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Chromatography—The Ultimate Analytical Tool II

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

Deadline for manuscript submissions: closed (31 January 2024) | Viewed by 13732

Special Issue Editors


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Guest Editor
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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Guest Editor
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece
Interests: analytical chemistry; microextraction sample preparation techniques; high-pressure liquid chromatography; gas chromatography; high-resolution mass spectrometry; chemometrics
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Separation, qualitative analysis, and quantitative analysis can be achieved by choosing the right conditions. Thus, numerous gas chromatographic, liquid chromatographic, and supercritical fluid chromatographic methods have been developed and applied to most types of samples and most kinds of analytes. Not to mention the fact that older varieties, such as paper chromatography and thin-layer chromatography, were pioneer analytical techniques in many laboratories.

In particular, when hyphenated to spectrometric techniques chromatography also allows for the identification of separated analytes in a single run. Highly sophisticated equipment can answer all analytical problems very quickly.

Chromatographers cooperate with many scientific fields and provide their insights to medical doctors, veterinarians, food scientists, biologists, dentists, archaeologists, etc.

The choice of two-dimensional approaches can expand the power of chromatographic techniques, either in heart-cut or comprehensive modes.

In this Special Issue, the Guest Editors are inviting analytical chemists to prove that their separation technique is the ultimate analytical tool.

Prof. Dr. Victoria Samanidou
Dr. Natasa Kalogiouri
Guest Editors

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Keywords

  • chromatography
  • high-performance liquid chromatography
  • ultra-high-performance liquid chromatography
  • gas chromatography
  • two-dimensional gas chromatography
  • two-dimensional liquid chromatography
  • paper chromatography
  • liquid chromatography
  • preparative chromatography
  • supercritical fluid chromatography
  • thin-layer chromatography

Published Papers (9 papers)

