Journal Description
Analytica
Analytica
is an international, peer-reviewed, open access journal on analytical chemistry and chemical analysis published quarterly online by MDPI.
- Open Access— free for readers, with article processing charges (APC) paid by authors or their institutions.
- High Visibility: indexed within ESCI (Web of Science), Scopus, CAPlus / SciFinder, and other databases.
- Rapid Publication: manuscripts are peer-reviewed and a first decision is provided to authors approximately 15.6 days after submission; acceptance to publication is undertaken in 4.1 days (median values for papers published in this journal in the second half of 2023).
- Recognition of Reviewers: APC discount vouchers, optional signed peer review, and reviewer names published annually in the journal.
Latest Articles
Detection of Gene Doping Using Dried Blood Spots from a Mouse Model with rAAV9 Vector-Mediated Human Erythropoietin Expression as a Pilot Study
Analytica 2024, 5(2), 263-272; https://doi.org/10.3390/analytica5020017 - 4 Jun 2024
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Rapid advancements in gene technology have raised concerns regarding the potential abuse of techniques, such as gene doping, for enhancing athletic performance. To identify this possibility, a reliable procedure for detecting doping genes is required. Although detection methods for doping genes have been
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Rapid advancements in gene technology have raised concerns regarding the potential abuse of techniques, such as gene doping, for enhancing athletic performance. To identify this possibility, a reliable procedure for detecting doping genes is required. Although detection methods for doping genes have been created, there are still areas for further improvement. One significant challenge is the high storage and transport costs of the test samples. For this issue, the dried blood spot (DBS) method can be a cost-effective solution. This study aimed to assess the practicality of incorporating DBSs into the gene doping detection process as a pilot study. Whole-blood samples were initially collected from mice engineered to express human erythropoietin from the rAAV vector. Then, the blood was placed in filter papers and left to dry at room temperature for five hours to form DBSs. These DBSs were subsequently preserved in sealed plastic bags at room temperature. After the extraction of DNA, DBSs were formed, and TaqMan-qPCR was utilized to detect the presence of rAAV vector-derived DNA. The finding confirmed that doping gene-specific fragments were successfully detected in DBSs. This outcome suggests that the DBS method is an effective approach to be considered when developing a comprehensive protocol for gene doping detection.
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Open AccessArticle
Electrochemical Determination of Catechol Using a Disposable Printed Electrode with Conductive Ink Based on Graphite and Carbon Black
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Sthephane Pereira de Oliveira, Thaís Cristina de Oliveira Cândido, Arnaldo César Pereira and Daniela Nunes da Silva
Analytica 2024, 5(2), 250-262; https://doi.org/10.3390/analytica5020016 - 1 Jun 2024
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Catechol (CT) is a phenolic compound widely used in various industrial sectors, but it is toxic; thus, there is a need for methods that aim to identify and quantify the existence of residues of this material in the environment. In this study a
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Catechol (CT) is a phenolic compound widely used in various industrial sectors, but it is toxic; thus, there is a need for methods that aim to identify and quantify the existence of residues of this material in the environment. In this study a disposable printed electrochemical sensor was developed as an effective alternative for determining CT in water samples. The electrode, called SPEC, was manufactured using the screen-printing method using polyethylene terephthalate (PET) as a support, in which a conductive ink based on carbonaceous materials was used to print the working and auxiliary electrodes and a silver/silver chloride of ink on the reference electrode. The optimal ratio for the conductive ink was 6.25% carbon black, 35.42% graphite, and 58.33% nail polish. The ink obtained was characterized by scanning electron microscopy (SEM). The assessment of the effect of pH on the redox process showed Nernstian behavior (0.057 V pH−1), indicating that the process involves the same number of protons and electrons. Under optimized conditions, with 0.2 mol L−1 acetate buffer at pH 5.0, and by square wave voltammetry, the sensor presented sensitivity values of 0.31 μA L μmol−1, a detection limit of 5.96 μmol L−1, and a quantification limit of 19.87 μmol L−1. The sensor was applied to determine CT in tap water samples, and the results showed recoveries between 97.95 and 100.17%.
