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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 (30 September 2023) | Viewed by 34721

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Special Issue Editors

Prof. Dr. Victoria Samanidou

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Guest Editor

Laboratory of Analytical Chemistry, School of Chemistry, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece
Interests: analytical chemistry; sample preparation; chromatography; HPLC; method validation; method development; separation science; food analysis; bioanalysis; environmental analysis; green analytical chemistry; sorptive extraction; microextraction techniques
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Prof. Dr. Verónica Pino

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Guest Editor

Department of Chemistry, Analytical Division, University of La Laguna, San Cristóbal de La Laguna, Spain
Interests: analytical sample preparation; novel materials; chromatography; ionic liquids and derivatives; metal-organic frameworks
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Dr. Natasa Kalogiouri

E-Mail Website
Guest Editor

Laboratory of Analytical Chemistry, School of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece
Interests: analytical chemistry; microextraction sample preparation techniques; high-pressure liquid chromatography; gas chromatography; high-resolution mass spectrometry; 2D chromatographic systems; metabolomics; chemometrics
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Special Issue Information

Dear Colleagues,

Undoubtedly, all pivotal advances in a great number of scientific fields rely on the respective advances in chemistry. Among all fields, analytical chemistry has the leading role.

Analytical methods are necessary in dentistry, medicine (both human and veterinary), archaeology, the pharmaceutical industry, food science and technology, and environmental sciences, and these are only a few examples. The multidisciplinary role of chemistry is reflected in all important advances from research groups in every technological progress, proving that analytical chemistry is the key issue in scientific progress.

In parallel with this outstanding role of analytical chemistry in a variety of scientific fields, we would particularly like to reflect the impact of female researchers in the field of analytical chemistry in this Special Issue to serve as a motivation guide for girls and women pursuing a STEM career.

Therefore, we invite well-established scientists to share the results of their research with the scientific community through this Special Issue, which aims to compile manuscripts written or lead by women analytical chemists

Prof. Dr. Victoria Samanidou
Prof. Dr. Verónica Pino
Dr. Natasa Kalogiouri
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 100 words) can be sent to the Editorial Office for announcement on this website.

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. Methods and Protocols is an international peer-reviewed open access semimonthly 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 1800 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

analytical chemistry
method development
method validation
analytical techniques
analytical methods
analytical applications
female scientists

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Published Papers (10 papers)

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Research

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22 pages, 1260 KiB

Open AccessArticle

Allergens and Other Harmful Substances in Hydroalcoholic Gels: Compliance with Current Regulation

by Ana Castiñeira-Landeira, Lua Vazquez, Thierry Dagnac, Maria Celeiro and María Llompart

Methods Protoc. 2023, 6(5), 95; https://doi.org/10.3390/mps6050095 - 7 Oct 2023

Cited by 1 | Viewed by 2161

Abstract

Hydroalcoholic gels or hand sanitisers have become essential products to prevent and mitigate the transmission of COVID-19. Depending on their use, they can be classified as cosmetics (cleaning the skin) or biocides (with antimicrobial effects). The aim of this work was to determine sixty personal care products frequently found in cosmetic formulations, including fragrance allergens, synthetic musks, preservatives and plasticisers, in hydroalcoholic gels and evaluate their compliance with the current regulation. A simple and fast analytical methodology based on solid-phase microextraction followed by gas chromatography–tandem mass spectrometry (SPME-GC-MS/MS) was validated and applied to 67 real samples. Among the 60 target compounds, 47 of them were found in the analysed hand sanitisers, highlighting the high number of fragrance allergens (up to 23) at concentrations of up to 32,458 μg g⁻¹. Most of the samples did not comply with the labelling requirements of the EU Regulation No 1223/2009, and some of them even contained compounds banned in cosmetic products such as plasticisers. Method sustainability was also evaluated using the metric tool AGREEPrep, demonstrating its greenness. Full article

(This article belongs to the Special Issue Women’s Special Issue Series: Analytical Methods)

