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Sample Preparation for Chromatographic Analysis—Advances, Perspectives and Applications
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Sample Preparation for Chromatographic Analysis—Advances, Perspectives and Applications

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

Deadline for manuscript submissions: closed (30 September 2024) | Viewed by 6347

Special Issue Editors

Prof. Dr. Dorota Wianowska

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Guest Editor
Department of Chromatography, Institute of Chemical Sciences, Faculty of Chemistry, Maria Curie-Sklodowska University in Lublin, Lublin, Poland
Interests: chromatographic analysis; sample preparation; extraction; secondary plant metabolites; biologically active compounds; endo- and exogenous compounds
Special Issues, Collections and Topics in MDPI journals
Prof. Dr. Anna Oniszczuk

E-Mail Website
Guest Editor
Department of Inorganic Chemistry, Medical University of Lublin, Chodźki 4a, 20-093 Lublin, Poland
Interests: biological properties; liquid chromatography, antioxidants; extraction methods; functional food; polyphenols
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Most of the procedures for the determination of organic compounds in complex and complicated samples involve chromatographic analysis. This is because chromatography, owing to the high separation power of the chromatographic systems and the use of very sensitive detectors, makes it possible to analyze even the smallest amount of a single compound against many interfering substances present in the sample. However, considering the samples that we deal with in everyday laboratory practice, the capabilities of chromatographic systems are not sufficient enough to ensure correct analysis results. A sample preparation stage is necessary in which the analyte will be separated as selectively as possible from the other components of the sample, concentrated, and additionally, the incompatible matrix of the primary sample will be replaced with a matrix compatible with the target analytical technique. Therefore, a properly prepared sample is not only the key to the success of the analysis, but also improves it, contributing to the increase in the number of analyses and a reduction in both labor time and costs.

Extraction is most often used to prepare the sample, and in the era of broadly understood miniaturization, miniaturized methods and extraction systems are used. This is a modern trend but also a prospect for the future, with the hope of improving the "greenness" of the analysis of food, pharmaceutical, cosmetic and many other products, not forgetting the analysis of physiological fluids for diagnostic and clinical purposes.

This Special Issue "Sample Preparation for Chromatographic Analysis - Advances, Perspectives and Applications" aims to highlight all contemporary sample preparation techniques, paying special attention to the extraction method and miniaturization of analytical procedures. The development and application of new technologies, procedures, and statistical tools for designing optimal isolation conditions and analysis in both experimental and theoretical studies is a short and definitely non-exhaustive list of possible topics in this Special Issue.

Prof. Dr. Dorota Wianowska
Prof. Dr. Anna Oniszczuk
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

  • liquid–liquid extraction
  • solid–liquid extraction
  • sorptive extraction
  • assisted extraction techniques
  • solventless extraction
  • microextraction techniques

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Published Papers (5 papers)

