Advances in Analytical Strategies to Study Biological and Environmental Samples

A special issue of Methods and Protocols (ISSN 2409-9279). This special issue belongs to the section "Biochemical and Chemical Analysis & Synthesis".

Deadline for manuscript submissions: closed (15 April 2023) | Viewed by 17666

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Guest Editor
Department of Chemistry, Sapienza University of Rome, Rome, Italy
Interests: analytical and bioanalytical chemistry; environmental chemistry and monitoring; elemental analysis; atomic spectroscopic techniques (ICP-MS, ICP-OES, CV-AFS, AMA, GF-AAS); sample treatment; determination of trace elements in foods
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Guest Editor
Department of Chemistry, Sapienza University of Rome, Rome, Italy
Interests: analytical and environmental chemistry; trace elemental analysis; atomic spectroscopic techniques; sample treatment; food analysis

Special Issue Information

Dear Colleagues,

The determination of chemical contaminants in biological and environmental matrices is potentially useful for assessing human health, monitoring occupational and environmental exposure, and evaluating environmental quality. On the other hand, owing to the lack of standardized analytical procedures (including sample treatment methods), it is not easy to compare and interpret the results (such as intervals and reference values) from different studies; reach significant conclusions in toxicological, clinical, environmental, and forensic investigations; and obtain data to support decisions on both human and environmental protection. Moreover, analyte loss, contamination, and/or interferences may also lead to a decrease in the results' analytical accuracy. Considering these aspects, all original research articles, communications, and review papers on all aspects of the analytical approches for biomonitoring are welcome, including, but not limited to:

  • sampling
  • sample preparation
  • analytical characteristics
  • analytical quality assurance and control
  • emerging environmental chemical contaminants
  • elements
  • application in field
  • human biological matrices
  • biomonitoring
  • chemical speciation

Dr. Maria Astolfi
Dr. Elisabetta Marconi
Guest Editors

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Published Papers (4 papers)