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Research

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16 pages, 4115 KiB  
Article
Comprehensive Characterization of Triterpene Saponins in Rhizoma Panacis Japonici by Offline Two-Dimensional Liquid Chromatography Coupled to Quadrupole Time-of-Flight Mass Spectrometry
by Subinuer Yasen, Chengrui Li, Siyuan Wang, Yixin Dong, Hang Li, Jie Chen, Yifan Meng, Ping Yu and Haiyan Zou
Molecules 2024, 29(6), 1295; https://doi.org/10.3390/molecules29061295 - 14 Mar 2024
Viewed by 638
Abstract
Rhizoma Panacis Japonici (RPJ) is an ancient herbal medicine from China that has long been employed for its medicinal benefits in relieving arthritis physical debility and diverse afflictions. The primary bioactive constituents found in RPJ are triterpene saponins, which exhibit numerous pharmacological actions, [...] Read more.
Rhizoma Panacis Japonici (RPJ) is an ancient herbal medicine from China that has long been employed for its medicinal benefits in relieving arthritis physical debility and diverse afflictions. The primary bioactive constituents found in RPJ are triterpene saponins, which exhibit numerous pharmacological actions, including anti-inflammatory, antioxidant, and immunomodulating effects. The present study established a straightforward and effective approach for characterizing triterpene saponins in RPJ. An offline HILIC × RP LC/QTOF-MS method was developed, along with a self-constructed in-house database containing 612 saponins reported in the Panax genus and 228 predicted metabolites. The approach achieved good chromatographic performance in isolating triterpene saponins of RPJ, with the HILIC column as the first dimension (1D) and the BEH C18 column as the second dimension (2D). The developed two-dimensional liquid chromatography system exhibited an orthogonality of 0.61 and a peak capacity of 1249. Detection was performed using a QTOF mass spectrometer in a data-independent manner (MSE) in a negative ion mode. Using the in-house database, the collected MS data were processed by an automatic workflow on UNIFI 1.8.2 software, which included data correction, matching of precursor and product ions, and peak annotation. In this study, 307 saponins were characterized from RPJ and 76 saponins were identified for the first time in Panax japonicus. This research not only enhances our understanding of the chemical characteristics of RPJ but also offers a simple and efficient method for analyzing the complex composition of herbal medicine. Full article
(This article belongs to the Special Issue Chromatography—The Ultimate Analytical Tool II)
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12 pages, 1924 KiB  
Article
The Validation and Determination of Empagliflozin Concentration in the Presence of Grapefruit Juice Using HPLC for Pharmacokinetic Applications
by Wael Abu Dayyih, Zainab Zakaraya, Mohammad Hailat, Nafe M. Al-Tawarah, Sahem Alkharabsheh, Haya Khalid Nadher, Zeyad Hailat, Samia M. Alarman, Anas Khaleel and Riad Awad
Molecules 2024, 29(6), 1236; https://doi.org/10.3390/molecules29061236 - 11 Mar 2024
Viewed by 855
Abstract
Type 2 diabetes mellitus is a multifactorial disorder whose primary manifestation usually initiates with elevated blood sugar levels. Several antidiabetic agents are used to manage type 2 diabetes mellitus, of which empagliflozin is an oral sodium-glucose co-transporter (SGLT-2) inhibitor in the kidney. This [...] Read more.
Type 2 diabetes mellitus is a multifactorial disorder whose primary manifestation usually initiates with elevated blood sugar levels. Several antidiabetic agents are used to manage type 2 diabetes mellitus, of which empagliflozin is an oral sodium-glucose co-transporter (SGLT-2) inhibitor in the kidney. This research aims to develop and validate a simple analytical method for determining empagliflozin levels in biological fluid and to further evaluate grapefruit juice’s impact on empagliflozin pharmacokinetics in rats. High-Performance Liquid Chromatography (HPLC) was used to establish a simple, rapid, and accurate method for determining empagliflozin levels in rat plasma, in the presence of grapefruit juice. Four groups of rats (n = 10 rats in each) were used in the preclinical study. Group A (healthy rats) received empagliflozin alone; Group B (healthy rats) received empagliflozin with grapefruit; Group C (diabetic rats) received empagliflozin with grapefruit; and Group D (healthy, negative control) received no medication. The rats (n = 10) were given grapefruit juice instead of water for seven days before receiving the empagliflozin dose (0.16 mg/kg). Some pharmacokinetic parameters for each group were determined. The maximum plasma concentration (Cmax) and area under the curve (AUC) of empagliflozin in Group A without grapefruit intake were 730 ng/mL and 9264.6 ng × h/mL, respectively, with Tmax (2 h). In Group B, Cmax was 1907 ng/mL and AUC was 10,290.75 ng × h/mL in the presence of grapefruit, with Tmax (1 h); whereas, in Group C, the Cmax was 2936 ng/mL and AUC was 18657 ng × h/mL, with Tmax (2 h). In conclusion, our results showed that the co-administration of grapefruit with empagliflozin should be cautiously monitored and avoided, in which grapefruit elevates the plasma level of empagliflozin. This may be attributed to the inhibition of the uridine enzyme in the grapefruit by hesperidin, naringin, and flavonoid. Full article