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Research

15 pages, 1428 KiB  
Article
Determination of PAH Contamination in Breast Milk Samples from Hungarian Volunteering Mothers, Using HPLC–FLD
by Bernard Collins Anditi, Viktória Poór, Dénes Szerencsés, István Szabó, Mátyás Wahr, Anikó Kőnig-Péter and Timea Dergez
Molecules 2024, 29(21), 5060; https://doi.org/10.3390/molecules29215060 - 26 Oct 2024
Viewed by 587
Abstract
(1) The evidence is mounting that polycyclic aromatic hydrocarbons (PAHs) are a class of hazardous organic compounds with established carcinogenic and toxic properties. Humans may be exposed to PAHs through several different routes, including diet, inhalation, and dermal contact. There is also a [...] Read more.
(1) The evidence is mounting that polycyclic aromatic hydrocarbons (PAHs) are a class of hazardous organic compounds with established carcinogenic and toxic properties. Humans may be exposed to PAHs through several different routes, including diet, inhalation, and dermal contact. There is also a possibility that they could transfer into breast milk following maternal exposure, which could potentially endanger breastfeeding infants. (2) The objective of this study was to ascertain the concentration of polycyclic aromatic hydrocarbons (PAHs) in breast milk samples from 50 Hungarian mothers, employing high-performance liquid chromatography with fluorescence detection (HPLC–FLD). An Incremental Life Risk Calculation (IRCL) model estimated the carcinogenic risk to infants. (3) Total PAH concentrations ranged from 0 to 78 ng/mL, with fluorene (5.3 ng/mL), phenanthrene (3.2 ng/mL), and pyrene (2.5 ng/mL) being the most abundant. PAHs were detected in 48 of the 50 samples, with phenanthrene present in 92% of samples. Dibenzo (a,h)anthracene was not detected. (4) According to the model measurements, most of the samples were within acceptable risk levels; however, 2 samples out of 50 posed a higher risk. Statistical analysis of questionnaires completed by the mothers indicated that factors such as diet, residence, and education may influence PAH levels in breast milk. Full article
(This article belongs to the Special Issue Sample Preparation for Chromatographic Analysis—Advances, Perspectives and Applications)
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14 pages, 2982 KiB  
Article
Method Development and Validation of an Aerosol Sampling Technique for the Analysis of Nicotine in Electronic Cigarette Aerosols
by Maarten Dill, Eric Deconinck and Sophia Barhdadi
Molecules 2024, 29(15), 3487; https://doi.org/10.3390/molecules29153487 - 25 Jul 2024
Cited by 1 | Viewed by 907
Abstract
Because of the increasing popularity of e-cigarettes, monitoring the e-cigarette market has become important for national health authorities to guarantee safety and quality. In the EU, the Tobacco Products Directive requires emission studies for e-cigarette products. The absence of industry guidelines for studying [...] Read more.
Because of the increasing popularity of e-cigarettes, monitoring the e-cigarette market has become important for national health authorities to guarantee safety and quality. In the EU, the Tobacco Products Directive requires emission studies for e-cigarette products. The absence of industry guidelines for studying these emissions and the lack of proper validation in the literature led us to develop and validate a method using the total error approach for the determination of nicotine in e-cigarette aerosols. A commercial vaping device was used to generate aerosols, which were then collected on Cambridge filter pads and measured for nicotine concentration by UHPLC-DAD after extraction. The method was successfully validated by generating accuracy profiles, which show that the β-expectation tolerance intervals remained below the acceptance limits of ±20%. Within-run repeatability and intermediate precision were considered acceptable since the highest RSD value obtained was below 5%. The method was applied to 15 commercial e-liquids. A complete validation of a method for the analysis of e-cigarette emissions is presented, including several parameters that impact the accuracy and reproducibility. Similar systematic approaches for method development and validation could be used for other e-cigarette emission analysis methods to ensure the reliability of the measurements. Full article
(This article belongs to the Special Issue Sample Preparation for Chromatographic Analysis—Advances, Perspectives and Applications)
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13 pages, 3981 KiB  
Article
Monitoring Exposure to Five Chemical Warfare Agents Using the Dried Urine Spot Technique and Liquid Chromatography-Mass Spectrometry/Mass Spectrometry—In Vivo Determination of Sarin Metabolite in Mice
by Lilach Yishai Aviram, Shai Dagan, Ariel Hindi, Shira Chapman, Rellie Gez and Eyal Drug
Molecules 2023, 28(23), 7687; https://doi.org/10.3390/molecules28237687 - 21 Nov 2023
Viewed by 1516
Abstract
Dried urine spot (DUS) is a micro-sample collection technique, known for its advantages in handling, storage and shipping. It also uses only a small volume of urine, an essential consideration in working with small animals, or in acute medical situations. Alkyl-phosphonic acids are [...] Read more.