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16 pages, 2558 KiB

Open AccessArticle

pH and NaCl Optimisation to Improve the Stability of Gold and Silver Nanoparticles’ Anti-Zearalenone Antibody Conjugates for Immunochromatographic Assay

by Thasmin Shahjahan, Bilal Javed, Vinayak Sharma and Furong Tian

Methods Protoc. 2023, 6(5), 93; https://doi.org/10.3390/mps6050093 - 3 Oct 2023

Cited by 6 | Viewed by 4072

Abstract

The aim of this research is to define optimal conditions to improve the stability of gold and silver nanoparticles’ anti-zearalenone antibody conjugates for their utilisation in lateral flow immunochromatographic assay (LFIA). The Turkevich–Frens method was used to synthesise gold nanoparticles (AuNPs), which were between 10 and 110 nm in diameter. Silver nanoparticles (AgNPs) with a size distribution of 2.5 to 100 nm were synthesised using sodium borohydride as a reducing agent. The onset of AuNP and AgNP aggregation occurred at 150 mM and 80 mM NaCl concentrations, respectively. Stable Au and Ag nanoparticle–antibody conjugates were achieved at 1.2 mM of K₂CO₃ concentration, which corresponds to the pH value of ≈7. Lastly, the highest degree of conjugation between Au and Ag nanoparticles and anti-zearalenone antibodies was at 4 and 6 µg/mL of antibody concentrations. The optimisation of the conjugation conditions can contribute to better stability of nanoparticles and their antibody conjugate and can improve the reproducibility of results of bioreporter molecules in biosensing lateral flow devices. Full article

(This article belongs to the Special Issue Women’s Special Issue Series: Analytical Methods)

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13 pages, 3213 KiB

Open AccessArticle

Ultrasound-Assisted Anthocyanins Extraction from Pigmented Corn: Optimization Using Response Surface Methodology

by Annisa Nurkhasanah, Titouan Fardad, Ceferino Carrera, Widiastuti Setyaningsih and Miguel Palma

Methods Protoc. 2023, 6(4), 69; https://doi.org/10.3390/mps6040069 - 30 Jul 2023

Cited by 9 | Viewed by 2785

Abstract

This study aimed to determine the optimal UAE conditions for extracting anthocyanins from pigmented corn using the Box–Behnken design (BBD). Six anthocyanins were identified in the samples and were used as response variables to evaluate the effects of the following working variables: extraction solvent pH (2–7), temperature (10–70 °C), solvent composition (0–50% methanol in water), and ultrasound power (20–80%). The extraction time (5–25 min) was evaluated for complete recovery. Response surface methodology suggested optimal conditions, specifically 36% methanol in water with pH 7 at 70 °C using 73% ultrasound power for 10 min. The method was validated with a high level of accuracy (>90% of recovery) and high precision (CV < 5% for both repeatability and intermediate precision). Finally, the proposed analytical extraction method was successfully applied to determine anthocyanins that covered a wide concentration range (36.47–551.92 mg kg⁻¹) in several pigmented corn samples revealing potential varieties providing more health benefits. Full article

(This article belongs to the Special Issue Women’s Special Issue Series: Analytical Methods)

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10 pages, 2028 KiB

Open AccessArticle

On-Site Multisample Determination of Chlorogenic Acid in Green Coffee by Chemiluminiscent Imaging

by Sergi Mallorca-Cebria, Yolanda Moliner-Martinez, Carmen Molins-Legua and Pilar Campins-Falcó

Methods Protoc. 2023, 6(1), 20; https://doi.org/10.3390/mps6010020 - 14 Feb 2023

Viewed by 1813

Abstract

The potential of antioxidants in preventing several diseases has attracted great attention in recent years. Indeed, these products are part of a multi-billion industry. However, there is a lack of scientific information about safety, quality, doses, and changes over time. In the present work, a simple multisample methodology based on chemiluminiscent imaging to determine chlorogenic acid (CHLA) in green coffee samples has been proposed. The multi-chemiluminiscent response was obtained after a luminol-persulfate reaction at pH 10.8 in a multiplate followed by image capture with a charge-coupled device (CCD) camera as a readout system. The chemiluminiscent image was used as an analytical response by measuring the luminescent intensity at 0 °C with the CCD camera. Under the optimal conditions, the detection limit was 20 µM and precision was also adequate with RSD < 12%. The accuracy of the proposed system was evaluated by studying the matrix effect, using a standard addition method. Recoveries of chlorogenic acid ranged from 93–94%. The use of the CCD camera demonstrated advantages such as analysis by image inspection, portability, and easy-handling which is of particular relevance in the application for quality control in industries. Furthermore, multisample analysis was allowed by one single image saving time, energy, and cost. The proposed methodology is a promising sustainable analytical tool for quality control to ensure green coffee safety through dosage control and proper labelling preventing potential frauds. Full article

(This article belongs to the Special Issue Women’s Special Issue Series: Analytical Methods)

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14 pages, 3144 KiB

Open AccessArticle

Determination of UV Filters in Waste Sludge Using QuEChERS Method Followed by In-Port Derivatization Coupled with GC–MS/MS

by Cemile Yücel, Ilgi Karapinar, Serenay Ceren Tüzün, Hasan Ertaş and Fatma Nil Ertaş

