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Analytica, Volume 6, Issue 4 (December 2025) – 4 articles

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18 pages, 1138 KB  
Review
Determination of Inorganic Elements in Paper Food Packaging Using Conventional Techniques and in Various Matrices Using Microwave Plasma Atomic Emission Spectrometry (MP-AES): A Review
by Maxime Chivaley, Samia Bassim, Vicmary Vargas, Didier Lartigue, Brice Bouyssiere and Florence Pannier
Analytica 2025, 6(4), 41; https://doi.org/10.3390/analytica6040041 - 9 Oct 2025
Viewed by 318
Abstract
As one of the world’s most widely used packaging materials, paper obtains its properties from its major component: wood. Variations in the species of wood result in variations in the paper’s mechanical properties. The pulp and paper production industry is known to be [...] Read more.
As one of the world’s most widely used packaging materials, paper obtains its properties from its major component: wood. Variations in the species of wood result in variations in the paper’s mechanical properties. The pulp and paper production industry is known to be a polluting industry and a consumer of a large amount of energy but remains an essential heavy industry globally. Paper production, based largely on the kraft process, is mainly intended for the food packaging sector and, thus, is associated with contamination risks. The lack of standardized regulations and the different analytical techniques used make information on the subject complex, particularly for inorganic elements where little information is available in the literature. Most research in this field is based on sample preparation using mineralization via acid digestion to obtain a liquid and homogeneous matrix, mainly with a HNO3/H2O2 mixture. The most commonly used techniques are Atomic Absorption Spectrometry (AAS), Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES), and Inductively Coupled Plasma Mass Spectrometry (ICP-MS), each with its advantages and disadvantages, which complicates the use of these tech-niques for routine analyses on an industrial site. In the same field of inorganic compound analysis, Microwave Plasma Atomic Emission Spectrometry (MP-AES) has become a real alternative to techniques such as AAS or ICP-AES. This technique has been used in several studies in the food and environmental fields. This publication aims to examine, for the first time, the state of the art regarding the analysis of inorganic elements in food packaging and different matrices using MP-AES. The entire manufacturing process is studied to identify possible sources of inorganic contaminants. Various analytical techniques used in the field are also presented, as well as research conducted with MP-AES to highlight the potential benefits of this technique in the field. Full article
(This article belongs to the Section Spectroscopy)
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14 pages, 1600 KB  
Article
Development and Validation of a Method for the Determination of Caffeine in a Small Volume of Saliva Using SPE-LC-DAD
by Suhail Alghanem and Ewelina Dziurkowska
Analytica 2025, 6(4), 40; https://doi.org/10.3390/analytica6040040 - 5 Oct 2025
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Abstract
(1) Background: Caffeine is one of the most widely consumed psychoactive substances. Its safety profile and short half-life make it an ideal drug model for studying the pharmacokinetics of caffeine. This study aimed to develop a method for determination of caffeine in a [...] Read more.
(1) Background: Caffeine is one of the most widely consumed psychoactive substances. Its safety profile and short half-life make it an ideal drug model for studying the pharmacokinetics of caffeine. This study aimed to develop a method for determination of caffeine in a small volume of saliva (200 µL). (2) Methods: Solid-phase extraction was employed to isolate caffeine from saliva, followed by quantitative analysis using liquid chromatography coupled with diode-array detection. Chromatographic separation was achieved on a C18 column, using a gradient mobile phase of acetonitrile and 0.1% formic acid. (3) Results: The method was validated for selectivity, linearity, precision, and accuracy. Linearity was established over the range of 10–10,000 ng/mL (R2 = 0.995). The coefficients of variation for intra- and inter-day precision for the three tested caffeine concentrations did not exceed 12.11%. Recovery from spiked saliva samples exceeded 90.53%. The developed method was applied to preliminary studies to follow the pharmacokinetics of caffeine in saliva. The concentration of the substance was studied in the saliva obtained from a volunteer after espresso consumption. (4) Conclusions: The developed method will offer a reliable approach for non-invasive caffeine monitoring in clinical and research applications. Full article
(This article belongs to the Section Sample Pretreatment and Extraction)
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13 pages, 1200 KB  
Article
Quantitative Assessment of Retention Mechanisms of Nucleosides on a Bare Silica Stationary Phase in Hydrophilic Interaction Liquid Chromatography (HILIC)
by David Kleiner, David Muscatiello, Zugeily Gutierrez, Vanessa Asare and Yong Guo
Analytica 2025, 6(4), 39; https://doi.org/10.3390/analytica6040039 - 3 Oct 2025
Viewed by 419
Abstract
Nucleosides are of significant interest to biomedical and pharmaceutical research and have been successfully separated in hydrophilic interaction liquid chromatography (HILIC). However, there have been few studies focusing on the retention mechanisms, and detailed retention mechanisms are not clearly understood. The quantitative assessment [...] Read more.
