
  • multivariate optimization
  • sample extraction
  • enviromentally friendly analytical methods

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Published Papers (4 papers)

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Research

Jump to: Review

14 pages, 1523 KB  
Article
Composition- and Temperature-Dependent Solubility of Sinomenine Hydrochloride in Ethanol–Water Mixtures
by Yuxin Bian, Honggen Wu and Wenlong Li
Separations 2025, 12(12), 324; https://doi.org/10.3390/separations12120324 - 21 Nov 2025
Viewed by 279
Abstract
Sinomenine Hydrochloride is a bioactive alkaloid extracted from the root and stem of the medicinal plant sinomenium acutum, and is widely used to treat rheumatoid arthritis. Relevant studies were consulted, and the solubility data of Sinomenine Hydrochloride in ethanol–water mixed solvent have not [...] Read more.
Sinomenine Hydrochloride is a bioactive alkaloid extracted from the root and stem of the medicinal plant sinomenium acutum, and is widely used to treat rheumatoid arthritis. Relevant studies were consulted, and the solubility data of Sinomenine Hydrochloride in ethanol–water mixed solvent have not been reported. It is essential to choose a proper solvent in the process of crystallization that has a significant influence on the purity and productivity. Therefore, it is necessary to determine the solubility of Sinomenine Hydrochloride under the conditions of different ratios of ethanol–water mixed solvent and temperature. In this study, the solubility of Sinomenine Hydrochloride in ethanol–water mixed solvent was determined using high-performance liquid chromatography within the temperature range of 283.15 K–308.15 K. At the same time, the CNIBS/R-K model, Modified Apelblat model, Yaws model, and Apelblat–Jouyban–Acree model were used to fit the solubility data, and the relevant thermodynamic parameters were calculated using the Van’t Hoff model. The results showed that the solubility of Sinomenine Hydrochloride was higher in pure water than in pure ethanol. Moreover, with the increase in the mass fraction of ethanol in the mixed solvent, the solubility of Sinomenine Hydrochloride showed a trend of increasing first and then decreasing. When the ethanol–water ratio was 5:5, the solubility of the compound reached the maximum. In addition, experimental data showed that the solubility of Sinomenine Hydrochloride was affected by temperature. In the experimental temperature range, the solubility increased with the increase in temperature. Among these four solubility models, the CNIBS/R-K model had the best fitting effect; the maximum RAD and RMSD were 4.622 × 10−3 and 4.079 × 10−3, respectively. The thermodynamic model fitting results showed that the predicted values were in good agreement with the experimental data, and the thermodynamic parameters ΔHd, ΔSd, and ΔGd were all positive values. This indicated that the dissolution of Sinomenine Hydrochloride in the ethanol–water mixture was a non-spontaneous and endothermic process. A proper ratio of ethanol–water and temperature improved the solubility of Sinomenine Hydrochloride. The data determined in this study can provide basic data for the industrial purification of Sinomenine Hydrochloride. Full article
(This article belongs to the Special Issue Sample Preparation and Chromatographic Analysis of Environmental Samples)
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13 pages, 988 KB  
Article
Extraction, Isolation, and Purification of Furanocoumarins from Invasive Heracleum sosnowskyi
by Vida Vickackaite, Karina Pilaityte and Vilius Poskus
Separations 2025, 12(7), 175; https://doi.org/10.3390/separations12070175 - 1 Jul 2025
Cited by 1 | Viewed by 1586
Abstract
Heracleum sosnowskyi Manden. (Sosnowsky’s hogweed), originally introduced to Central and Eastern Europe as a fodder crop, has become a highly invasive species due to its ecological adaptability, high reproductive capacity, and efficient seed dispersal. Despite its negative impact on native flora and its [...] Read more.
Heracleum sosnowskyi Manden. (Sosnowsky’s hogweed), originally introduced to Central and Eastern Europe as a fodder crop, has become a highly invasive species due to its ecological adaptability, high reproductive capacity, and efficient seed dispersal. Despite its negative impact on native flora and its health risks to humans and animals, the species also represents a valuable source of biologically active compounds. In this study, we demonstrate that the leaves of H. sosnowskyi contain substantial amounts of furanocoumarins—phototoxic compounds with notable therapeutic potential, particularly as natural photosensitizers in anticancer therapies. To extract furanocoumarins from H. sosnowskyi, microwave-assisted extraction (MAE) was employed, with optimization of key parameters including extraction solvent (hexane), temperature (70 °C), extraction time (10 min), and solvent-to-solid ratio (20:1). Four major compounds—angelicin (2.3 mg/g), psoralen (0.15 mg/g), methoxsalen (0.76 mg/g), and bergapten (3.14 mg/g)—were identified and quantified using gas chromatography–mass spectrometry and gas chromatography with flame ionization detection. To purify the extract and selectively isolate the target compounds, a solid-phase extraction method was developed using a Strata Eco-Screen sorbent and stepwise elution with a hexane–acetone mixture. As a result, pure angelicin, pure methoxsalen, and various mixtures of the furanocoumarins were obtained. These findings highlight the potential of H. sosnowskyi as a sustainable source of furanocoumarins for pharmaceutical applications. Full article
(This article belongs to the Special Issue Sample Preparation and Chromatographic Analysis of Environmental Samples)
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Review