Methods Protoc. 2022, 5(6), 92; https://doi.org/10.3390/mps5060092 - 23 Nov 2022

Cited by 4 | Viewed by 2919

Abstract

UV filters (UVFs) are widely used in personal care and in industrial products for protection against photodegradation. In recent years, their potential toxicological and environmental effects have received growing attention. Due to their excessive use, their residue levels in the environment are gradually increasing and they tend to accumulate on biological wastewater treatment sludge. The utilization of sludge as fertilizer could be one of the main routes of UVF contamination in the environment. Therefore, the development of a reliable and sensitive method of analyzing their trace level residues in waste sludge samples is of great importance. The success of the method largely depends on the sample preparation technique in such complex matrices. This study presents a rapid, sensitive and green analysis method for eight UVFs in sludge samples, selected for their rather low no-observed-effect concentrations (NOEC). For this purpose, the QuEChERS methodology was coupled with in-port derivatization for subsequent detection of the targeted UVFs via GC–MS/MS. The analysis time was substantially shortened using this method, and reagent utilization was also reduced. The method was validated in the sludge samples, and high recovery (66–123%) and low RSD values (<25.6%) were obtained. In addition, major contributing uncertainty sources and expanded uncertainties were determined. Full article

(This article belongs to the Special Issue Women’s Special Issue Series: Analytical Methods)

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10 pages, 1346 KiB

Open AccessArticle

An Efficient, Simultaneous Electrochemical Assay of Rosuvastatin and Ezetimibe from Human Urine and Serum Samples

by Leyla Karadurmus, Sevinc Kurbanoglu, Bengi Uslu and Sibel A. Ozkan

Methods Protoc. 2022, 5(6), 90; https://doi.org/10.3390/mps5060090 - 1 Nov 2022

Cited by 7 | Viewed by 2477

Abstract

The drug combination of rosuvastatin (ROS) and ezetimibe (EZE) is used to treat hypercholesterolemia. In this work, a simultaneous electrochemical examination of ROS and EZE was conducted for the first time. The electrochemical determination of ROS and EZE was carried out using adsorptive stripping differential pulse voltammetry (AdSDPV) on a glassy carbon electrode (GCE) in 0.1 M H₂SO₄. The effects of the pH, scan rate, deposition potential, and time on the detection of ROS and EZE were analyzed. Under optimum conditions, the developed sensor exhibited a linear response between 1.0 × 10⁻⁶ M and 2.5 × 10⁻⁵ M for EZE and 5.0 × 10⁻⁶ M, and 1.25 × 10⁻⁵ M for ROS. The detection limits for ROS and EZE were 3.0 × 10⁻⁷ M and 2.0 × 10⁻⁶ M, respectively. The developed sensor was validated in terms of linear range, accuracy, precision, the limit of determination (LOD), and the limit of quantification (LOQ), and it was evaluated according to ICH Guidelines and USP criteria. The proposed method was also used to determine ROS and EZE in human urine and serum samples, which are reported in terms of recovery studies. Full article

(This article belongs to the Special Issue Women’s Special Issue Series: Analytical Methods)

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16 pages, 2053 KiB

Open AccessArticle

Simultaneous Quantification of Bisphenol-A and 4-Tert-Octylphenol in the Live Aquaculture Feed Artemia franciscana and in Its Culture Medium Using HPLC-DAD

by Despoina Giamaki, Konstantina Dindini, Victoria F. Samanidou and Maria Touraki

Methods Protoc. 2022, 5(3), 38; https://doi.org/10.3390/mps5030038 - 1 May 2022

Cited by 4 | Viewed by 4391

Abstract

Aquaculture, a mass supplier of seafood, relies on plastic materials that may contain the endocrine disruptors bisphenol-A (BPA) and tert-octylphenol (t-OCT). These pollutants present toxicity to Artemia, the live aquaculture feed, and are transferred through it to the larval stages of the cultured organisms. The purpose of this work is the development and validation of an analytical method to determine BPA and t-OCT in Artemia and their culture medium, using n-octylphenol as the internal standard. Extraction of the samples was performed with H₂O/TFA (0.08%)–methanol (3:1), followed by SPE. Analysis was performed in a Nucleosil column with mobile phases A (95:5, v/v, 0.1% TFA in H₂O:CH₃CN) and B (5:95, v/v, 0.08% TFA in H₂O:CH₃CN). Calibration curves were constructed in the range of concentrations expected following a 24 h administration of BPA (10 μg/mL) or t-OCT (0.5 μg/mL), below their respective LC₅₀. At the end of exposure to the pollutants, their total levels appeared reduced by about 32% for BPA and 35% for t-OCT, and this reduction could not be accounted for by photodegradation (9–19%). The developed method was validated in terms of linearity, accuracy, and precision, demonstrating the uptake of BPA and t-OCT in Artemia. Full article

