molecules-logo

Journal Browser

Journal Browser

Development of Analytical Methods in Food, Biological and Environmental Samples Determination

A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (28 February 2022) | Viewed by 35606

Special Issue Editors


E-Mail Website
Guest Editor
Department of Physical Chemistry, Medical University of Lublin, Chodźki 4a, 20-093 Lublin, Poland
Interests: separation of biologically active compounds with chromatographic and electromigrational techniques; with the use of various mobile phases; including those containing surfactants
Special Issues, Collections and Topics in MDPI journals

E-Mail Website
Guest Editor
Faculty of Chemistry and Pharmacy, University of Sofia Saint Kliment Ohridski, 1164 Sofia, Bulgaria
Interests: analytical atomic spectroscopy; speciation analysis; methods for separation and concentration; analysis of environmental samples, biological samples, food samples and beverages; development of analytical procedures; ecolegislation
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Scientists are still looking for new or improved methods for the determination of many compounds in various sample types. The determined solutes have various origins and their actions toward humans or animals can be positive or negative. Thus, the development of a method that leads to the identification and then determination of minor or even ultra-minor is important. The problem to be solved is not only the detection of a very small amount of analyte but also how to deal with the matrix problem. The latter may be food, biological, or even environmental.

The successful separation and then identification compounds contribute to the achievement of many analytical methods. Distinguishing mixture compounds is based on differences in their physicochemical properties, and various techniques are involved (chromatographic, spectroscopic, electroanalytical). Some of these techniques enhance sensitivity and are linked with various detection techniques (electrochemical, DAD, NMR, MS).

I encourage our colleagues to share their scientific achievements in the field of analytical method development in this Special Issue. Papers on the determination of solutes in food, biological, and environmental samples are especially welcome but the issue is not confined to these topics. 

Dr. Beata Polak
Dr. Irina B. Karadjova
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. Molecules 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 2700 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

  • determination of various compounds
  • electromigrational
  • chromatographic
  • spectral methods
  • various matrices

Related Special Issues

Published Papers (10 papers)

Order results
Result details
Select all
Export citation of selected articles as:

Research

Jump to: Review

12 pages, 1580 KiB  
Article
Monitoring Farmed Fish Welfare by Measurement of Cortisol as a Stress Marker in Fish Feces by Liquid Chromatography Coupled with Tandem Mass Spectrometry
by Vanessa Andrea Meling, Kjetil Berge, David Lausten Knudsen, Per Ola Rønning and Cato Brede
Molecules 2022, 27(8), 2481; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27082481 - 12 Apr 2022
Cited by 5 | Viewed by 2445
Abstract
The aquaculture industry has become a sustainable source of food for humans. Remaining challenges include disease issues and ethical concerns for the discomfort and stress of farmed fish. There is a need for reliable biomarkers to monitor welfare in fish, and the stress [...] Read more.
The aquaculture industry has become a sustainable source of food for humans. Remaining challenges include disease issues and ethical concerns for the discomfort and stress of farmed fish. There is a need for reliable biomarkers to monitor welfare in fish, and the stress hormone cortisol has been suggested as a good candidate. This study presents a novel method for measurement of cortisol in fish feces based on enzymatic hydrolysis, liquid–liquid extraction, derivatization, and finally instrumental analysis by liquid chromatography coupled with tandem mass spectrometry. Hydrolysis and extraction conditions were optimized. Cortisol appeared to be mostly conjugated to sulfate and less conjugated to glucuronic acid in the studied samples of feces from farmed Atlantic salmon. The method was suitable for quantification of cortisol after enzymatic deconjugation by either combined glucuronidase and sulfatase activity, or by glucuronidase activity alone. The limit of detection was 0.15 ng/g, the limit of quantification was 0.34 ng/g, and the method was linear (R2 > 0.997) up to 380 ng/g, for measurement of cortisol in wet feces. Method repeatability and intermediate precision were acceptable, both with a coefficient of variation (CV) of 11%. Stress level was high in fish released into seawater, and significantly reduced after eight days. Full article
Show Figures

