Feature Papers in Analytica

A special issue of Analytica (ISSN 2673-4532).

Deadline for manuscript submissions: closed (31 July 2025) | Viewed by 26429

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Department of Pharmacy, University of G. d'Annunzio Chieti and Pescara, Chieti, Italy
Interests: innovative (micro) extraction procedures (MEPS, FPSE, DLLME, SULLE, MAE, etc.) and hyphenated instrument configurations; bioactive compounds (drugs, drugs associations, and natural bioactive compounds); characterization, fingerprints, and method validation; HPLC; mass spectrometry (MS and MS/MS)
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Special Issue Information

Dear Colleagues,

We are pleased to announce this new Special Issue on “Feature Papers in Analytica”. This Special Issue is devoted to publishing high-quality articles that describe the most significant and cutting-edge research in all areas that fit the scope of the journal.

The Special Issue publishes articles on all aspects of fundamental and applied analytical chemistry. The scope includes chromatography (GC, HPLC, UPLC, SFE, HPTLC, GC x GC, LC x LC), hyphenated instrument configurations (e.g., LC-MS) and new devices, sample pretreatment and extraction, electroanalysis (voltammetry, polarography), sensors (chemosensors and biosensors), spectroscopy (chemi- and bio-luminescence, fluorescence, UV/Vis, NMR, IR, MS, atomic and molecular spectroscopy, absorption and emission spectroscopy), thermal analysis, and chemometrics.

Accepted papers can cover the various application fields of analytical chemistry such as environmental, biological, clinical/pharmaceutical, -omics (proteomics, metabolomics), forensic, and industrial (quality control). We have no limitations on the paper types. Papers describing the challenges and added value of interdisciplinary work are also welcome.

Dr. Marcello Locatelli
Guest Editor

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Keywords

  • green chemistry (GC)
  • green analytical chemistry (GAC)
  • green sample preparation (GSP)
  • circular analytical chemistry (CAC)
  • instrumental analysis
  • innovative configurations
  • multidimensional analysis
  • quantitative analysis
  • complex matrices
  • chemometrics

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Published Papers (9 papers)