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Open AccessArticle
Development of Noninvasive Method for the Automated Analysis of Nine Steroid Hormones in Human Saliva by Online Coupling of In-Tube Solid-Phase Microextraction with Liquid Chromatography–Tandem Mass Spectrometry
by
Takashi Hitomi and Hiroyuki Kataoka
Analytica 2024, 5(2), 233-249; https://doi.org/10.3390/analytica5020015 - 9 May 2024
Abstract
Accurate measurement of steroid hormones is crucial to elucidate new mechanisms of action and diagnose steroid metabolism-related diseases. This study presents a simple, sensitive, and automated analytical method for nine representative steroid hormones. The method involves on-line coupling of in-tube solid-phase microextraction (IT-SPME)
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Accurate measurement of steroid hormones is crucial to elucidate new mechanisms of action and diagnose steroid metabolism-related diseases. This study presents a simple, sensitive, and automated analytical method for nine representative steroid hormones. The method involves on-line coupling of in-tube solid-phase microextraction (IT-SPME) with liquid chromatography–tandem mass spectrometry (LC–MS/MS). The steroid hormones were extracted and enriched on a Supel-Q PLOT capillary column using IT-SPME. Subsequently, they were separated and detected within 6 min using a Discovery HS F5-3 column and positive ion mode multiple reaction monitoring system via LC–MS/MS. Calibration curves of these compounds using each stable isotope-labeled internal standard (IS) showed linearity with correlation coefficients greater than 0.9990 in the range of 0.01–40 ng/mL, with limits of detection (S/N = 3) of 0.7–21 pg/mL. Moreover, intra- and inter-day variations were lower than 8.1 and 15% (n = 6), respectively. The recoveries of these compounds from saliva samples were in the range of 82–114%. The developed IT-SPME/LC–MS/MS method of steroid hormones is a highly sensitive, specific, and non-invasive analytical method that allows extraction and enrichment with no organic solvents, and enables direct automated online analysis by simply ultrafiltrating a small sample of saliva.
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(This article belongs to the Section Sample Pretreatment and Extraction)
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Open AccessArticle
Quantification of Recycled PET in Commercial Bottles by IR Spectroscopy and Chemometrics
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Alessandro Zappi, Alessandra Biancolillo, Nicholas Kassouf, Valentina Marassi, Pietro Morozzi, Laura Tositti and Dora Melucci
Analytica 2024, 5(2), 219-232; https://doi.org/10.3390/analytica5020014 - 8 May 2024
Abstract
A novel approach for the quantification of recycled polyethylene terephthalate (r-PET) in commercial bottles is presented. Fifty-eight bottle samples from several brands and producers containing different percentages of r-PET were purchased from the market. Samples were analyzed by two spectroscopic methods: near-infrared (NIR)
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A novel approach for the quantification of recycled polyethylene terephthalate (r-PET) in commercial bottles is presented. Fifty-eight bottle samples from several brands and producers containing different percentages of r-PET were purchased from the market. Samples were analyzed by two spectroscopic methods: near-infrared (NIR) spectroscopy and attenuated total reflection (ATR) spectroscopy in the mid-infrared (MIR) region. No chemical pre-treatment was applied before analyses. The spectra were analyzed by partial-least squares (PLS) regression, and two models for NIR and MIR data were computed. Then, a multi-block regression was applied to join the two datasets. All models were validated by cross-validation and by excluding and projecting onto the model the replicated spectra of one sample at a time. Results demonstrated the potential of this approach, especially considering the variability of commercial samples in terms of additives, shape, or thickness of the bottles: for samples close to the centroids of the models (i.e., from 10 to 50% r-PET), the predictions of multi-block method seldom departed from the expected values of ±10%. Only for samples with 0% declared r-PET, the models showed poor prediction abilities.
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(This article belongs to the Section Chemometrics)
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Open AccessArticle
Treatment of Water Contaminated by Ship Oil: Study of Adsorption in a Fixed-Bed Column
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Rachel de M. Ferreira, Bernardo Dia Ribeiro, Danielle M. A. Stapelfeldt and Maria de F. R. Moreira
Analytica 2024, 5(2), 203-218; https://doi.org/10.3390/analytica5020013 - 1 May 2024
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Aquatic macrophytes like Salvinia sp. have rapid proliferation and a great capacity for ecological adaptation. In addition to these characteristics, this study points to their ability to adsorb contaminants such as dyes, metals, and oils. This work aims, through an adsorption study, to
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Aquatic macrophytes like Salvinia sp. have rapid proliferation and a great capacity for ecological adaptation. In addition to these characteristics, this study points to their ability to adsorb contaminants such as dyes, metals, and oils. This work aims, through an adsorption study, to propose an alternative treatment using chemically modified Salvinia sp. (SOH) biomass to remove oil from water. Batch adsorption experiments were performed to observe the effects of concentration, pH, time, temperature, desorption, and reuse of the biomass. The adsorption mechanisms, performance, kinetics, isotherm, thermodynamics, and reusability of biomass were evaluated. Both adsorbents were well-defined by the Freundlich model isotherm. According to the results obtained, the qmax was 898.0 mg g−1 for SOH in oil-in-salt water emulsion in 15 min and 930.59 mg g−1 for Salvinia sp. in natura (SS) in the oil-in-water emulsion. In the fixed-bed column adsorption, the adsorption capacity was 2.99 g g−1 for SS and 3.49 g g−1 for SOH, and the saturation capacity was 42.89 g g−1 SS and 42.99 g g−1 SOH. According to the adsorption models, the Bohart–Adams model best fits the experimental data of this study. The SOH adsorbed oil recovery test was successful, with 100% oil recovery.