Figure 1

10 pages, 1928 KiB  
Article
Modified Natural Rubber as a Simple Chemical Sensor with Smartphone Detection for Formaldehyde Content in a Seafood Sample
by Chonnipa Yeerum, Piyanat Issarangkura Na Ayutthaya, Kullapon Kesonkan, Kanokwan Kiwfo, Ploenpit Boochathum, Kate Grudpan and Monnapat Vongboot
Molecules 2022, 27(7), 2159; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27072159 - 27 Mar 2022
Cited by 3 | Viewed by 2565
Abstract
A new biodegradable platform-based sensor for formaldehyde assay is proposed. Natural rubber latex was modified to polylactic acid–chloroacetated natural rubber polymer blend sheets. The polymer blend sheet was grafted using a water-based system with amine monomers as a platform, with a spot exhibiting [...] Read more.
A new biodegradable platform-based sensor for formaldehyde assay is proposed. Natural rubber latex was modified to polylactic acid–chloroacetated natural rubber polymer blend sheets. The polymer blend sheet was grafted using a water-based system with amine monomers as a platform, with a spot exhibiting positive polarity for immobilizing with anionic dye (Acid Red 27). The sensor was exposed to formaldehyde. The color intensity of the dye on the sensor spot would decrease. Using a smartphone with image processing (via ImageJ program), the color intensity change (∆B) could be followed. A linear calibration, ∆B intensity = 0.365 [FA] + 6.988, R2 = 0.997, was obtained for 10–150 mM FA with LOD and LOQ at 3 and 10 mM, respectively (linear regression method). The precision was lower than 20% RSD. Application to real seafood samples was demonstrated. The ready-to-use sensor with the proposed method was cost-effective, was portable for on-site analysis, and demonstrated green chemical analysis. Full article
Show Figures

Figure 1

16 pages, 3023 KiB  
Article
Highly Sensitive Determination of Tenofovir in Pharmaceutical Formulations and Patients Urine—Comparative Electroanalytical Studies Using Different Sensing Methods
by Natalia Festinger, Kaja Spilarewicz-Stanek, Kamila Borowczyk, Dariusz Guziejewski and Sylwia Smarzewska
Molecules 2022, 27(6), 1992; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27061992 - 19 Mar 2022
Cited by 8 | Viewed by 2661
Abstract
This paper discusses the electrochemical behavior of antiviral drug Tenofovir (TFV) and its possible applicability towards electroanalytical determination with diverse detection strategies using square-wave voltammetry. Namely, oxidation processes were investigated using glassy carbon electrode with graphene oxide surface modification (GO/GCE), while the reduction [...] Read more.
This paper discusses the electrochemical behavior of antiviral drug Tenofovir (TFV) and its possible applicability towards electroanalytical determination with diverse detection strategies using square-wave voltammetry. Namely, oxidation processes were investigated using glassy carbon electrode with graphene oxide surface modification (GO/GCE), while the reduction processes, related to the studied analyte, were analyzed at a renewable silver amalgam electrode (Hg(Ag)FE). Scanning electron microscopy imaging confirmed the successful deposition of GO at the electrode surface. Catalytic properties of graphene oxide were exposed while being compared with those of bare GCE. The resultant modification of GCE with GO enhanced the electroactive surface area by 50% in comparison to the bare one. At both electrodes, i.e., GO/GCE and Hg(Ag)FE, the TFV response was used to examine and optimize the influence of square-wave excitation parameters, i.e., square wave frequency, step potential and amplitude, and supporting electrolyte composition and its pH. Broad selectivity studies were performed with miscellaneous interfering agents influence, including ascorbic acid, selected saccharides and aminoacids, metal ions, non-opioid analgesic metamizole, non-steroidal anti-inflammatory drug omeprazole, and several drugs used along with TFV treatment. The linear concentration range for TFV determination at GO/GCE and Hg(Ag)FE was found to be 0.3–30.0 µmol L–1 and 0.5–7.0 µmol L–1, respectively. The lowest LOD was calculated for GO/GCE and was equal to 48.6 nmol L–1. The developed procedure was used to detect TFV in pharmaceutical formulations and patient urine samples and has referenced utilization in HPLC studies. Full article
Show Figures