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Research

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16 pages, 856 KB  
Article
Investigation of Halloumi Cheese Adulteration Due to the Addition of Milk Powder Using BET and FTIR Measurements
by Maria Tarapoulouzi, Małgorzata Ruggiero-Mikołajczyk, Ioannis Pashalidis and Charis R. Theocharis
Analytica 2025, 6(3), 34; https://doi.org/10.3390/analytica6030034 - 8 Sep 2025
Viewed by 489
Abstract
Halloumi cheese, a traditional Cypriot dairy product with Protected Designation of Origin (PDO) status, is renowned for its unique texture and high melting point. PDO certification is crucial for Halloumi cheese as it ensures the product’s authenticity, protects its traditional production methods and [...] Read more.
Halloumi cheese, a traditional Cypriot dairy product with Protected Designation of Origin (PDO) status, is renowned for its unique texture and high melting point. PDO certification is crucial for Halloumi cheese as it ensures the product’s authenticity, protects its traditional production methods and geographical origin, and safeguards consumers and producers against fraud and mislabeling. However, concerns over adulteration, particularly through the addition of skim milk powder, pose challenges to its authenticity and quality control. This study is the first to analyze Halloumi cheese using Brunauer–Emmett–Teller (BET) analysis and Fourier Transform Infrared (FTIR) spectroscopy, providing a novel approach to assessing its composition and authenticity. Furthermore, it marks the first time Halloumi samples have been examined in the context of PDO certification. Alongside PDO-certified Halloumi, two additional sample sets were produced following PDO specifications for moisture, fat, and salt content, with the controlled incorporation of skim milk powder as an adulterant at concentrations of 1% and 5%. Principal component analysis (PCA) was employed to visualize and interpret the spectral data, revealing promising results. Chemometric analysis showed that the specific surface area from BET measurements and the FTIR spectral subregion between 1650 and 1100 cm−1 were key factors, and they were retained for model construction. These findings could play a crucial role in establishing official food fraud detection methodologies, particularly for the Cyprus and EU markets. While this study serves as an initial investigation, additional samples will be tested in future studies to validate these preliminary results and to assess the potential of applying these techniques in real-world food fraud detection scenarios. Full article
(This article belongs to the Special Issue Feature Papers in Analytica)
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18 pages, 1379 KB  
Article
Rapid and Efficient Magnetic Nanoparticle-Based Method for Cd Determination in Brazilian Cachaça Using Flame Atomic Absorption Spectrometry
by Saulo Alves de Souza, Cristiane dos Reis Feliciano, Grazielle Cabral de Lima, Ítalo Agnis da Silva Gomes, Nathália Carvalho Costa, Bruno Alves Rocha and Mariane Gonçalves Santos
Analytica 2025, 6(3), 33; https://doi.org/10.3390/analytica6030033 - 8 Sep 2025
Viewed by 505
Abstract
The contamination of food and beverages with heavy metals, such as Cd, presents significant health risks, underscoring the need for reliable and sensitive analytical methods. This study introduces the development of a rapid, cost-effective, and environmentally friendly method for Cd determination in cachaça, [...] Read more.
The contamination of food and beverages with heavy metals, such as Cd, presents significant health risks, underscoring the need for reliable and sensitive analytical methods. This study introduces the development of a rapid, cost-effective, and environmentally friendly method for Cd determination in cachaça, a traditional Brazilian sugarcane spirit. Magnetic nanoparticles (Fe3O4) functionalized with tetraethyl orthosilicate are synthesized and employed as adsorbents in a dispersive magnetic solid-phase extraction procedure. The extracted Cd is quantified using flame atomic absorption spectrometry. A full factorial experimental design is used to optimize key parameters, including the sorbent mass, adsorption time, desorption time, and acid concentration. The method demonstrates excellent analytical performance, with a linear calibration range (R2 = 0.99), detection limit of 0.0046 mg L−1, and quantification limit of 0.0200 mg L−1. Moreover, validation results show high precision (coefficient of variation < 9.10%) and accuracy (recovery rates between 92.00% and 120.00%). When analyzing commercial cachaça samples, cadmium was detected in all five specimens. Notably, in one sample the cadmium concentration exceeded Brazil’s maximum permissible limit of 0.0200 mg kg−1, underscoring the importance of this work for ensuring food safety. The proposed method offers a sensitive, reproducible, and sustainable approach for analysis of potentially toxic trace metals in alcoholic beverages, reinforcing its potential for routine monitoring and regulatory compliance. Full article
(This article belongs to the Special Issue Feature Papers in Analytica)
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17 pages, 10934 KB  
Article
Chemical, Diagnostic, and Instrumental Analysis of an Ancient Roman Cippus funebris from the First Century AD
by Mauro Castrucci, Mauro Tomassetti, Emanuele Dell’Aglio, Giovanni Visco, Maria Pia Sammartino and Marco Castracane
Analytica 2025, 6(1), 11; https://doi.org/10.3390/analytica6010011 - 13 Mar 2025
Viewed by 1434
Abstract
A diagnostic chemical analysis has been performed on a Roman Cippus funebris in precious white marble located close to an ancient Roman road. The Cippus was in good condition but almost completely covered by a black patina, requiring a conservative cleaning intervention. The [...] Read more.
