Research as Development Perspective

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Chromatographic Separations".

Deadline for manuscript submissions: closed (30 September 2018) | Viewed by 46643

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Laboratory of Analytical Chemistry, School of Chemistry, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece
Interests: analytical chemistry; sample preparation; chromatography; HPLC; method validation; method development; separation science; food analysis; bioanalysis; environmental analysis; green analytical chemistry; sorptive extraction; microextraction techniques
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Department of Chemistry, Aristotle University, 54124 Thessaloniki, Greece
Interests: hyphenated techniques and mass spectrometry; atomic spectrometry techniques; speciation analysis; sample pretreatment techniques; chemometrics
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

This Special Issue, “Research as Development Perspective”, is dedicated to data presented at the 1st Conference in Chemistry for Graduate, Postgraduate Students, and PhD candidates, at the Aristotle University of Thessaloniki, which is the outcome of research by young chemists in Northern Greece. The scope of this conference is to provide younger chemists, but also last year’s students, with the opportunity to be well prepared for their next career steps with respect to the increasing demands in the job-market. Moreover, they will have the possibility of presenting their scientific results to a large audience and strengthen their soft skills. Last, but not least, the active engagement of students in the organization of the conference aims to enhance their teamwork abilities, a skill considered as highly valuable for reaching professional maturity. The conference is organized by the Chemistry Department of the Aristotle University of Thessaloniki, the Association of Greek Chemists-Division of Central and Western Macedonia and the Association of Chemists in Northern Greece.

Scientific Topics covered in Special Issue

  • Analytical Chemistry-Quality Control
  • Inorganic-Bioinorganic Chemistry-Nanotechnology
  • Archaeometry-Maintenance and restoration of cultural monuments
  • Biochemistry-Clinical Chemistry
  • Chemical Education and Teaching
  • Organic Chemistry-Natural Products
  • Physical-Theoretical and Computational Chemistry
  • Toxicology-Medicinal Chemistry
  • Environmental Chemistry and Technology-Pollution Control
  • Polymer Chemistry and Technology
  • Food Chemistry and Technology
  • Chemical Technology-Materials- Green Chemistry

Prof. Dr. Victoria F. Samanidou
Prof. Dr. George Zachariadis
Guest Editors

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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. Separations is an international peer-reviewed open access monthly journal published by MDPI.

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Published Papers (7 papers)