Graphical abstract

15 pages, 2587 KiB  
Article
Pharmacokinetic Characterization of the DDAH1 Inhibitors ZST316 and ZST152 in Mice Using a HPLC-MS/MS Method
by Arduino A. Mangoni, Tommaso Ceruti, Roberta Frapolli, Massimo Russo, Stefania Fichera, Massimo Zucchetti and Sara Tommasi
Molecules 2022, 27(3), 1017; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27031017 - 02 Feb 2022
Cited by 5 | Viewed by 1685
Abstract
The pharmacokinetic profile of ZST316 and ZST152, arginine analogues with inhibitory activity towards human dimethylarginine dimethylaminohydrolase-1 (DDAH1), was investigated in mice using a newly developed HPLC-MS/MS method. The method proved to be reproducible, precise, and accurate for the measurement of the compounds in [...] Read more.
The pharmacokinetic profile of ZST316 and ZST152, arginine analogues with inhibitory activity towards human dimethylarginine dimethylaminohydrolase-1 (DDAH1), was investigated in mice using a newly developed HPLC-MS/MS method. The method proved to be reproducible, precise, and accurate for the measurement of the compounds in plasma and urine. Four-week-old female FVB mice received a single dose of ZST316 and ZST152 by intravenous bolus (30 mg/Kg) and oral gavage (60 mg/Kg). ZST316 Cmax was 67.4 µg/mL (intravenous) and 1.02 µg/mL (oral), with a half-life of 6 h and bioavailability of 4.7%. ZST152 Cmax was 24.9 µg/mL (intravenous) and 1.65 µg/mL (oral), with a half-life of 1.2 h and bioavailability of 33.3%. Urinary excretion of ZST152 and ZST316 was 12.5%–22.2% and 2.3%–7.5%, respectively. At least eight urinary metabolites were identified. After chronic intraperitoneal treatment with the more potent DDAH1 inhibitor, ZST316 (30 mg/Kg/day for three weeks), the bioavailability was 59% and no accumulation was observed. Treatment was well tolerated with no changes in body weight vs. untreated animals and no clinical signs of toxicity or distress. The results of this study show that ZST316 has a favorable pharmacokinetic profile, following intraperitoneal administration, to investigate the effects of DDAH1 inhibition in mice. Full article
Show Figures

Figure 1

12 pages, 1604 KiB  
Article
A New Approach for Determination of the Botanical Origin of Monofloral Bee Honey, Combining Mineral Content, Physicochemical Parameters, and Self-Organizing Maps
by Tsvetomil Voyslavov, Elisaveta Mladenova and Ralitsa Balkanska
Molecules 2021, 26(23), 7219; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26237219 - 28 Nov 2021
Cited by 10 | Viewed by 2080
Abstract
A new approach for the botanical origin determination of monofloral bee honey is developed. The methodology combines mineral content and physicochemical parameters determination with intelligent statistics such as self-organizing maps (SOMs). A total of 62 monofloral bee honey samples were analysed, including 31 [...] Read more.
A new approach for the botanical origin determination of monofloral bee honey is developed. The methodology combines mineral content and physicochemical parameters determination with intelligent statistics such as self-organizing maps (SOMs). A total of 62 monofloral bee honey samples were analysed, including 31 linden, 14 rapeseed, 13 sunflower, and 4 acacia. All of them were harvested in 2018 and 2019 from trusted beekeepers, after confirming their botanical origin, using melissopalynological analysis. Nine physicochemical parameters were determined, including colour, water content, pH, electrical conductivity, hydroxymethylfurfural content, diastase activity, specific optical rotation, invertase activity, and proline. The content of thirty chemical elements (Ag, Al, As, B, Ba, Bi, Ca, Cd, Co, Cr, Cs, Cu, Fe, Ga, In, K, Li, Mg, Mn, Na, Ni, P, Pb, Rb, S, Se, Sr, Te, V, and Zn) was measured using ICP-OES, ICP-MS, and FAAS as instrumental techniques. The visualisation of the SOMs shows an excellent separation of honey samples in five well-defined clusters—linden, rapeseed, acacia, sunflower, and polyfloral honey—using the following set of 16 descriptors: diastase activity, hydroxymethylfurfural content, invertase activity, pH, specific optical rotation, water content, Al, B, Cr, Cs, K, Na, Ni, Rb, V, and Zn. Full article
Show Figures