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Open AccessReview
Poly- and Perfluoroalkyl Substance (PFAS) Analysis in Environmental Matrices: An Overview of the Extraction and Chromatographic Detection Methods
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Alessia Iannone, Fabiana Carriera, Cristina Di Fiore and Pasquale Avino
Analytica 2024, 5(2), 187-202; https://doi.org/10.3390/analytica5020012 - 19 Apr 2024
Abstract
Per- and polyfluoroalkyl substances (PFASs) are carbon–fluorine compounds with widespread industrial and domestic use, posing potential toxicological risks to humans and ecosystems. Several analytical methods have been developed to assess the occurrence of PFASs in the environment, but a standardized method, applicable to
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Per- and polyfluoroalkyl substances (PFASs) are carbon–fluorine compounds with widespread industrial and domestic use, posing potential toxicological risks to humans and ecosystems. Several analytical methods have been developed to assess the occurrence of PFASs in the environment, but a standardized method, applicable to all matrices, is still lacking. This paper reviews the extraction and chromatographic detection methods for PFAS assessment in environmental samples, considering parameters such as the LOD, LOQ, and recoveries. Solid phase extraction (SPE) is commonly used, showing high recovery rates for water, soil, and sediment samples using HBL and WAX polymeric sorbents (85–100% and 93–111.5%, respectively). LC-MS has demonstrated low LODs and LOQs in seawater (0.01–0.08 ng L−1; 0.03–0.24 ng L−1), marine sediment (0.002–0.018 ng g−1; 0.004–0.054 ng g−1), and dust (0.08–0.68 pg g−1; 0.26–2.25 pg g−1), indicating its sensitivity when detecting trace PFAS levels. Evaluating PFASs is crucial for the development of future removal strategies and risk assessments. Potential solutions including the use of PFAS substitutes and innovative adsorption techniques for their adsorption could present promise in reducing their environmental presence.
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(This article belongs to the Section Chromatography)
Open AccessArticle
A Metabolomics Study by 1H HRMAS NMR: From Sheep Milk to a Pressed-Curd Cheese: A Proof of Concept
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David Castejón, José Segura, Karen Paola Cruz-Díaz, Víctor Remiro, María Encarnación Fernández-Valle, María Dolores Romero de Ávila, Palmira Villa and María Isabel Cambero
Analytica 2024, 5(2), 170-186; https://doi.org/10.3390/analytica5020011 - 13 Apr 2024
Abstract
For the first time, High-Resolution Magic Angle Nuclear Magnetic Resonance spectroscopy (NMR-HRMAS) was applied to directly identify specific metabolites from a Spanish raw ewe’s milk and enzymatic coagulation pressed-curd cheese (Protected Geographical Indication: Castellano) manufactured by two procedures (traditional/artisanal vs. industrial) and
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For the first time, High-Resolution Magic Angle Nuclear Magnetic Resonance spectroscopy (NMR-HRMAS) was applied to directly identify specific metabolites from a Spanish raw ewe’s milk and enzymatic coagulation pressed-curd cheese (Protected Geographical Indication: Castellano) manufactured by two procedures (traditional/artisanal vs. industrial) and including the ewe’s raw milk. The NMR parameters were optimized to study the complex matrixes of this type of cheese. In addition, conventional overcrowded 1H-NMR-HRMAS spectra were selectively simplified by a Carr–Purcell–Meiboom–Gill (CPMG) sequence or a stimulated echo pulse sequence by bipolar gradients (DIFF), thus modulating spin–spin relaxation times and diffusion of molecular components, respectively. 1H-NMR-HRMAS spectroscopy displayed important information about cheese metabolites, which can be associated with different manufacturing processes (industrial vs. traditional) and ripening times (from 2 to 90 days). These results support that this spectroscopy is a useful technique to monitor the ripening process, from raw milk to commercial ripened cheese, using a minimum intact sample, implying the absence of time-consuming sample pretreatments.
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(This article belongs to the Collection Analytical and Applied Chemistry: the challenges and opportunities for growth in the 21st century)
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Open AccessArticle
Headspace-Selected Ion Flow Tube Mass Spectrometry Workflows for Rapid Screening and Quantitation of Hazardous Volatile Impurities in Personal Care Products
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Mark J. Perkins, Colin J. Hastie and Vaughan S. Langford
Analytica 2024, 5(2), 153-169; https://doi.org/10.3390/analytica5020010 - 2 Apr 2024
Abstract
Personal care products (PCPs) are intended for regular application by consumers and therefore assuring the safety of these products is very important. Recently, benzene contamination has been highlighted in certain PCPs. The present study applies selected ion flow tube mass spectrometry (SIFT-MS) to
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Personal care products (PCPs) are intended for regular application by consumers and therefore assuring the safety of these products is very important. Recently, benzene contamination has been highlighted in certain PCPs. The present study applies selected ion flow tube mass spectrometry (SIFT-MS) to a simultaneous headspace analysis of benzene, 1,4-dioxane, and formaldehyde—all known or suspected carcinogens—in nine haircare products with supporting qualitative analysis by gas chromatography–mass spectrometry (GC-MS). Headspace-SIFT-MS method development is compatible with the method of standard additions, which is necessary for the quantitation of volatile impurities in these complex emulsions. Benzene was quantified above the low-ng g−1 limit of quantitation (LOQ) in three products, dioxane above the sub-μg g−1 LOQ in all products, and formaldehyde above the low-μg g−1 LOQ in two products, providing a quantitative analysis at concentrations relevant to consumer safety. This study facilitated the development of generic workflows for SIFT-MS method development and application in routine analysis of PCPs. The assessment of workflows for SIFT-MS compared to a conventional GC-MS analysis suggests that 8- to 30-fold throughput enhancements may be possible for quantitative and screening analysis using SIFT-MS.
