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Analytica, Volume 5, Issue 1 (March 2024) – 9 articles

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14 pages, 473 KiB  
Article
Analytical Compatibility between Various Techniques for Determining Dissolved Manganese in Produced Water
by Gabriela Knippelberg Bifano Manea, Vanusa Bueno Freire, Rainerio Escalfoni Junior and Elcio Cruz de Oliveira
Analytica 2024, 5(1), 139-152; https://0-doi-org.brum.beds.ac.uk/10.3390/analytica5010009 - 15 Mar 2024
Cited by 1 | Viewed by 931
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 [...] Read more.
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. Full article
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20 pages, 4115 KiB  
Article
Physicochemical Characterization of ‘Moroccan Picholine’ Olive (Olea europaea L.) Oil Produced in Southern Morocco Using Multivariate Statistical Analysis
by Jamila Gagour, Otmane Hallouch, Abderrahim Asbbane, Abdellatif Laknifli, El Hassan Sakar, Khalid Majourhat and Said Gharby
Analytica 2024, 5(1), 119-138; https://0-doi-org.brum.beds.ac.uk/10.3390/analytica5010008 - 5 Mar 2024
Cited by 2 | Viewed by 1266
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 [...] Read more.
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. Full article
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12 pages, 7154 KiB  
Article
Characterization of Bixin by UV-Visible Spectroscopy and HPLC, and Its Application as Latent Fingermark Developer
by 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://0-doi-org.brum.beds.ac.uk/10.3390/analytica5010007 - 3 Mar 2024
Viewed by 871
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 [...] Read more.
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. Full article
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17 pages, 2278 KiB  
Article
Optimization of Pulsed Electric Field-Based Extraction of Bioactive Compounds from Cannabis sativa Leaves
by Dimitrios Mpakos, Theodoros Chatzimitakos, Vassilis Athanasiadis, Martha Mantiniotou, Eleni Bozinou and Stavros I. Lalas
Analytica 2024, 5(1), 90-106; https://0-doi-org.brum.beds.ac.uk/10.3390/analytica5010006 - 4 Feb 2024
Cited by 1 | Viewed by 1136
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, [...] Read more.
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. Full article
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16 pages, 3602 KiB  
Article
Disposable Voltammetric Immunosensor for Determination and Quantification of Biomarker CA 15-3 in Biological Specimens
by Ana Elisa F. Oliveira, Arnaldo César Pereira, Mayra A. C. Resende and Lucas Franco Ferreira
Analytica 2024, 5(1), 74-89; https://0-doi-org.brum.beds.ac.uk/10.3390/analytica5010005 - 2 Feb 2024
Viewed by 943
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 [...] Read more.
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. Full article
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20 pages, 1654 KiB  
Review
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://0-doi-org.brum.beds.ac.uk/10.3390/analytica5010004 - 2 Feb 2024
Cited by 1 | Viewed by 1301
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 [...] Read more.
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. Full article
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26 pages, 9269 KiB  
Article
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://0-doi-org.brum.beds.ac.uk/10.3390/analytica5010003 - 13 Jan 2024
Cited by 1 | Viewed by 1050
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 [...] Read more.
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. Full article
(This article belongs to the Section Chemometrics)
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11 pages, 2299 KiB  
Article
A Pre-Trial Study to Identify Species of Origin in Halloumi Cheese Utilising Chemometrics with Near-Infrared and Hyperspectral Imaging Technologies
by 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://0-doi-org.brum.beds.ac.uk/10.3390/analytica5010002 - 9 Jan 2024
Viewed by 1340
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 [...] Read more.
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%). Full article
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16 pages, 1071 KiB  
Article
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://0-doi-org.brum.beds.ac.uk/10.3390/analytica5010001 - 2 Jan 2024
Viewed by 1351
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 [...] Read more.
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. Full article
(This article belongs to the Special Issue New Analytical Techniques and Methods in Pharmaceutical Science)
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