Nucleosides are of significant interest to biomedical and pharmaceutical research and have been successfully separated in hydrophilic interaction liquid chromatography (HILIC). However, there have been few studies focusing on the retention mechanisms, and detailed retention mechanisms are not clearly understood. The quantitative assessment methodology based on the linear relationship between the observed retention factors and the phase ratio has been shown to be a new tool to investigate the retention mechanisms of polar compounds in HILIC. This study evaluated the retention mechanisms of 16 nucleosides on a bare silica column. The retention contributions by partitioning, adsorption, and electrostatic attractions are quantitatively determined, and the main retention mechanism can be unambiguously identified for each nucleoside. The study results indicate that the main retention mechanism can shift with the salt concentration in the mobile phase, but partitioning seems to dominate at higher salt concentrations. In addition, the partitioning coefficients are measured using the quantitative assessment methodology and have a relatively strong correlation with the log P values of the nucleosides. Considering large errors in the log P values for these very polar compounds, the partitioning coefficients measured experimentally in the HILIC system may provide a more accurate measure for polarity assessment. Full article
(This article belongs to the Section Chromatography)
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23 pages, 1003 KB  
Article
Enhanced “Greener” and Sustainable Ultrasonic Extraction of Bioactive Components from Waste Wild Apple (Malus sylvestris (L.) Mill.) Fruit Dust: The Impact of Pretreatment with Natural Deep Eutectic Solvents
by Slađana V. Dončić, Dragan Z. Troter, Miroslav M. Sovrlić, Nebojša D. Zdravković, Aleksandar G. Kočović, Miloš N. Milosavljević, Milos Stepovic, Emina M. Mrkalić, Jelena B. Zvezdanović, Dušica P. Ilić and Sandra S. Konstantinović
Analytica 2025, 6(4), 38; https://doi.org/10.3390/analytica6040038 - 2 Oct 2025
Viewed by 442
Abstract
Significant depletion of natural resources, coupled with increased environmental pollution resulting from the constant evolution of global industrialization, poses a considerable problem. Therefore, it is unsurprising that sustainable “green” chemistry and technology are gathering the worldwide scientific community, whose common goal is to [...] Read more.
Significant depletion of natural resources, coupled with increased environmental pollution resulting from the constant evolution of global industrialization, poses a considerable problem. Therefore, it is unsurprising that sustainable “green” chemistry and technology are gathering the worldwide scientific community, whose common goal is to find applicable solutions for the abovementioned problems. This paper combined the ultrasonic extraction method (a form of “green” technology) with natural deep eutectic solvents (NADESs, a type of “green” solvent) for the production of extracts from an industrial by-product (discarded waste wild apple dust). Waste wild apple dust was pretreated with different NADESs in order to explore the pretreatment benefits regarding ultrasonic extraction of bioactive compounds. Among all solvents used, aqueous propylene glycol was chosen as the best system, which, combined with Reline NADES pretreatment, provided the highest TPC and TFC values, together with the best antioxidant activities. UHPLC-DAD-MS analyses of extracts revealed the presence of natural organic acids, quercetin and kaempferol derivatives, tannins, and flavones. Following this procedure, valorization of agro-industrial apple herbal waste resulted in obtaining extracts with high potential for utilization in different industrial branches (food and pharmaceutical industries), contributing to both cleaner production and reduced environmental impact. Full article
(This article belongs to the Section Sample Pretreatment and Extraction)
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