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(This article belongs to the Collection Analytical and Applied Chemistry: the challenges and opportunities for growth in the 21st century)
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Analytical Compatibility between Various Techniques for Determining Dissolved Manganese in Produced Water
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Gabriela Knippelberg Bifano Manea, Vanusa Bueno Freire, Rainerio Escalfoni Junior and Elcio Cruz de Oliveira
Analytica 2024, 5(1), 139-152; https://doi.org/10.3390/analytica5010009 - 15 Mar 2024
Cited by 1
Abstract
Petroleum-produced water is the primary effluent generated during the oil extraction process, presenting high flow rates, and containing a series of chemical components that are harmful to the environment, such as dissolved manganese. The proof of metrological compatibility between laboratories and different test
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Petroleum-produced water is the primary effluent generated during the oil extraction process, presenting high flow rates, and containing a series of chemical components that are harmful to the environment, such as dissolved manganese. The proof of metrological compatibility between laboratories and different test methods or techniques is an analytical challenge when complying with environmental laws and regulations, which is the aim of this study. The first step of this study was to compare the results of manganese content in real test samples of produced water between some laboratories that used different test methods, that is, flame atomic absorption spectrophotometry, inductively coupled plasma optical emission spectroscopy, and inductively coupled plasma mass spectrometry. Based on one-way analysis of variance, systematic errors were found. The following step was to visit a specific lab, where one could confirm the relevance of the wavelength parameters, operating conditions for the view configuration, and effects of the saline matrices. Finally, a compatibility assessment between the reference laboratory and a new laboratory, which implemented and validated its analytical methodology based on these analytical adjustments, and the experiences and lessons learned in the previous step, was undertaken by a paired t-test.
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(This article belongs to the Collection Analytical and Applied Chemistry: the challenges and opportunities for growth in the 21st century)
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Physicochemical Characterization of ‘Moroccan Picholine’ Olive (Olea europaea L.) Oil Produced in Southern Morocco Using Multivariate Statistical Analysis
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Jamila Gagour, Otmane Hallouch, Abderrahim Asbbane, Abdellatif Laknifli, El Hassan Sakar, Khalid Majourhat and Said Gharby
Analytica 2024, 5(1), 119-138; https://doi.org/10.3390/analytica5010008 - 5 Mar 2024
Abstract
This study focuses on evaluating the characteristics of olive oil produced in the Taroudant province (southern Morocco), making this the first comprehensive study focusing on olive oil from the ‘Moroccan Picholine’ cultivar. Our objective was to elucidate the distinctive qualities of olive oil
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This study focuses on evaluating the characteristics of olive oil produced in the Taroudant province (southern Morocco), making this the first comprehensive study focusing on olive oil from the ‘Moroccan Picholine’ cultivar. Our objective was to elucidate the distinctive qualities of olive oil from this region, providing valuable insights into its potential contributions to the country’s olive oil sector. For this purpose, several quality criteria (free fatty acids, moisture content, saponification value, and iodine value), oxidation indices (peroxide value, specific UV extinction coefficients, and oxidizability value), and purity indices (fatty acids and sterol composition) were evaluated. Our results reveal minor-to-significant variations (p < 0.05) in the quality and oxidation parameters. Specifically, our results indicate diverse ranges for free fatty acids (0.33–3.62 g/100 g), peroxide values (0.85–4.01 mEq O2/kg oil), K232 (1.68 to 2.73), and K270 (0.09–0.34). Furthermore, consistently high levels of oleic acid (55.8 to 73.1%) and β-sitosterol (94.2 to 97%) were observed in the studied samples. These outcomes were confirmed through the use principal component analysis and hierarchical cluster analysis. Likewise, important correlations were outlined among the studied parameters. Multidimensional analyses not only highlight inherent variations, but also facilitate the classification of the analyzed olive oils into distinct categories. The results suggest that the Taroudant province exhibits favorable conditions for producing high-quality olive oil.