Graphical abstract

12 pages, 1896 KiB  
Article
Imaging Flow Cytometry to Study Biofilm-Associated Microbial Aggregates
by Michał Konieczny, Peter Rhein, Katarzyna Czaczyk, Wojciech Białas and Wojciech Juzwa
Molecules 2021, 26(23), 7096; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26237096 - 24 Nov 2021
Cited by 11 | Viewed by 2683
Abstract
The aim of the research was to design an advanced analytical tool for the precise characterization of microbial aggregates from biofilms formed on food-processing surfaces. The approach combined imaging flow cytometry with a machine learning-based interpretation protocol. Biofilm samples were collected from three [...] Read more.
The aim of the research was to design an advanced analytical tool for the precise characterization of microbial aggregates from biofilms formed on food-processing surfaces. The approach combined imaging flow cytometry with a machine learning-based interpretation protocol. Biofilm samples were collected from three diagnostic points of the food-processing lines at two independent time points. The samples were investigated for the complexity of microbial aggregates and cellular metabolic activity. Thus, aggregates and singlets of biofilm-associated microbes were simultaneously examined for the percentages of active, mid-active, and nonactive (dead) cells to evaluate the physiology of the microbial cells forming the biofilm structures. The tested diagnostic points demonstrated significant differences in the complexity of microbial aggregates. The significant percentages of the bacterial aggregates were associated with the dominance of active microbial cells, e.g., 75.3% revealed for a mushroom crate. This confirmed the protective role of cellular aggregates for the survival of active microbial cells. Moreover, the approach enabled discriminating small and large aggregates of microbial cells. The developed tool provided more detailed characteristics of bacterial aggregates within a biofilm structure combined with high-throughput screening potential. The designed methodology showed the prospect of facilitating the detection of invasive biofilm forms in the food industry environment. Full article
Show Figures

Figure 1

8 pages, 777 KiB  
Communication
Validation of a Fast and Simple HPLC-UV Method for the Quantification of Adenosine Phosphates in Human Bronchial Epithelial Cells
by Ana Teresa Juarez-Facio, Violaine Martin de Lagarde, Christelle Monteil, Jean-Marie Vaugeois, Cécile Corbiere and Tiphaine Rogez-Florent
Molecules 2021, 26(20), 6324; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26206324 - 19 Oct 2021
Cited by 6 | Viewed by 2927
Abstract
A new HPLC method for the simultaneous quantitative analysis of adenosine triphosphate (ATP), adenosine diphosphate (ADP), and adenosine monophosphate (AMP) was developed and validated. ATP, ADP, and AMP were extracted from human bronchial epithelial cells with a rapid extraction procedure and separated with [...] Read more.
A new HPLC method for the simultaneous quantitative analysis of adenosine triphosphate (ATP), adenosine diphosphate (ADP), and adenosine monophosphate (AMP) was developed and validated. ATP, ADP, and AMP were extracted from human bronchial epithelial cells with a rapid extraction procedure and separated with a C18 column (3 × 150 mm, 2.7 µm) using isocratic elution with a mobile phase consisting of 50 mM of potassium hydrogen phosphate (pH 6.80). The absorbance was monitored at 254 nm. The calibration curves were linear in 0.2 to 10 µM, selective, precise, and accurate. This method allowed us to quantify the nucleotides from two cell models: differentiated NHBE primary cells grown at the air–liquid interface (ALI) and BEAS-2B cell line. Our study highlighted the development of a sensitive, simple, and green analytical method that is faster and less expensive than other existing methods to measure ATP, ADP, and AMP and can be carried out on 2D and 3D cell models. Full article
Show Figures