A diagnostic chemical analysis has been performed on a Roman Cippus funebris in precious white marble located close to an ancient Roman road. The Cippus was in good condition but almost completely covered by a black patina, requiring a conservative cleaning intervention. The restorer in charge of the restoration asked us to make a preliminary diagnosis, on the basis of which we could suggest the most appropriate intervention. The Cippus was dedicated to the young Quintus Cornelius Proclianus, who died at the age of 15, by his mother Valeria Calpurnia Scopele. It perfectly fits into the Roman funerary liturgy and also shows an Etruscan-type iconography that seems to confirm the Etruscan Gens of the family and its dating to the 1st century AD. Ion chromatography (IC) analyses were performed to determine anions and cations on solutions obtained from the extraction of salts from the four samples of the Cippus. pH, conductivity, and red-ox potential measures, as well as UV-visible spectra were carried out on the same solutions. A small fragment, spontaneously fallen from the Cippus’ surface, was also observed by optical microscopy (OM) and scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS). From the analyses, the dark patina that covered the surface before cleaning turned out to be made of black crusts, that is, smog particles adsorbed on sulfates, but above all, by a layer of microflora. The results allowed us to suggest some conservative interventions. Full article
(This article belongs to the Special Issue Feature Papers in Analytica)
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12 pages, 1626 KB  
Article
Odor Dilution Assessment for Explosive Detection
by Dillon E. Huff, Ariela Cantu, Sarah A. Kane, Lauren S. Fernandez, Jaclyn E. Cañas-Carrell, Nathaniel J. Hall and Paola A. Prada-Tiedemann
Analytica 2024, 5(3), 402-413; https://doi.org/10.3390/analytica5030025 - 9 Aug 2024
Viewed by 2831
Abstract
Canine olfaction is a highly developed sense and is utilized for the benefit of detection applications, ranging from medical diagnostics to homeland security and defense prevention strategies. Instrumental validation of odor delivery methods is key to standardize canine olfaction research to establish baseline [...] Read more.
Canine olfaction is a highly developed sense and is utilized for the benefit of detection applications, ranging from medical diagnostics to homeland security and defense prevention strategies. Instrumental validation of odor delivery methods is key to standardize canine olfaction research to establish baseline data for explosive detection applications. Solid-phase microextraction gas chromatography (SPME/GC-MS) was used to validate the odor delivery of an olfactometer. Three explosive classes were used in this study: composition C-4 (C-4), trinitrotoluene (TNT), and ammonium nitrate (AN). Dynamic airflow sampling yielded the successful detection of previously reported target volatile organic compounds (VOCs): 2,3-dimethyl-2,3-dinitrobutane (DMNB) in C-4 and 2-ethylhexan-1-ol (2E1H) in ammonium nitrate and TNT across odor dilutions of 80%, 50%, 25%, 12%, and 3%. C-4 highlighted the most reliable detection from the olfactometer device, depicting a response decrease as a function of dilution factor of its key odor volatile DMNB across the entire range tested. TNT only portrayed 2-ethylhexan-1-ol as a detected odor volatile with a detection response as a function of dilution from 80% down to 12%. Comparatively, ammonium nitrate also depicted 2-ethylhexan-1-ol as an odor volatile in the dynamic airflow sampling but with detection only within the upper scale of the dilution range (80% and 50%). The results suggest the importance of monitoring odor delivery across different dilution ranges to provide quality control for explosive odor detection using dynamic airflow systems. Full article
(This article belongs to the Special Issue Feature Papers in Analytica)
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26 pages, 709 KB  
Article
Analytical Applications of Voltammetry in the Determination of Heavy Metals in Soils, Plant Tissues, and Water—Prospects and Limitations in the Co-Identification of Metal Cations in Environmental Samples
by Efthymia Chatziathanasiou, Vasiliki Liava, Evangelia E. Golia and Stella Girousi
Analytica 2024, 5(3), 358-383; https://doi.org/10.3390/analytica5030023 - 2 Aug 2024
Cited by 7 | Viewed by 5267
Abstract
Heavy metals represent a class of chemical elements that includes metalloids, bases and transition metals, lanthanides, and actinides. They are distinguished for their toxicity in small concentrations and their negative effects on the environment and human health; consequently, their monitoring has to be [...] Read more.
Heavy metals represent a class of chemical elements that includes metalloids, bases and transition metals, lanthanides, and actinides. They are distinguished for their toxicity in small concentrations and their negative effects on the environment and human health; consequently, their monitoring has to be improved to manage the risks. The determination of heavy metals is carried out mainly by analytical methods, using spectroscopy, spectrometry, and electroanalysis. However, the interest has shifted to new and faster methodologies and techniques for heavy metal analysis, with particular emphasis on voltammetry. Voltammetry is preferred for heavy metal detection owing to the advantages of low cost, simplicity, ease of operation, fast analysis, portability, the ability to monitor environmental samples in the field, and high sensitivity and selectivity. Therefore, this study summarizes the applications of voltammetry in heavy metal determination mainly in water, soil, and plant samples, and presents an evaluation of sensitivity, selectivity, and applicability. Full article
(This article belongs to the Special Issue Feature Papers in Analytica)
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Review