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(This article belongs to the Collection Analytical and Applied Chemistry: the challenges and opportunities for growth in the 21st century)
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Characterization of Bixin by UV-Visible Spectroscopy and HPLC, and Its Application as Latent Fingermark Developer
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Danielle Tapia Bueno, Amanda Fonseca Leitzke, Rosane Lopes Crizel, Cristina Jansen-Alves, Emanuel Gomes Bertizzolo, Juliana Porciuncula da Silva, Gabrielly Quartieri Sejanes, Kristiane de Cássia Mariotti and Claudio Martin Pereira de Pereira
Analytica 2024, 5(1), 107-118; https://doi.org/10.3390/analytica5010007 - 3 Mar 2024
Abstract
Fingerprints are essential for human identification and are valuable tools in criminal investigations. The pursuit of new materials for digital printing is expanding, with increasing interest in natural compounds such as bixin, sourced from annatto seeds. Despite its traditional use as a natural
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Fingerprints are essential for human identification and are valuable tools in criminal investigations. The pursuit of new materials for digital printing is expanding, with increasing interest in natural compounds such as bixin, sourced from annatto seeds. Despite its traditional use as a natural dye with medicinal properties, the potential of bixin in papilloscopy remains largely untapped. In this study, we meticulously extracted bixin from annatto seeds and meticulously developed composites incorporating zinc carbonate (bixin/ZnCO3) and kaolinite (bixin/kaolinite). UV-visible spectroscopy was used for characterization, and the extracted bixin showed absorption peaks at 429, 453, and 481 nm, which were very similar to standard peaks at 429, 457, and 487 nm. The two samples also had the same retention times (7.07 min) according to further liquid chromatography analysis. Sweat pores were easier to detect thanks to the effectiveness of the bixin/ZnCO3 and bixin/kaolinite composites in creating high contrast sebaceous and natural latent fingerprints. These results highlight the composites’ potential as novel and fascinating instruments for papilloscopy applications, which might also improve forensic investigations.
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(This article belongs to the Collection Analytical and Applied Chemistry: the challenges and opportunities for growth in the 21st century)
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Optimization of Pulsed Electric Field-Based Extraction of Bioactive Compounds from Cannabis sativa Leaves
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Dimitrios Mpakos, Theodoros Chatzimitakos, Vassilis Athanasiadis, Martha Mantiniotou, Eleni Bozinou and Stavros I. Lalas
Analytica 2024, 5(1), 90-106; https://doi.org/10.3390/analytica5010006 - 4 Feb 2024
Abstract
The current investigation examines the application of pulsed electric fields (PEFs) for isolating polyphenols from Cannabis sativa var. Futura 75 leaves. Firstly, the solvent composition, which included ethanol, water, and various mixtures of the two, was explored, along with the liquid-to-solid ratio. Subsequently,
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The current investigation examines the application of pulsed electric fields (PEFs) for isolating polyphenols from Cannabis sativa var. Futura 75 leaves. Firstly, the solvent composition, which included ethanol, water, and various mixtures of the two, was explored, along with the liquid-to-solid ratio. Subsequently, the primary parameters associated with PEFs (namely, pulse duration, pulse period, electric field intensity, and treatment duration) were optimized. The extracted samples were analyzed to determine their total polyphenol content (TPC), and individual polyphenols were also evaluated through high-performance liquid chromatography. In addition, the antioxidant activity of the extracts was assessed through ferric-reducing antioxidant power (FRAP) and DPPH assays. The extracts prepared utilizing PEFs were compared to the extracts obtained without PEFs in terms of their TPC, FRAP values, and DPPH activity. The results indicate that the most effective extraction parameters were a pulse duration of 10 μs, a pulse period of 1000 μs, and an electric field strength of 0.9 kV/cm after 25 min of extraction. The most efficient solvent was determined to be a 50% (v/v) mixture of ethanol and water in a 20:1 liquid-to-solid ratio. The extract obtained under the optimal conditions exhibited a ~75% increase in TPC compared to the extract obtained without any application of PEFs, while some individual polyphenols exhibited an increase of up to ~300%. Furthermore, significant increases of ~74% and ~71% were observed in FRAP and DPPH assays. From the information provided, it was observed that the tested variables had an impact on the recovery of polyphenols from C. sativa leaves.
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(This article belongs to the Collection Analytical and Applied Chemistry: the challenges and opportunities for growth in the 21st century)
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Open AccessArticle
Disposable Voltammetric Immunosensor for Determination and Quantification of Biomarker CA 15-3 in Biological Specimens
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Ana Elisa F. Oliveira, Arnaldo César Pereira, Mayra A. C. Resende and Lucas Franco Ferreira
Analytica 2024, 5(1), 74-89; https://doi.org/10.3390/analytica5010005 - 2 Feb 2024
Abstract
A disposable voltammetric immunosensor was developed to measure breast cancer biomarker 15-3 (CA 15-3) in human saliva and serum samples. Screen-printed paper-based electrodes (f-SPE) previously fabricated by our research group using homemade conductive inks were used as transducers, which were later modified only
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A disposable voltammetric immunosensor was developed to measure breast cancer biomarker 15-3 (CA 15-3) in human saliva and serum samples. Screen-printed paper-based electrodes (f-SPE) previously fabricated by our research group using homemade conductive inks were used as transducers, which were later modified only with gold nanoparticles to immobilize anti-CA 15-3 antibodies. The sensor was operated using antigen–antibody interactions in conjunction with a redox species (ferrocyanide potassium) for the indirect determination of the CA 15-3 antigen. The device characterization involved atomic force microscopy (AFM) and electrochemical analysis. Optimization of the construction and response of the immunosensor was achieved at incubation times of 6 h for anti-CA 15-3, 1 h for bovine serum albumin, and 1 h for interaction with CA 15-3. The sensor displays a linear range between 2 and 16 U/mL, with a sensitivity of 0.012 μA/U mL−1, a limit of detection (LOD) of 0.56 U/mL, and a limit of quantification (LOQ) of 1.88 U/mL. The interfering substances minimally affected the signal, with 4.94% response variation, and the reproducibility of the immunosensor demonstrated a relative standard deviation (RSD) of 5.65%. The sensor successfully determined the CA 15-3 concentration in human serum and saliva, demonstrating its potential for clinical analysis.