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24 pages, 1470 KB  
Review
Recent Trends in Solid-Phase Microextraction for the Monitoring of Drugs of Abuse in Wastewater
by Pedro Dinis, Eugenia Gallardo and Cláudia Margalho
Separations 2025, 12(9), 256; https://doi.org/10.3390/separations12090256 - 22 Sep 2025
Viewed by 1731
Abstract
Wastewater analysis plays a central role in monitoring patterns of drug use within specific populations. It provides objective and real-time estimates of consumption, with minimal ethical concerns. In the current European context, drugs of abuse continue to be detected in wastewater, with varying [...] Read more.
Wastewater analysis plays a central role in monitoring patterns of drug use within specific populations. It provides objective and real-time estimates of consumption, with minimal ethical concerns. In the current European context, drugs of abuse continue to be detected in wastewater, with varying incidences across countries. Their monitoring enables the prioritisation of public health and legal interventions by healthcare professionals and drug monitoring agencies. Therefore, the development and implementation of efficient methodologies for monitoring drugs of abuse in wastewater samples is of critical importance. This systematic review aims to explore the use of miniaturised sample extraction techniques based on solid-phase microextraction for the determination of drugs of abuse in wastewater. In fact, the extraction procedure must be fast, effective, and selective in order to retain the analytes of interest. Miniaturised techniques have thus emerged as promising alternatives to conventional methods. Magnetic solid-phase extraction (MSPE) and molecularly imprinted polymers (MIPs) represent the most widely applied solid-phase microextraction techniques in recent years for the analysis of drugs of abuse in wastewater. Looking ahead, future perspectives include the development of eco-friendly workflows, automated and time-efficient techniques, increasingly selective sorbents, and robust analytical methods. Full article
(This article belongs to the Special Issue Sample Preparation and Chromatographic Analysis of Environmental Samples)
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24 pages, 1664 KB  
Review
Microextraction and Eco-Friendly Techniques Applied to Solid Matrices Followed by Chromatographic Analysis
by Attilio Naccarato, Rosangela Elliani and Antonio Tagarelli
Separations 2025, 12(5), 124; https://doi.org/10.3390/separations12050124 - 14 May 2025
Cited by 5 | Viewed by 2003
Abstract
In this review, a 5-year overview on environmentally friendly approaches for the extraction of the most relevant organic pollutants in soil, sediment, particulate matter, and sewage sludge coupled with chromatographic analysis is reported. Organic contaminants encompass various compounds derived from personal care products, [...] Read more.
In this review, a 5-year overview on environmentally friendly approaches for the extraction of the most relevant organic pollutants in soil, sediment, particulate matter, and sewage sludge coupled with chromatographic analysis is reported. Organic contaminants encompass various compounds derived from personal care products, industrial chemicals, microplastics, organic matter combustion, agricultural practices, and plasticizer material. The principles of green analytical chemistry (GAC) and green sample preparation (GSP) serve as a guideline for the development of more environmentally sustainable analytical protocols. This study focuses attention on microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE), matrix solid-phase dispersion (MSPD), and microextraction techniques, such as solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE), hollow-fiber liquid-phase microextraction (HF-LPME), spray-assisted droplet formation-based liquid-phase microextraction (SADF-LPME), and dispersive liquid–liquid extraction (DLLME). These approaches represent the most relevant eco-friendly sample preparation for the advanced extraction of target analytes from environmental solid samples. Full article
(This article belongs to the Special Issue Sample Preparation and Chromatographic Analysis of Environmental Samples)
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