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15 pages, 4519 KB  
Review
Microcrystal Delivery Using a Syringe and Syringe Pump Method for Serial Crystallography
by Ki Hyun Nam
Analytica 2025, 6(1), 5; https://doi.org/10.3390/analytica6010005 - 16 Feb 2025
Cited by 1 | Viewed by 1873
Abstract
Serial crystallography (SX) determines the crystal structures of target molecules at room temperature with minimal radiation damage. During SX data collection, the stable delivery of many microcrystals to the X-ray interaction point is crucial for efficient sample consumption and effective beamtime usage. Most [...] Read more.
Serial crystallography (SX) determines the crystal structures of target molecules at room temperature with minimal radiation damage. During SX data collection, the stable delivery of many microcrystals to the X-ray interaction point is crucial for efficient sample consumption and effective beamtime usage. Most microcrystal delivery techniques for SX require sophisticated devices or specialized techniques, which can be challenging for data collection. This review introduces a straightforward method that delivers microcrystal samples in SX experiments using a commercially available syringe and syringe pump. This method does not require specialized skills for sample delivery and can be tested in the laboratory prior to SX data collection at the beamline. Advantages and disadvantages of this method are also discussed, along with various application cases. This straightforward sample delivery approach is concluded to facilitate efficient SX data collection. Full article
(This article belongs to the Special Issue Feature Papers in Analytica)
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20 pages, 1369 KB  
Review
Boron Nitride Nanostructures (BNNs) Within Metal–Organic Frameworks (MOFs): Electrochemical Platform for Hydrogen Sensing and Storage
by Azizah Alamro and Thanih Balbaied
Analytica 2024, 5(4), 599-618; https://doi.org/10.3390/analytica5040040 - 30 Nov 2024
Cited by 3 | Viewed by 2943
Abstract
Boron nitride nanostructures (BNNs), including nanotubes, nanosheets, and nanoribbons, are renowned for their exceptional thermal stability, chemical inertness, mechanical strength, and high surface area, making them suitable for advanced material applications. Metal–organic frameworks (MOFs), characterized by their porous crystalline structures, high surface area, [...] Read more.
Boron nitride nanostructures (BNNs), including nanotubes, nanosheets, and nanoribbons, are renowned for their exceptional thermal stability, chemical inertness, mechanical strength, and high surface area, making them suitable for advanced material applications. Metal–organic frameworks (MOFs), characterized by their porous crystalline structures, high surface area, and tunable porosity, have emerged as excellent candidates for gas adsorption and storage applications, particularly in the context of hydrogen. This paper explores the synthesis and properties of BNNs and MOFs, alongside the innovative approach of integrating BNNs within MOFs to create composite materials with synergistic properties. The integration of BNNs into MOFs enhances the overall thermal and chemical stability of the composite while improving hydrogen sensing and storage performance. Various synthesis methods for both BNNs and MOFs are discussed, including chemical vapor deposition, solvothermal synthesis, and in situ growth, with a focus on their scalability and reproducibility. Furthermore, the mechanisms underlying hydrogen sensing and storage are examined, including physisorption, chemisorption, charge transfer, and work function modulation. Electrochemical characterization techniques, such as cyclic voltammetry, electrochemical impedance spectroscopy, and galvanostatic charge–discharge, are used to analyze the performance of BNN-MOF systems in hydrogen storage and sensing applications. These methods offer insights into the material’s electrochemical behavior and its potential to store hydrogen efficiently. Potential industrial applications of BNN-MOF composites are highlighted, particularly in fuel cells, hydrogen-powered vehicles, safety monitoring in hydrogen production and distribution networks, and energy storage devices. The integration of these materials can contribute significantly to the development of more efficient hydrogen energy systems. Finally, this study outlines key recommendations for future research, which include optimizing synthesis techniques, improving the hydrogen interaction mechanisms, enhancing the stability and durability of BNN-MOF composites, and performing comprehensive economic and environmental assessments. BNN-MOF composites represent a promising direction in the advancement of hydrogen sensing and storage technologies, offering significant potential to support the transition toward sustainable energy systems and hydrogen-based economies. Full article