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(This article belongs to the Collection Analytical and Applied Chemistry: the challenges and opportunities for growth in the 21st century)
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Insights into Analytical Precision: Understanding the Factors Influencing Accurate Vitamin A Determination in Various Samples
by
Yauheni Shastak, Wolf Pelletier and Andrea Kuntz
Analytica 2024, 5(1), 54-73; https://doi.org/10.3390/analytica5010004 - 2 Feb 2024
Cited by 1
Abstract
The accurate assessment of vitamin A in animal feed and tissues is vital for safeguarding animal well-being and ensuring high-quality nutritional feed. However, challenges in achieving precise results persist, necessitating a comprehensive understanding of the influencing factors. This review delves into the historical
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The accurate assessment of vitamin A in animal feed and tissues is vital for safeguarding animal well-being and ensuring high-quality nutritional feed. However, challenges in achieving precise results persist, necessitating a comprehensive understanding of the influencing factors. This review delves into the historical progression of analytical techniques, from colorimetric assays and spectrophotometry to advanced chromatographic methods and non-destructive spectroscopic approaches. Factors influencing analytical precision are scrutinized, encompassing sample preparation, storage conditions, interfering substances, and human errors. The crucial role of quality control and standardized protocols in ensuring the reproducibility and reliability of results is emphasized. Moreover, this review highlights the need for tailored analytical approaches to account for the complexities of sample matrices and the significance of cutting-edge technologies, including on-site analysis and data science integration, in enhancing analytical precision. By acknowledging the challenges and prospects in vitamin A analysis, this paper provides insights for optimizing analytical methodologies and promoting animal welfare and product safety.
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(This article belongs to the Collection Analytical and Applied Chemistry: the challenges and opportunities for growth in the 21st century)
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Open AccessArticle
1H-NMR-Based Chemometric Analysis of Echinacea Species to Predict Effectors of Myeloid Progenitor Stimulation
by
Suresh K. Nagumalli, Joshua T. Salley and Jeffrey D. Carstens
Analytica 2024, 5(1), 28-53; https://doi.org/10.3390/analytica5010003 - 13 Jan 2024
Cited by 1
Abstract
Echinacea, a herbaceous, perennial flowering plant from the Compositae (Asteraceae) family, exhibits stimulating effects on myeloid progenitors (CFU-GMs) in rat bone marrow, as demonstrated in our previous study using a 75% (v v−1) ethanol extract of aerial parts. Expanding on
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Echinacea, a herbaceous, perennial flowering plant from the Compositae (Asteraceae) family, exhibits stimulating effects on myeloid progenitors (CFU-GMs) in rat bone marrow, as demonstrated in our previous study using a 75% (v v−1) ethanol extract of aerial parts. Expanding on this work, we have investigated eleven different Echinacea samples that belong to three species for their myeloid progenitor-stimulating activity. Simultaneously, we employed 1H-NMR spectroscopy (400 MHz, 0.02–10.02 ppm) and chemometric analysis to predict constituents responsible for activity. Female Sprague–Dawley rats received oral doses of ethanol extracts (0–200 mg extract dry weight kg−1 body weight) of Echinacea for seven days. Bone marrow cells were then cultured with CFU-GM growth factors. Extracts showing a statistically significant (p < 0.05) increase in CFU-GM, compared to the control, were considered active. Significant CFU-GM increases were observed in rats treated with seven Echinacea samples, ranging from 39% to 91% higher than the control, while four samples were inactive. All five Echinacea purpurea samples showed myeloid progenitor-stimulating activity, while one sample each of Echinacea angustifolia and Echinacea pallida also exhibited the same activity. By applying orthogonal partial least squares discriminant analysis (OPLS-DA) to the 1H-NMR spectra, we identified specific spectral bins (0.70–1.98 ppm aliphatic and 6.38–7.76 ppm aromatic) correlating with myelopoiesis stimulation. These findings highlight the potential of chemometric analysis using 1H-NMR spectroscopy to infer the chemical classes that could be responsible for the bioactive properties of complex herbal mixtures, like Echinacea.