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18 pages, 9239 KiB  
Article
Combined Use of Non-Invasive and Micro-Invasive Analytical Investigations to Understand the State of Conservation and the Causes of Degradation of I Tesori del Mare (1901) by Plinio Nomellini
by Andrea Macchia, Chiara Biribicchi, Laura Rivaroli, Hélène Aureli, Eleonora Cerafogli, Irene Angela Colasanti, Paola Carnazza, Giuseppe Demasi and Mauro Francesco La Russa
Methods Protoc. 2022, 5(3), 52; https://doi.org/10.3390/mps5030052 - 18 Jun 2022
Cited by 7 | Viewed by 2006
Abstract
In this study, the investigation of the oil painting on canvas I Tesori del Mare made by Plinio Nomellini in 1901 is presented. The aim of the research was threefold: the examination of the state of conservation in view of the restoration treatment, [...] Read more.
In this study, the investigation of the oil painting on canvas I Tesori del Mare made by Plinio Nomellini in 1901 is presented. The aim of the research was threefold: the examination of the state of conservation in view of the restoration treatment, together with the identification of the causes of degradation and the study of the artistic technique. During the years, the artwork underwent several cleaning and fixing interventions, resulting in a patchy appearance of the surface. Nevertheless, the presence of consistent liftings persists, while the protective coating shows uneven chromatic alteration, both requiring further analysis. Multispectral imaging allowed for better visualization of the figuration’s structure and the restored areas. The combined use of Raman spectroscopy, Fourier Transform Infrared spectroscopy in the Attenuated Total Reflection mode (FT-IR ATR), and Scanning Electron Microscopy coupled with an Energy Dispersive Spectroscopy (SEM/EDS) enabled better understanding of the stratigraphy through the identification of some pigments, the binder, and the aged varnish layer on the top. SEM/EDS highlighted the presence of zinc in both the ground layer and the paint layers. Furthermore, FT-IR ATR spectroscopy showed peaks related to metal soaps such as zinc stearate, which are known to cause severe delamination of the paint layers, explaining the recurring lifting issues. Eventually, the varnish layer was found to be acrylic resin, presumably mixed with varnishes applied in past restoration treatments. Full article
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16 pages, 5908 KiB  
Article
In-Situ Comparative Study of Eucalyptus, Basil, Cloves, Thyme, Pine Tree, and Tea Tree Essential Oil Biocide Efficacy
by Andrea Macchia, Hélène Aureli, Fernanda Prestileo, Federico Ortenzi, Shaila Sellathurai, Antonella Docci, Eleonora Cerafogli, Irene Angela Colasanti, Michela Ricca and Mauro Francesco La Russa
Methods Protoc. 2022, 5(3), 37; https://doi.org/10.3390/mps5030037 - 27 Apr 2022
Cited by 10 | Viewed by 3424
Abstract
Bio-colonization is a dynamic and multiphasic process headed by microorganisms. Conventional treatments to process affected stone materials include chemical biocides, whose formulations are mainly composed of quaternary ammonium salts(QAs), reported to be toxic for human health, dangerous for the environment, and not biodegradable. [...] Read more.
Bio-colonization is a dynamic and multiphasic process headed by microorganisms. Conventional treatments to process affected stone materials include chemical biocides, whose formulations are mainly composed of quaternary ammonium salts(QAs), reported to be toxic for human health, dangerous for the environment, and not biodegradable. Accordingly, novel green and eco-friendly products are a promising alternative to treat stone materials deteriorated by microorganism colonization. In this study, the efficacy of pure essential oils (EOs) and a mix of EOs was assessed in situ and compared to a conventional biocide based on QAs, and two commercially green products based on EOs, which were taken as references, through application on a mosaic located at the Archaeological Park of Ostia Antica (Rome). The EO biocide efficacy was analyzed by ultraviolet induced luminescence, spectro-colorimetry and bio-luminometry analyses while the possibility of their permanence on simulated substrate was studied by FTIR spectroscopy. It was observed by FTIR analysis, that EOs considered volatile can leave a residue after the application; typical fingerprint bands at about 2926, 1510, and 1455 cm−1 were recorded in the EO spectra. Every tested oil was confirmed to have a biocide action although minimal in relation to the most conventional products based on QAs. The synergy of the essential oils revealed positive results, showing a stronger biocide efficacy. Further investigation should be carried out to develop the method of application and study of essential oils on cultural heritage. Full article
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11 pages, 2188 KiB  
Article
How to Clean and Safely Remove HF from Acid Digestion Solutions for Ultra-Trace Analysis: A Microwave-Assisted Vessel-Inside-Vessel Protocol
by Marco Pinna, Arianna Signorelli, Gilberto Binda, Carlo Dossi, Laura Rampazzi, Davide Spanu and Sandro Recchia
Methods Protoc. 2022, 5(2), 30; https://doi.org/10.3390/mps5020030 - 03 Apr 2022
Cited by 4 | Viewed by 4474
Abstract
The complete dissolution of silicate-containing materials, often necessary for elemental determination, is generally performed by microwave-assisted digestion involving the forced use of hydrofluoric acid (HF). Although highly efficient in dissolving silicates, this acid exhibits many detrimental effects (e.g., formation of precipitates, corrosiveness to [...] Read more.
The complete dissolution of silicate-containing materials, often necessary for elemental determination, is generally performed by microwave-assisted digestion involving the forced use of hydrofluoric acid (HF). Although highly efficient in dissolving silicates, this acid exhibits many detrimental effects (e.g., formation of precipitates, corrosiveness to glassware) that make its removal after digestion essential. The displacement of HF is normally achieved by evaporation in open-vessel systems: atmospheric contamination or loss of analytes can occur when fuming-off HF owing to the non-ultraclean conditions necessarily adopted for safety reasons. This aspect strongly hinders determination at the ultra-trace level. To overcome this issue, we propose a clean and safe microwave-assisted procedure to induce the evaporative migration of HF inside a sealed “vessel-inside-vessel” system: up to 99.9% of HF can be removed by performing two additional microwave cycles after sample dissolution. HF migrates from the digestion solution to a scavenger (ultrapure H2O) via a simple physical mechanism, and then, it can be safely dismissed/recycled. The procedure was validated by a soil reference material (NIST 2710), and no external or cross-contamination was observed for the 27 trace elements studied. The results demonstrate the suitability of this protocol for ultra-trace analysis when the utilization of HF is mandatory. Full article
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10 pages, 964 KiB  
Protocol
Simple Acid Digestion Procedure for the Determination of Total Mercury in Plankton by Cold Vapor Atomic Fluorescence Spectroscopy
by João Pereira Santos, Lirie Mehmeti and Vera I. Slaveykova
Methods Protoc. 2022, 5(2), 29; https://doi.org/10.3390/mps5020029 - 25 Mar 2022
Cited by 9 | Viewed by 6554
Abstract
Plankton, at the bottom of the food web, play a central role in the entry of mercury into the aquatic biota. To investigate their role in mercury uptake, reliable analytical procedures for Hg analysis are highly sought. Wet digestion procedures for determining total [...] Read more.
Plankton, at the bottom of the food web, play a central role in the entry of mercury into the aquatic biota. To investigate their role in mercury uptake, reliable analytical procedures for Hg analysis are highly sought. Wet digestion procedures for determining total mercury in different biological matrices have been established since years, however only few studies focused on planktonic samples. In the present work, a simple and cost-effective wet digestion method was developed for the determination of total mercury in samples of small plankton material using a cold vapor atomic fluorescence spectroscopy (CVAFS). The optimization of the digestion method was achieved by using glass vessels with Teflon caps, low amount of acids (3 mL w/w 65% HNO3 or 3 mL 50% v/v HNO3), a constant temperature of 85 °C, the presence and absence of pre-ultrasound treatment, and a continuous digestion period (12 h). Certified reference materials IAEA-450 (unicellular alga Scenedesmus obliquus) and BRC-414 (plankton matrix) were used to optimize and validate the digestion method. The recovery efficiency of the proposed method for IAEA-450 and BCR-414 (3.1 mg and 21.5 mg) ranged between 94.1 ± 7.6% and 97.2 ± 4.6%. The method displayed a good recovery efficiency and precision for plankton matrices of low size. Thus, allowing better digestion of planktonic samples for mercury analysis using CVAFS techniques. Full article
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