(This article belongs to the Special Issue Chromatography—The Ultimate Analytical Tool II)
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11 pages, 2001 KiB  
Article
Analysis of Softwood Lignans by Comprehensive Two-Dimensional Liquid Chromatography
by Danil I. Falev, Ilya S. Voronov, Alexandra A. Onuchina, Anna V. Faleva, Nikolay V. Ul’yanovskii and Dmitry S. Kosyakov
Molecules 2023, 28(24), 8114; https://doi.org/10.3390/molecules28248114 - 15 Dec 2023
Cited by 1 | Viewed by 779
Abstract
Lignans constitute a large group of phenolic plant secondary metabolites possessing high bioactivity. Their accurate determination in plant extracts with a complex chemical composition is challenging and requires advanced separation techniques. In the present study, a new approach to the determination of lignans [...] Read more.
Lignans constitute a large group of phenolic plant secondary metabolites possessing high bioactivity. Their accurate determination in plant extracts with a complex chemical composition is challenging and requires advanced separation techniques. In the present study, a new approach to the determination of lignans in coniferous knotwood extracts as the promising industrial-scale source of such compounds based on comprehensive two-dimensional liquid chromatography separation and UV spectrophotometric detection is proposed. First and second-dimension column screening showed that the best results can be obtained using a combination of non-polar and polar hydroxy group embedded octadecyl stationary phases with moderate (~40%) “orthogonality”. The optimization of LC × LC separation conditions allowed for the development of a new method for the quantification of the five lignans (secoisolariciresinol, matairesinol, pinoresinol, 7-hydroxymatairesinol, and nortrachelogenin) in knotwood extracts with limits of quantification in the range of 0.27–0.95 mg L−1 and a linear concentration range covering at least two orders of magnitude. Testing the developed method on coniferous (larch, fir, spruce, and pine) knotwood extracts demonstrated the high selectivity of the analysis and the advantages of LC × LC in the separation and accurate quantification of the compounds co-eluting in one-dimensional HPLC. Full article
(This article belongs to the Special Issue Chromatography—The Ultimate Analytical Tool II)
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16 pages, 1584 KiB  
Article
Development, Validation, and Two-Year Application of Rapid and Simple LC-MS/MS-Based Method for the Determination of K2MK-7 in Blood Samples
by Łukasz Paprotny, Dorota Szewczak, Iryna Bryshten and Dorota Wianowska
Molecules 2023, 28(18), 6523; https://doi.org/10.3390/molecules28186523 - 8 Sep 2023
Viewed by 1031
Abstract
Biological properties of menaquinone-7, one of the vitamin K2 vitamers (K2MK-7), both those proven and those that remain to be investigated, arouse extensive interest that goes beyond the strictly scientific framework. The most important of them is the prevention of age-related diseases, considering [...] Read more.
Biological properties of menaquinone-7, one of the vitamin K2 vitamers (K2MK-7), both those proven and those that remain to be investigated, arouse extensive interest that goes beyond the strictly scientific framework. The most important of them is the prevention of age-related diseases, considering that we live in the times identified as the era of aging societies and many people are exposed to the vitamin K2MK-7 deficiency. Therefore, an effective analytical protocol that can be adopted as a diagnostic and preventive analytics tool is needed. Herein, a simple sample preparation method followed by the liquid chromatography-tandem mass spectrometry-based method (LC-MS/MS), was used for the selective and sensitive determination of K2MK-7 in serum samples. Under the optimized conditions, using 500 µL of serum and the same amount of n-hexane, the reproducibility and the accuracy were obtained in the ranges of 89–97% and 86–110%, respectively, and the limit of detection value was 0.01 ng/mL. This method was used for the routine analysis. Statistical interpretation of the data from 518 samples obtained during 2 years of practice allowed for obtaining information on the content and distribution of K2MK-7 in the Polish population, broken down by the sex and age groups. Full article
(This article belongs to the Special Issue Chromatography—The Ultimate Analytical Tool II)
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15 pages, 9833 KiB  
Article
Epoxidation of Methyl Esters as Valuable Biomolecules: Monitoring of Reaction
by Martin Hájek, Tomáš Hájek, David Kocián, Karel Frolich and András Peller
Molecules 2023, 28(6), 2819; https://doi.org/10.3390/molecules28062819 - 21 Mar 2023
Cited by 2 | Viewed by 1700
Abstract
The paper is focused on the epoxidation of methyl esters prepared from oil crops with various profiles of higher fatty acids, especially unsaturated, which are mainly contained in the non-edible linseed and Camelina sativa oil (second generation). The novelty consists in the separation [...] Read more.