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(This article belongs to the Section Chemometrics)
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A Pre-Trial Study to Identify Species of Origin in Halloumi Cheese Utilising Chemometrics with Near-Infrared and Hyperspectral Imaging Technologies
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Maria Tarapoulouzi, Natasha Logan, Mike Hardy, Holly Montgomery, Simon A. Haughey, Christopher T. Elliott and Charis R. Theocharis
Analytica 2024, 5(1), 17-27; https://doi.org/10.3390/analytica5010002 - 9 Jan 2024
Abstract
Halloumi cheese has recently gained a Protected Designation of Origin (PDO) indicator, which is related to the place (Cyprus) in which halloumi cheese is made. The PDO label is linked with several requirements, e.g., milk species, quantities, etc.; thus, it is important to
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Halloumi cheese has recently gained a Protected Designation of Origin (PDO) indicator, which is related to the place (Cyprus) in which halloumi cheese is made. The PDO label is linked with several requirements, e.g., milk species, quantities, etc.; thus, it is important to study this product regarding authenticity. The utility of using two spectroscopic techniques, hyperspectral imaging (HSI) (400–1000 nm) and conventional near-infrared spectroscopy (NIR) (800–2500 nm) were assessed for the discrimination of 17 Cypriot halloumi cheese types, which could be categorized as of cow or goat–sheep origin. The aim of this study was to obtain spectral information for halloumi cheese using other promising infrared and imaging spectroscopic techniques as a comparison to a previously acquired mid-infrared (MIR) spectroscopy dataset. NIR and HSI are both fast and easy techniques in application, both of which provide significant information in food analysis. Chemometric analysis was crucial for interpreting the spectroscopic data by applying the unsupervised methods: principal component analysis (PCA) and hierarchical cluster analysis (HCA). The HSI model was found to be based intuitively on the appearance of cheese samples after freeze-drying (e.g., color; yellow/white, and texture; oily/dry), while the NIR grouping of samples was determined to be based on composition, mainly fat, protein and lactose content of the cheese samples. The HSI model returned distinct clusters of the two halloumi cheese types, cow and goat–sheep origin, with one outlier (16/17 accuracy; 94%), while the NIR model proved less accurate (13/17; 76%).
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(This article belongs to the Collection Analytical and Applied Chemistry: the challenges and opportunities for growth in the 21st century)
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Determination of the Active Pharmaceutical Ingredients in Saridon Tablets Using an Economical and Sensitive Thin Layer Chromatography Method Combined with Densitometry
by
Alina Pyka-Pająk
Analytica 2024, 5(1), 1-16; https://doi.org/10.3390/analytica5010001 - 2 Jan 2024
Abstract
A new TLC–densitometric method has been developed for the identification and quantification of paracetamol (PA), propyphenazone (PP) and caffeine (C) in Saridon tablets using the NP-TLC technique combined with densitometry. This method allows for the simultaneous determination of PA, PP, and C in
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A new TLC–densitometric method has been developed for the identification and quantification of paracetamol (PA), propyphenazone (PP) and caffeine (C) in Saridon tablets using the NP-TLC technique combined with densitometry. This method allows for the simultaneous determination of PA, PP, and C in the same sample. Among all the tested chromatographic conditions, the mixture consisting of chloroform + toluene + ethyl acetate + ethanol + acetic acid (18:18:7.5:5.0:0.3, v/v/v/v/v) and a silica gel 60F254 plate proved to be the most effective for the separation of the three tested active pharmaceutical ingredients (APIs) and substances related to paracetamol. The full validation of the proposed NP-TLC method proved that it is specific, precise, accurate, robust and sensitive. The percentage content in relation to the content declared by the manufacturer was for propyphenazone 99.8%, paracetamol 101.6% and caffeine 100.8%, which was in accordance with pharmacopoeial requirements. The results presented indicate the possibility of using the developed method in the routine control of pharmaceutical preparations containing these APIs. The proposed method is economical and more sensitive compared to the previously proposed planar methods for the simultaneous determination of APIs. What is more, the presented method may be an excellent economical alternative when the HPLC method is unavailable for such a determination.
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(This article belongs to the Special Issue New Analytical Techniques and Methods in Pharmaceutical Science)
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Physicochemical and Microstructural Characteristics of Sulfated Polysaccharide from Marine Microalga
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Diana Fimbres-Olivarria, Jorge Marquez-Escalante, Karla G. Martínez-Robinson, Valeria Miranda-Arizmendi, Yubia De Anda-Flores, Agustín Rascon-Chu, Francisco Brown-Bojorquez and Elizabeth Carvajal-Millan
Analytica 2023, 4(4), 527-537; https://doi.org/10.3390/analytica4040036 - 5 Dec 2023
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Marine algae are a valuable source of polysaccharides. However, the information available on sulfated polysaccharides from microalgae is limited. Navicula sp. is a microalga present in the Sea of Cortez, of which little is known regarding their polysaccharides’ properties. This study investigated the
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Marine algae are a valuable source of polysaccharides. However, the information available on sulfated polysaccharides from microalgae is limited. Navicula sp. is a microalga present in the Sea of Cortez, of which little is known regarding their polysaccharides’ properties. This study investigated the physicochemical and microstructural characteristics of Navicula sp. sulfated polysaccharide (NSP). The Fourier transform infrared spectrum of NSP showed distinctive bands (1225 and 820 cm−1, assigned to S–O and C–O–S stretching, respectively), confirming the molecular identity. NSP registered molecular weight, intrinsic viscosity, a radius of gyration, and a hydrodynamic radius of 1650 kDa, 197 mL/g, 61 nm, and 36 nm, respectively. The zeta potential, electrophoretic mobility, conductivity, and diffusion coefficient of the molecule were −5.8 mV, −0.45 µm cm/s V, 0.70 mS/cm, and 2.9 × 10−9 cm2/s, respectively. The characteristic ratio and persistence length calculated for NSP were 4.2 and 1.3 nm, suggesting a nonstiff polysaccharide chain conformation. The Mark–Houwink–Sakurada α and K constants were 0.5 and 1.67 × 10−1, respectively, indicating a molecular random coil structure. NSP scanning electron microscopy revealed a rough and porous surface. Knowing these polysaccharides’ physicochemical and microstructural characteristics can be the starting point for elucidating their structure–function relationship as a valuable tool in advanced biomaterial design.