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Research

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13 pages, 2151 KiB  
Article
NSAIDs Determination in Human Serum by GC-MS
by Adamantios Krokos, Elisavet Tsakelidou, Eleni Michopoulou, Nikolaos Raikos, Georgios Theodoridis and Helen Gika
Separations 2018, 5(3), 37; https://doi.org/10.3390/separations5030037 - 16 Jul 2018
Cited by 13 | Viewed by 6156
Abstract
Non-steroidal anti-inflammatory drugs (NSAIDs) are being widely consumed without medical prescription and are often the cause of intoxication, usually in young children. For this, there is a special need in their determination in routine toxicology analysis. As screening methods mainly focus on drugs [...] Read more.
Non-steroidal anti-inflammatory drugs (NSAIDs) are being widely consumed without medical prescription and are often the cause of intoxication, usually in young children. For this, there is a special need in their determination in routine toxicology analysis. As screening methods mainly focus on drugs of abuse (DOA) that are alkaline compounds in their majority, they are not optimized for acidic drugs, such as NSAIDs. Thus, more specific methods are needed for the detection and quantification of this class of drugs. In this study, the efficient extraction of NSAIDs from blood serum and their accurate determination is studied. Optimum pH extraction conditions were studied and thereafter different derivatization procedures for their detection. From the derivatization reagents used, N,O-Bis(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% Trimethylchlorosilane (TMCS) was found to be the optimum choice for the majority of the examined NSAIDs; pH of 3.7 was selected as the most efficient for the extraction step. Herein the formation of the lactam of diclofenac was also thoroughly investigated. The developed Gas Chromatography-Mass Spectrometry (GC-MS) method had a run time of 15 min with the mass spectrometer operating in Electron Impact (EI) within the mass range of 40 to 500 amu. The method was linear with R2 above 0.991 and limits of quantitation (LOQ) ranging from 6 to 414 ng/mL. The intra-day accuracy and precision were found between 1.03%–9.79% and 88%–110%, respectively, and the inter-day accuracy and precision were between 1.87%–10.79% and 91%–113%. The optimum protocol was successfully applied to real clinical samples, where intoxication of NSAIDs was suspected. Full article
(This article belongs to the Special Issue Research as Development Perspective)
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17 pages, 2995 KiB  
Article
Non-Destructive X-ray Spectrometric and Chromatographic Analysis of Metal Containers and Their Contents, from Ancient Macedonia
by Christos S. Katsifas, Despina Ignatiadou, Anastasia Zacharopoulou, Nikolaos Kantiranis, Ioannis Karapanagiotis and George A. Zachariadis
Separations 2018, 5(2), 32; https://doi.org/10.3390/separations5020032 - 11 Jun 2018
Cited by 8 | Viewed by 4024
Abstract
This work describes a holistic archaeometric approach to ancient Macedonian specimens. In the region of the ancient city Lete, the deceased members of a rich and important family were interred in a cluster of seven tombs (4th century BC). Among the numerous grave [...] Read more.
This work describes a holistic archaeometric approach to ancient Macedonian specimens. In the region of the ancient city Lete, the deceased members of a rich and important family were interred in a cluster of seven tombs (4th century BC). Among the numerous grave goods, there was also a set of metal containers preserving their original content. The physico-chemical analysis of the containers and their contents was performed in order to understand the purpose of their use. For the containers, Energy Dispersive micro-X-Ray Fluorescence (EDμXRF) spectroscopy was implemented taking advantage of its non-invasive character. The case (B35) and the small pyxis (B37) were made of a binary Cu-Sn alloy accompanied by a slight amount of impurities (Fe, Pb, As) and the two miniature bowls were made of almost pure Cu. For the study of the contents, a combination of EDμXRF, X-Ray Diffraction (XRD), and Gas Chromatography—Mass Spectrometry (GC-MS) was carried out. Especially for the extraction of the volatile compounds, the Solid Phase Micro-Extraction (SPME) technique was used in the headspace mode. Because of the detection of Br, High Pressure Liquid Chromatography coupled to a Diode-Array-Detector (HPLC-DAD) was implemented, confirming the existence of the ancient dye shellfish purple (porphyra in Greek). The analytical results of the combined implementation of spectrometric and chromatographic analytical techniques of the metal containers and their contents expand our knowledge about the pharmaceutical practices in Macedonia during the 4th century BC. Full article
(This article belongs to the Special Issue Research as Development Perspective)
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16 pages, 4780 KiB  
Article
Silk Fibroin Nanoparticles for Drug Delivery: Effect of Bovine Serum Albumin and Magnetic Nanoparticles Addition on Drug Encapsulation and Release
by Olga Gianak, Eleni Pavlidou, Charalambos Sarafidis, Vassilis Karageorgiou and Eleni Deliyanni
Separations 2018, 5(2), 25; https://doi.org/10.3390/separations5020025 - 23 Apr 2018
Cited by 36 | Viewed by 7158
Abstract
Silk fibroin nanoparticles were prepared in the present study based on phase separation between silk fibroin and polyvinyl alcohol. The drug encapsulation efficiency of the prepared nanoparticles was examined at a range of concentrations from 10 ppm to 500 ppm for pramipexole, curcumin, [...] Read more.
Silk fibroin nanoparticles were prepared in the present study based on phase separation between silk fibroin and polyvinyl alcohol. The drug encapsulation efficiency of the prepared nanoparticles was examined at a range of concentrations from 10 ppm to 500 ppm for pramipexole, curcumin, and propranolol hydrochloride. Silk fibroin nanoparticles encapsulated with propranolol presented the highest drug release profile. In order to improve the drug encapsulation efficiency and drug release performance, a modification of silk fibroin nanoparticles with bovine serum albumin and magnetic nanoparticles was tried. The modification was found to improve the drug encapsulation and release of the modified nanoparticles. Bovine-serum-modified nanoparticles presented the best improvement. Full article
(This article belongs to the Special Issue Research as Development Perspective)
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9 pages, 3873 KiB  
Article
Separation Optimization of a Mixture of Ionized and Non-Ionized Solutes under Isocratic and Gradient Conditions in Reversed-Phase HPLC by Means of Microsoft Excel Spreadsheets
by Chrysostomi Zisi, Athina Maria Mangipa, Eleftheria Boutou and Adriani Pappa-Louisi
Separations 2018, 5(1), 19; https://doi.org/10.3390/separations5010019 - 18 Mar 2018
Cited by 1 | Viewed by 6084
Abstract
Τhe crucial role of mobile phase pH for optimizing the separation of a mixture of ionized and non-ionized compounds on a Phenomenex extended pH-range reversed-phase column (Kinetex 5 µm EVO C18) was examined. A previously developed Excel-spreadsheet-based software was used for the whole [...] Read more.
Τhe crucial role of mobile phase pH for optimizing the separation of a mixture of ionized and non-ionized compounds on a Phenomenex extended pH-range reversed-phase column (Kinetex 5 µm EVO C18) was examined. A previously developed Excel-spreadsheet-based software was used for the whole separation optimization procedure of the sample of interest under isocratic conditions as well as under single linear organic modifier-gradients in different eluent pHs. The importance and the advantages of performing a computer-aided separation optimization compared with a trial-and-error optimization method were realized. Additionally, this study showed that the optimized separation conditions for a given stationary phase may be used to achieve successful separations on new columns of the same type and size. In general, the results of this work could give chromatographers a feel of confidence to establish desired separations of a mixture of ionizable and neutral compounds in reversed-phase columns. Full article
(This article belongs to the Special Issue Research as Development Perspective)
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11 pages, 819 KiB  
Article
Development and Validation of an HPLC-DAD Method for the Simultaneous Extraction and Quantification of Bisphenol-A, 4-Hydroxybenzoic Acid, 4-Hydroxyacetophenone and Hydroquinone in Bacterial Cultures of Lactococcus lactis
by Angelos T. Rigopoulos, Victoria F. Samanidou and Maria Touraki
Separations 2018, 5(1), 12; https://doi.org/10.3390/separations5010012 - 6 Feb 2018
Cited by 9 | Viewed by 7380
Abstract
Bisphenol-A, a synthetic organic compound with estrogen mimicking properties, may enter bloodstream through either dermal contact or ingestion. Probiotic bacterial uptake of bisphenol can play a major protective role against its adverse health effects. In this paper, a method for the quantification of [...] Read more.
Bisphenol-A, a synthetic organic compound with estrogen mimicking properties, may enter bloodstream through either dermal contact or ingestion. Probiotic bacterial uptake of bisphenol can play a major protective role against its adverse health effects. In this paper, a method for the quantification of BPA in bacterial cells of L. lactis and of BPA and its potential metabolites 4-hydroxybenzoic Acid, 4-hydroxyacetophenone and hydroquinone in the culture medium is described. Extraction of BPA from the cells was performed using methanol–H2O/TFA (0.08%) (5:1 v/v) followed by SPE. Culture medium was centrifuged and filtered through a 0.45 μm syringe filter. Analysis was conducted in a Nucleosil column, using a gradient of A (95:5 v/v H2O: ACN) and B (5:95 v/v H2O: ACN, containing TFA, pH 2), with a flow rate of 0.5 mL/min. Calibration curves (0.5–600 μg/mL) were constructed using 4-n-Octylphenol as internal standard (1 > R2 > 0.994). Limit of Detection (LOD) and Limit of Quantification (LOQ) values ranged between 0.23 to 4.99 μg/mL and 0.69 to 15.1 μg/mL respectively. A 24 h administration experiment revealed a decline in BPA concentration in the culture media up to 90.27% while the BPA photodegradation levels were low. Our results demonstrate that uptake and possible metabolism of BPA in L. lactis cells facilitates its removal. Full article
(This article belongs to the Special Issue Research as Development Perspective)
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Review