Graphical abstract

16 pages, 2690 KiB  
Article
Raffinose Capped Silver Nanoparticles: A New Localized Surface Plasmon Resonance Based Sensor for Selective Quantification of Cr(VI) in Waste Waters
by Penka Vasileva, Lubomir Djerahov and Irina Karadjova
Molecules 2021, 26(17), 5418; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26175418 - 06 Sep 2021
Cited by 3 | Viewed by 1838
Abstract
In this study, a new method for selective determination of Cr(VI) in water samples at pH 4 is presented using raffinose capped silver nanoparticles (Ag/Raff NPs) as an optical sensor. The method is based on the variation of LSPR absorption band intensity as [...] Read more.
In this study, a new method for selective determination of Cr(VI) in water samples at pH 4 is presented using raffinose capped silver nanoparticles (Ag/Raff NPs) as an optical sensor. The method is based on the variation of LSPR absorption band intensity as a result of electrostatic interaction between the negatively charged Ag/Raff NPs and positive Cr(III) ions, in-situ produced by chemical reduction of Cr(VI) with ascorbic acid, combined with the fast kinetics of Cr(III) coordination to the –OH groups of the capping agent on the nanoparticle surface, further causing the nanoparticle aggregation. The calibration curve for Cr(VI) is linear in the range 2.5–7.5 μmol L−1, the limit of quantification achieved is 1.9 μmol L−1, and values of relative standard deviation vary from 3 to 5% for concentration level 1.9–7.5 μmol L−1. The interference studies performed in the presence of various metal ions show very good selectivity of Ag/Raff NPs toward Cr(VI) species. The added–found method is used to confirm the accuracy and precision of developed analytical approach. Full article
Show Figures

Figure 1

Review

Jump to: Research

32 pages, 6407 KiB  
Review
High Performance Liquid Chromatography (HPLC) with Fluorescence Detection for Quantification of Steroids in Clinical, Pharmaceutical, and Environmental Samples: A Review
by Fatima Hameedat, Sahar Hawamdeh, Soraya Alnabulsi and Aref Zayed
Molecules 2022, 27(6), 1807; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27061807 - 10 Mar 2022
Cited by 15 | Viewed by 8811
Abstract
Steroids are compounds widely available in nature and synthesized for therapeutic and medical purposes. Although several analytical techniques are available for the quantification of steroids, their analysis is challenging due to their low levels and complex matrices of the samples. The efficiency and [...] Read more.
Steroids are compounds widely available in nature and synthesized for therapeutic and medical purposes. Although several analytical techniques are available for the quantification of steroids, their analysis is challenging due to their low levels and complex matrices of the samples. The efficiency and quick separation of the HPLC combined with the sensitivity, selectivity, simplicity, and cost-efficiency of fluorescence, make HPLC coupled to fluorescence detection (HPLC-FLD) an ideal tool for routine measurement and detection of steroids. In this review, we covered HPLC-FLD methods reported in the literature for the steroids quantification in clinical, pharmaceutical, and environmental applications, focusing on the various approaches of fluorescent derivatization. The aspects related to analytical methodology including sample preparation, derivatization reagents, and chromatographic conditions will be discussed. Full article
Show Figures

Graphical abstract

20 pages, 3792 KiB  
Review
Mapping the Chemistry of Hair Strands by Mass Spectrometry Imaging—A Review
by Mai H. Philipsen, Emma R. Haxen, Auraya Manaprasertsak, Per Malmberg and Emma U. Hammarlund
Molecules 2021, 26(24), 7522; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26247522 - 11 Dec 2021
Cited by 3 | Viewed by 6149
Abstract
Hair can record chemical information reflecting our living conditions, and, therefore, strands of hair have become a potent analytical target within the biological and forensic sciences. While early efforts focused on analyzing complete hair strands in bulk, high spatial resolution mass spectrometry imaging [...] Read more.
Hair can record chemical information reflecting our living conditions, and, therefore, strands of hair have become a potent analytical target within the biological and forensic sciences. While early efforts focused on analyzing complete hair strands in bulk, high spatial resolution mass spectrometry imaging (MSI) has recently come to the forefront of chemical hair-strand analysis. MSI techniques offer a localized analysis, requiring fewer de-contamination procedures per default and making it possible to map the distribution of analytes on and within individual hair strands. Applying the techniques to hair samples has proven particularly useful in investigations quantifying the exposure to, and uptake of, toxins or drugs. Overall, MSI, combined with optimized sample preparation protocols, has improved precision and accuracy for identifying several elemental and molecular species in single strands of hair. Here, we review different sample preparation protocols and use cases with a view to make the methodology more accessible to researchers outside of the field of forensic science. We conclude that—although some challenges remain, including contamination issues and matrix effects—MSI offers unique opportunities for obtaining highly resolved spatial information of several compounds simultaneously across hair surfaces. Full article
Show Figures

Figure 1

Back to TopTop