(This article belongs to the Special Issue Women’s Special Issue Series: Analytical Methods)

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Review

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15 pages, 602 KiB

Open AccessReview

New Prospects in the Electroanalysis of Heavy Metal Ions (Cd, Pb, Zn, Cu): Development and Application of Novel Electrode Surfaces

by Vasiliki Keramari, Sophia Karastogianni and Stella Girousi

Methods Protoc. 2023, 6(4), 60; https://doi.org/10.3390/mps6040060 - 26 Jun 2023

Cited by 17 | Viewed by 3314

Abstract

The detection of toxic heavy metal ions, especially cadmium (Cd), lead (Pb), zinc (Zn), and copper (Cu), is a global problem due to ongoing pollution incidents and continuous anthropogenic and industrial activities. Therefore, it is important to develop effective detection techniques to determine the levels of pollution from heavy metal ions in various media. Electrochemical techniques, more specifically voltammetry, due to its properties, is a promising method for the simultaneous detection of heavy metal ions. This review examines the current trends related to electrode formation and analysis techniques used. In addition, there is a reference to advanced detection methods based on the nanoparticles that have been developed so far, as well as formation with bismuth and the emerging technique of screen-printed electrodes. Finally, the advantages of using these methods are highlighted, while a discussion is presented on the benefits arising from nanotechnology, as it gives researchers new ideas for integrating these technologies into devices that can be used anywhere at any time. Reference is also made to the speciation of metals and how it affects their toxicity, as it is an important subject of research. Full article

(This article belongs to the Special Issue Women’s Special Issue Series: Analytical Methods)

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17 pages, 716 KiB

Open AccessReview

Solid-Phase Microextraction—Gas Chromatography Analytical Strategies for Pesticide Analysis

by Juan Aspromonte, Carlina Lancioni and Giorgia Purcaro

Methods Protoc. 2022, 5(5), 82; https://doi.org/10.3390/mps5050082 - 17 Oct 2022

Cited by 13 | Viewed by 4057

Abstract

Due to their extensive use and the globalized commerce of agricultural goods, pesticides have become a global concern. Despite the undoubtful advantages of their use in agricultural practices, their misuse is a threat to the environment and human health. Their analysis in environmental samples and in food products continues to gain interest in the analytical chemistry community as they are challenging matrices, and legal concentration limits are particularly low (in the order of ppb). In particular, the use of solid-phase microextraction (SPME) has gained special attention in this field thanks to its potential to minimize the matrix effect, while enriching its concentration, allowing very low limits of detection, and without the need of a large amount of solvents or lengthy procedures. Moreover, its combination with gas chromatography (GC) can be easily automated, making it a very interesting approach for routine analysis. In this review, advances and analytical strategies for the use of SPME coupled with GC are discussed and compared for the analysis of pesticides in food and environmental samples, hopefully encouraging its further development and routine application in this field. Full article

(This article belongs to the Special Issue Women’s Special Issue Series: Analytical Methods)

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Other

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12 pages, 1544 KiB

Open AccessProtocol

Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Leaf and Bark Samples of Sambucus nigra Using High-Performance Liquid Chromatography (HPLC)

by Fausto Viteri, Nazly E. Sánchez and Katiuska Alexandrino

Methods Protoc. 2023, 6(1), 17; https://doi.org/10.3390/mps6010017 - 8 Feb 2023

Cited by 8 | Viewed by 3826

Abstract

Polycyclic aromatic hydrocarbons (PAHs) are ubiquitous organic compounds coming from natural or anthropogenic activities. Tree organs such as leaves and barks have been used to monitor urban air quality and have achieved remarkable ecological importance. However, the potential of many tree species as biomonitors is still unknown and efforts should be focused on conducting studies that analyze their capabilities with a viable analytical method. In this work, an analytical method for quantification of the 16 EPA priority PAHs from the leaves and bark of Sambucus nigra was validated. In general, the method showed good linearity, detection limits, precision, and recoveries, demonstrating that it is suitable for analyzing PAHs in both the leaves and bark of the Sambucus nigra species for which no analytical method for PAHs is yet available. The high prevalence of fluoranthene in the samples, which is a PAH related to coal combustion and biomass burning, and benzo[a]pyrene, which has a carcinogenic effect, was identified. Full article

(This article belongs to the Special Issue Women’s Special Issue Series: Analytical Methods)

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