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26 pages, 780 KiB  
Review
Food Sample Preparation for the Determination of Sulfonamides by High-Performance Liquid Chromatography: State-of-the-Art
by Dimitrios Bitas, Abuzar Kabir, Marcello Locatelli and Victoria Samanidou
Separations 2018, 5(2), 31; https://doi.org/10.3390/separations5020031 - 4 Jun 2018
Cited by 34 | Viewed by 7512
Abstract
Antibiotics are a common practice in veterinary medicine, mainly for therapeutic purposes. Sectors of application include livestock farming, aquacultures, and bee-keeping, where bacterial infections are frequent and can be economically damaging. However, antibiotics are usually administered in sub-therapeutic doses as prophylactic and growth [...] Read more.
Antibiotics are a common practice in veterinary medicine, mainly for therapeutic purposes. Sectors of application include livestock farming, aquacultures, and bee-keeping, where bacterial infections are frequent and can be economically damaging. However, antibiotics are usually administered in sub-therapeutic doses as prophylactic and growth promoting agents. Due to their excessive use, antibiotic residues can be present in foods of animal origin, which include meat, fish, milk, eggs, and honey, posing health risks to consumers. For this reason, authorities have set maximum residue limits (MRLs) of certain antibiotics in food matrices, while analytical methods for their determination have been developed. This work focuses on antibiotic extraction and determination, part of which was presented at the “1st Conference in Chemistry for Graduate, Postgraduate Students and PhD Candidates at the Aristotle University of Thessaloniki”. Taking a step further, this paper is a review of the most recent sample preparation protocols applied for the extraction of sulfonamide antibiotics from food samples and their determination with high-performance liquid chromatography (HPLC), covering a five-year period. Full article
(This article belongs to the Special Issue Research as Development Perspective)
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Other