(This article belongs to the Special Issue Feature Papers in Analytica)
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24 pages, 3186 KB  
Review
3D-Printed Electrochemical Sensors: A Comprehensive Review of Clinical Analysis Applications
by Thaís Cristina de Oliveira Cândido, Daniela Nunes da Silva, Marcella Matos Cordeiro Borges, Thiago Gabry Barbosa, Scarlat Ohanna Dávila da Trindade and Arnaldo César Pereira
Analytica 2024, 5(4), 552-575; https://doi.org/10.3390/analytica5040037 - 11 Nov 2024
Cited by 12 | Viewed by 4290
Abstract
Three-dimensional printing technology has emerged as a versatile and cost-effective alternative for the fabrication of electrochemical sensors. To enhance sensor sensitivity and biocompatibility, a diverse range of biocompatible and conductive materials can be employed in these devices. This allows these sensors to be [...] Read more.
Three-dimensional printing technology has emerged as a versatile and cost-effective alternative for the fabrication of electrochemical sensors. To enhance sensor sensitivity and biocompatibility, a diverse range of biocompatible and conductive materials can be employed in these devices. This allows these sensors to be modified to detect a wide range of analytes in various fields. 3D-printed electrochemical sensors have the potential to play a pivotal role in personalized medicine by enabling the real-time monitoring of metabolite and biomarker levels. These data can be used to personalize treatment strategies and optimize patient outcomes. The portability and low-cost nature of 3D-printed electrochemical sensors make them suitable for point-of-care (POC) diagnostics. These tests enable rapid and decentralized analyses, aiding in diagnosis and treatment decisions in resource-limited settings. Among the techniques widely reported in the literature for 3D printing, the fused deposition modeling (FDM) technique is the most commonly used for the development of electrochemical devices due to the easy accessibility of equipment and materials. Focusing on the FDM technique, this review explores the critical factors influencing the fabrication of electrochemical sensors and discusses potential applications in clinical analysis, while acknowledging the challenges that need to be overcome for its effective adoption. Full article
(This article belongs to the Special Issue Feature Papers in Analytica)
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26 pages, 949 KB  
Review
Recent Advances in Monitoring Microbial Toxins in Food Samples by HPLC-Based Techniques: A Review
by Gabriela Elizabeth Quintanilla-Villanueva, Araceli Sánchez-Álvarez, Raisa Estefanía Núñez-Salas, Melissa Marlene Rodríguez-Delgado, Donato Luna-Moreno and Juan Francisco Villarreal-Chiu
Analytica 2024, 5(4), 512-537; https://doi.org/10.3390/analytica5040035 - 11 Oct 2024
Cited by 4 | Viewed by 4529
Abstract
This study examines the significant impact of bacterial, algal, and fungal toxins on foodborne illnesses, and stresses the importance of advanced detection techniques, such as high-performance liquid chromatography (HPLC)-based methodologies. It emphasizes the urgent need for further advancements in these techniques to ensure [...] Read more.
This study examines the significant impact of bacterial, algal, and fungal toxins on foodborne illnesses, and stresses the importance of advanced detection techniques, such as high-performance liquid chromatography (HPLC)-based methodologies. It emphasizes the urgent need for further advancements in these techniques to ensure food safety, as they offer significant benefits, including low detection limits and the ability to be combined with other techniques to detect a wide range of toxins. In this regard, HPLC has emerged as a versatile and sensitive analytical technique for this purpose. Various HPLC methods, often enhanced with detectors such as ultraviolet (UV), fluorescence (FD), and mass spectrometry (MS), have been developed to identify and quantify microbial toxins in a wide variety of food samples. Recent advancements include HPLC-FD methods that utilize the natural fluorescence of certain aflatoxins, improving detection sensitivity. HPLC-MS/MS and UHPLC-MS/MS techniques offer high selectivity and sensitivity, making them suitable for detecting a wide range of toxins in trace quantities. The adaptability of HPLC, combined with innovative detection technologies and sample preparation methods, holds significant potential for enhancing food safety monitoring and reducing the global burden of foodborne diseases. Full article
(This article belongs to the Special Issue Feature Papers in Analytica)
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