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Development and Characterization of Conductive Ink Composed of Graphite and Carbon Black for Application in Printed Electrodes
by
Thaís Cristina de Oliveira Cândido, Arnaldo César Pereira and Daniela Nunes da Silva
Analytica 2023, 4(4), 513-526; https://doi.org/10.3390/analytica4040035 - 4 Dec 2023
Cited by 2
Abstract
This work developed a conductive ink composed of carbonaceous material for printing electrochemical sensors. The optimized ink comprises graphite, carbon black, and nail polish, respectively (35.3:11.7:53%), as well as acetone as a solvent. The proportion was optimized with consideration of the binder’s solubilization,
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This work developed a conductive ink composed of carbonaceous material for printing electrochemical sensors. The optimized ink comprises graphite, carbon black, and nail polish, respectively (35.3:11.7:53%), as well as acetone as a solvent. The proportion was optimized with consideration of the binder’s solubilization, the ink’s suitability for the screen-printing process, and lower electrical resistance. The materials used, and the resulting ink, were analyzed by way of Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), Raman spectroscopy, electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV). The charge transfer resistance (Rct) obtained was 0.348 kΩ. The conductive ink was used to print an electrode on a PET substrate, and a flexible and disposable electrode was obtained. The electroactive area obtained was 13.7 cm2, which was calculated by the Randles-Sevcik equation. The applicability of the device was demonstrated with a redox probe, providing a sensitivity of 0.02 µ A L mmol−1. The conductive ink has adequate homogeneity for producing electrodes using the screen-printing technique, with a low estimated production cost of $ 0.09 mL−1.
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(This article belongs to the Section Electroanalysis)
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Oxidative Stability of Virgin and Refined Argan [Argania spinosa L. (Skeels)] Oil under Accelerated Aging Conditions and Shelf-Life Prediction at Room Temperature: A Comparative Study
by
Rabha Aissa, Abderrahim Asbbane, Samira Oubannin, Laila Bijla, Zahra Bousaid, Otmane Hallouch, Said El Harkaoui, Bertrand Matthäus, El Hassan Sakar and Saïd Gharby
Analytica 2023, 4(4), 500-512; https://doi.org/10.3390/analytica4040034 - 2 Dec 2023
Cited by 2
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Argan kernels, fruits regurgitated by goats, are 30% cheaper than the regular kernels used to prepare food argan oil. The use of such argan kernels as a cosmetic ingredient, after refining, is thus economically attractive. The oxidative stability of argan oil prepared from
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Argan kernels, fruits regurgitated by goats, are 30% cheaper than the regular kernels used to prepare food argan oil. The use of such argan kernels as a cosmetic ingredient, after refining, is thus economically attractive. The oxidative stability of argan oil prepared from sub-quality kernels is not known. In the present paper, the physicochemical quality, oxidative stability indices, and bioactive compounds of refined argan oil (RAO) obtained from sub-quality kernels and virgin argan oil (VAO) were compared and evaluated over a period of storage of 12 weeks at 60 °C. Quality parameters consisted of free fatty acids (FFAs), peroxide value (PV), p-anisidine value (p-AV), UV extinction coefficients (K232 and K270), total oxidation, iodine and saponification values, induction time, fatty acid composition, and tocopherol content. Our outcomes reveal that the combined effects of refining and storage generally resulted in high values of the routinely measured quality indices, including FFA, p-AV, K270, K232, and PV. Likewise, refining reduced the levels of individual tocopherols and unsaturated fatty acids (USFAs) but increased saturated fatty acids (SFAs). Similar trends were observed under storage with decreased levels of tocopherols and high SFA for both RAO and VAO. Storage also resulted in an increased level of USFAs in the case of RAO but not in VAO. The obtained results show that RAO was more sensitive to oxidation than VAO. At room temperature, RAO had a shorter induction time of six months, implying that RAO will have a shorter shelf life compared to VAR. Thus, such instability means that the refining process for argan oil must be carried out with great care, and this oil needs to be protected once refined.
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