Dried urine spot (DUS) is a micro-sample collection technique, known for its advantages in handling, storage and shipping. It also uses only a small volume of urine, an essential consideration in working with small animals, or in acute medical situations. Alkyl-phosphonic acids are the direct and indicative metabolites of organophosphorus chemical warfare agents (OP-CWAs) and are present in blood and urine shortly after exposure. They are therefore crucially important for monitoring casualties in war and terror scenarios. We report here a new approach for the determination of the metabolites of five CWAs in urine using DUS. The method is based on a simple and rapid sample preparation, using only 50 µL of urine, spotted and dried on DBS paper, extracted using 300 µL methanol/water and analyzed via targeted LC-MS/MS. The detection limits for the five CWAs, sarin (GB), soman (GD), cyclosarin (GF), VX and RVX in human urine were from 0.5 to 5 ng/mL. Recoveries of (40–80%) were obtained in the range of 10–300 ng/mL, with a linear response (R2 > 0.964, R > 0.982). The method is highly stable, even with DUS samples stored up to 5 months at room temperature before analysis. It was implemented in a sarin in vivo exposure experiment on mice, applied for the time course determination of isopropyl methylphosphonic acid (IMPA, sarin hydrolysis product) in mice urine. IMPA was detectable even with samples drawn 60 h after the mice’s (IN) exposure to 1 LD50 sarin. This method was also evaluated in a non-targeted screening for multiple potential CWA analogs (LC-Orbitrap HRMS analysis followed by automatic peak detection and library searches). The method developed here is applicable for rapid CWA casualty monitoring. Full article
(This article belongs to the Special Issue Sample Preparation for Chromatographic Analysis—Advances, Perspectives and Applications)
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13 pages, 1929 KiB  
Article
The Use of Extraction on C18-Silica-Modified Magnetic Nanoparticles for the Determination of Ciprofloxacin and Ofloxacin in Meat Tissues
by Izabella Kośka, Paweł Kubalczyk, Michał Cichomski and Aneta Kisielewska
Molecules 2023, 28(16), 6123; https://doi.org/10.3390/molecules28166123 - 18 Aug 2023
Cited by 2 | Viewed by 1214
Abstract
A simple, fast, and low-cost method of extraction using magnetic nanoparticles was developed for sample preparation in the determination of ciprofloxacin and ofloxacin in meat tissues with the use of capillary electrophoresis. This study is the first utilization of silica-coated magnetic nanoparticles with [...] Read more.
A simple, fast, and low-cost method of extraction using magnetic nanoparticles was developed for sample preparation in the determination of ciprofloxacin and ofloxacin in meat tissues with the use of capillary electrophoresis. This study is the first utilization of silica-coated magnetic nanoparticles with attached C18 chains to extract fluoroquinolones from meat tissues. This method is therefore characterized by a very simple sample preparation procedure, but on the other hand, by satisfactory precision and accuracy. Magnetic nanoparticles with an appropriately modified surface were placed in an Eppendorf tube, then conditioned with methanol, next rinsed with water and, finally, a homogenized tissue sample was added. At the neutral pH of the sample solution, these compounds do not have a charge and are able to adsorb on the modified particles. After extraction, the nanoparticles were dried and, then, desorption of analytes was conducted with the use of a mixture of 0.1 mol/L HCl and acetonitrile (1:1). This approach made it possible to purify the sample matrix and to obtain satisfactory LOQ levels for the method using the CE technique with UV-Vis detection. In this method, the LOD and LOQ values for both analytes were 0.04 nmol/g tissue and 0.15 nmol/g tissue, respectively. The calibration curves were linear in the entire concentration range, and the accuracy and the recovery of the method were at the satisfactory levels. The square value of the linear correlation coefficients (R2) for Cpx and Ofx were 0.9995 and 0.9992, respectively. The precision value of the method was within the range of 3–11% and accuracy was in the range of 93–110%. Full article
(This article belongs to the Special Issue Sample Preparation for Chromatographic Analysis—Advances, Perspectives and Applications)
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11 pages, 2682 KiB  
Article
A Comparative Analysis on the Environmental Impact of Selected Methods for Determining the Profile of Fatty Acids in Cheese
by Izabela Narloch and Grażyna Wejnerowska
Molecules 2023, 28(13), 4981; https://doi.org/10.3390/molecules28134981 - 25 Jun 2023
Cited by 2 | Viewed by 1505
Abstract
The fatty acid profile of cheese influences its sensory parameters, such as color, texture, or flavor. Examining the fatty acid profile also helps to assess the nutritional value of the cheese that is being tested. However, the determination of fatty acids in cheese [...] Read more.
The fatty acid profile of cheese influences its sensory parameters, such as color, texture, or flavor. Examining the fatty acid profile also helps to assess the nutritional value of the cheese that is being tested. However, the determination of fatty acids in cheese samples is a multi-stage and time-consuming task. In addition, large amounts of toxic organic solvents are used to prepare samples for analysis purposes. This paper presents the results of a study to determine the fatty acid profile of yellow cheese samples. Six different methods of sample preparation were compared for analysis purposes. The profile of fatty acids was determined using gas chromatography with flame ionization detection (GC-FID). The study showed significant differences (p > 0.05) in the resulting fatty acid profile between the methods used. It was found that the most reliable fatty acid profile results were obtained using methods derived from the Folch method. In addition, tools such as the Analytical Eco-Scale tool and the Analytical Greenness Metric for Sample Preparation (AGREEprep) tool were used to assess the greenness of the methods used. In the case of the Analytical Eco-Scale tool, all six methods scored ‘acceptable green analysis’ with scores ranging from 61 to 73. However, an evaluation of methods using the AGREEprep metric showed that the results of the methods (0.13–0.27) did not show the “greenness” of the analytical methods. Full article
(This article belongs to the Special Issue Sample Preparation for Chromatographic Analysis—Advances, Perspectives and Applications)
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