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10 pages, 2138 KiB  
Technical Note
Method Development of Phosphorus and Boron Determination in Fertilizers by ICP-AES
by Emanouela Viso and George Zachariadis
Separations 2018, 5(3), 36; https://doi.org/10.3390/separations5030036 - 9 Jul 2018
Cited by 5 | Viewed by 5901
Abstract
Simultaneous determination of phosphorus and boron in fertilizers was performed by Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES). Three different samples were analyzed, of which two were inorganic and one was of organic composition. Analysis of the samples was performed after heated acidic [...] Read more.
Simultaneous determination of phosphorus and boron in fertilizers was performed by Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES). Three different samples were analyzed, of which two were inorganic and one was of organic composition. Analysis of the samples was performed after heated acidic digestion to completely dissolve them, using two different acid mixtures. A solution of HCl + HNO3 was used to digest the inorganic fertilizers, and a solution of H2SO4 + HNO3 for the organic fertilizer. The spectral emission lines used were 213.617 nm and 214.917 nm for P and 249.772 nm, 249.677 nm and 208.957 nm for B. The detection and quantification limits for P were between 10–20 mg/kg and 40–80 mg/kg respectively, while for B they ranged between 10–30 mg/kg and 40–100 mg/kg respectively. The repeatability of the technique was found to be within the range 0.9–17.0% for P and 1.7–23.4% for B, expressed as relative standard deviation (RSD). The concentrations found by the proposed method are in good agreement with those reported on their package labels. Full article
(This article belongs to the Special Issue Research as Development Perspective)
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