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Extraction Techniques for Sample Preparation

A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: 31 July 2026 | Viewed by 1517

Special Issue Editors


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Guest Editor
Department of Pharmacy, University “G. d’Annunzio” of Chieti-Pescara, I-66100 Chieti, Italy
Interests: HPLC/UHPLC; sample preparation; LC-MS separations; gas chromatography; solid-phase extraction
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Guest Editor Assistant
Department of Pharmacy, University “G. d’Annunzio” of Chieti-Pescara, I-66100 Chieti, Italy
Interests: nanostructured materials; drug delivery; energy storage; CO2 capture; electrospinning; material characterization; sustainable technologies
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Sample preparation has long been recognized as the bottleneck in the analytical process, estimated to account for 70% of the overall chemical analysis. Errors introduced during this phase of chemical analysis can irreparably compromise the results. The scientific community has continually sought to improve sample preparation by developing increasingly advanced techniques aimed at maximizing recovery and eliminating interferences that could adversely impact the analysis. Currently, sample preparation techniques can be categorized into three categories: sorbent-based techniques, organic solvent-based techniques, and techniques based on the use of supercritical or subcritical fluids. In the past decade, the miniaturization of these techniques has gained significant attention from the scientific community, along with the development of nanocomposite materials and next-generation solvents. Sample preparation techniques are frequently coupled with instrumental methodologies for the determination and quantitation of analytes, such as high-performance liquid chromatography (HPLC) or gas chromatography (GC), both of which can be paired with standard detectors or mass spectrometry (MS). This Special Issue aims to highlight sample preparation techniques that can be effectively applied in the extraction or micro-extraction of analytes from various matrices and their determination through instrumental methods or sensor-based approaches.

Dr. Vincenzo Ferrone
Guest Editor

Dr. Pantaleone Bruni
Guest Editor Assistant

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Keywords

  • sorbent-based extraction
  • liquid-based extraction
  • supercritical- or subcritical-based extraction
  • HPLC determination
  • GC determination
  • LC-MS-based analysis
  • chemical fingerprinting

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Published Papers (2 papers)

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Research

14 pages, 954 KB  
Article
Solid Phase Extraction and Determination of Tetracycline Using Gold Nanoparticles Stabilized in a Polymethacrylate Matrix
by Nadezhda V. Saranchina, Daria E. Kuznetsova, Nataliya A. Gavrilenko and Mikhail A. Gavrilenko
Molecules 2025, 30(22), 4458; https://doi.org/10.3390/molecules30224458 - 19 Nov 2025
Abstract
A polymethacrylate matrix (PMM) is proposed for the solid-phase extraction and determination of tetracycline (TC). The study of the influence of medium acidity, temperature, and contact time on the extraction of tetracycline by PMM showed that tetracycline is extracted by the matrix in [...] Read more.
A polymethacrylate matrix (PMM) is proposed for the solid-phase extraction and determination of tetracycline (TC). The study of the influence of medium acidity, temperature, and contact time on the extraction of tetracycline by PMM showed that tetracycline is extracted by the matrix in the form of a singly charged anion H2TC, within the pH range of 8.9–9.7, with distribution coefficients reaching (5–6) × 103 mL/g. Following the extraction process using PMM and PMM-Au0, the direct determination of tetracycline in the solid phase is possible without an elution step. This is achieved by using as the analytical signal both the intrinsic absorption and the instrumentally measured peak area of the anionic form of tetracycline, H2TC, in the matrix, with detection limits of 0.03 and 0.01 mg/L, respectively, and the fluorescence of tetracycline in PMM and PMM-Au0, with detection limits of 0.001 and 0.005 mg/L, respectively. The applicability of the digital colorimetry method for the quantitative determination of tetracycline based on its fluorescence in the solid phase is demonstrated. Methodologies for the determination of tetracycline using PMM and PMM-Au0 were developed and tested in the analysis of river and bottled water samples, biological fluid, as well as honey and milk samples. Full article
(This article belongs to the Special Issue Extraction Techniques for Sample Preparation)
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21 pages, 1599 KB  
Article
Development and Validation of HPLC-DAD/FLD Methods for the Determination of Vitamins B1, B2, and B6 in Pharmaceutical Gummies and Gastrointestinal Fluids—In Vitro Digestion Studies in Different Nutritional Habits
by Georgios Kamaris, Nikoletta Pantoudi and Catherine K. Markopoulou
Molecules 2025, 30(19), 3902; https://doi.org/10.3390/molecules30193902 - 26 Sep 2025
Viewed by 1181
Abstract
Two HPLC-based analytical methods, one with DAD and the other with an FLD detector, were developed and validated for the simultaneous analysis of B1, B2, and B6 vitamins, both in pharmaceutical gummies and in gastric and intestinal fluids [...] Read more.
Two HPLC-based analytical methods, one with DAD and the other with an FLD detector, were developed and validated for the simultaneous analysis of B1, B2, and B6 vitamins, both in pharmaceutical gummies and in gastric and intestinal fluids (with water or milk or orange juice). For the detection of B1 by fluorometry, a pre-column oxidation/derivatization process was accomplished in the presence of B2 and B6 vitamins. The methods were performed on an Aqua column (250 mm × 4.6 mm, 5 mm) at 40 °C, with isocratic elution (70% NaH2PO4 buffer pH 4.95 and 30% methanol) and a flow rate of 0.9 mL/min. Both were validated according to ICH specifications in terms of linearity (R2 > 0.999), accuracy (% Mean Recovery 100 ± 3%) and precision (%RSD < 3.23). For the analysis of the samples, a stability study (in diluents, pH and fluids) was conducted, while for their purification two different extraction procedures, a liquid/solid for the gummies (%Recovery > 99.8%) and a Solid Phase Extraction (SPE) for the Gastrointestinal (G.I.) fluids, (%Recovery 100 ± 5%) were developed. Finally, to investigate whether the co-administration of B-complex with water, orange juice or milk plays a significant role in their release from gummies, a three-phase in vitro digestion protocol was applied. The results did not show significant differences with a slight superiority in the release of B2 and B6 with water, while B1 with orange juice. Full article
(This article belongs to the Special Issue Extraction Techniques for Sample Preparation)
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