The paper is focused on the epoxidation of methyl esters prepared from oil crops with various profiles of higher fatty acids, especially unsaturated, which are mainly contained in the non-edible linseed and Camelina sativa oil (second generation). The novelty consists in the separation and identification of all products with oxirane ring formed through a reaction and in the determination of time course. Through the epoxidation, many intermediates and final products were formed, i.e., epoxides with different number and/or different position of oxirane rings in carbon chain. For the determination, three main methods (infrared spectroscopy, high-pressure liquid chromatography and gas chromatography with mass spectrometry) were applied. Only gas chromatography enables the separation of individual epoxides, which were identified on the base of the mass spectra, molecule ion and time course of products. The determination of intermediates enables: (i) control of the epoxidation process, (ii) determination of the mixture of epoxides in detail and so the calculation of selectivity of each product. Therefore, the epoxidation will be more environmentally friendly especially for advanced applications of non-edible oil crops containing high amounts of unsaturated fatty acids. Full article
(This article belongs to the Special Issue Chromatography—The Ultimate Analytical Tool II)
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19 pages, 3243 KiB  
Article
Evidence for the Hydration of Some Organic Compounds during Reverse-Phase HPLC Analysis
by Igor G. Zenkevich, Abdennour Derouiche and Daria A. Nikitina
Molecules 2023, 28(2), 734; https://doi.org/10.3390/molecules28020734 - 11 Jan 2023
Cited by 2 | Viewed by 1506
Abstract
Some polar analytes (X) can reversibly form hydrates in water-containing eluents under the conditions of reversed-phase HPLC analysis, X + H2O X × H2O. One of the methods to detect their formation is the recurrent approximation of the [...] Read more.
Some polar analytes (X) can reversibly form hydrates in water-containing eluents under the conditions of reversed-phase HPLC analysis, X + H2O X × H2O. One of the methods to detect their formation is the recurrent approximation of the net retention times of such analytes, tR(C + ΔC) = atR(C) + b, where ΔC = const is the constant step in the variation of the organic modifier content of an eluent. These dependencies are linear if hydrates are not formed, but in the case of hydrate formation, they deviate from linearity under high water content. It has been shown that UV spectroscopic parameters, namely, relative optical densities: Arel = A1)/A2), depend on eluent composition for some organic compounds, but their variations cannot be used as indicators for hydrate formation. The coefficients that characterize the dependence of the analyte retention indices on the organic component concentration of an eluent, dRI/dC, appeared to be the most informative additional criterion for hydration. The values of these coefficients for most polar analytes are largely negative (dRI/dC < 0), whereas, for nonpolar compounds, they are largely positive (dRI/dC > 0). Full article
(This article belongs to the Special Issue Chromatography—The Ultimate Analytical Tool II)
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14 pages, 1919 KiB  
Article
An Optimized HPLC-DAD Methodology for the Determination of Anthocyanins in Grape Skins of Red Greek Winegrape Cultivars (Vitis vinifera L.)
by Natasa P. Kalogiouri, Christina Karadimou, Mary S. Avgidou, Elissavet Petsa, Emmanouil-Nikolaos Papadakis, Serafeim Theocharis, Ioannis Mourtzinos, Urania Menkissoglu-Spiroudi and Stefanos Koundouras
Molecules 2022, 27(20), 7107; https://doi.org/10.3390/molecules27207107 - 21 Oct 2022
Cited by 2 | Viewed by 1880
Abstract
A rapid and simple HPLC-DAD analytical method was developed and optimized for the determination of anthocynanins in three red Greek winegrape varieties (Kotsifali, Limnio, and Vradiano). The critical parameters, such as the acidifying solvent and the extraction temperature, which affect the extraction of [...] Read more.
A rapid and simple HPLC-DAD analytical method was developed and optimized for the determination of anthocynanins in three red Greek winegrape varieties (Kotsifali, Limnio, and Vradiano). The critical parameters, such as the acidifying solvent and the extraction temperature, which affect the extraction of anthocyanins from the grapes, were studied to find the optimum values. The developed methodology was validated in terms of selectivity, linearity, accuracy, and precision and presented satisfactory results. The limits of quantification (LOQs) ranged between 0.20 mg/kg to 0.60 mg/kg, and the limits of detection (LODs) ranged between 0.06 mg/kg and 0.12 mg/kg. The RSD% of the within-day and between-day assays were lower than 6.2% and 8.5%, respectively, showing adequate precision. The accuracy ranged between 91.6 and 119% for within-day assay and between 89.9 and 123% for between-day assay. Sixteen samples from the main regions of each variety as well as from the official ampelographic collections of Greece were collected during the 2020 growing season and were further analyzed by HPLC-DAD. Notable differences in the anthocyanin content were detected among the cultivars using hierarchical cluster analysis (HCA). Full article
(This article belongs to the Special Issue Chromatography—The Ultimate Analytical Tool II)
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12 pages, 1249 KiB  
Article
Rapid Simultaneous Quantification of 1-Formyl-2,2-Dimethylhydrazine and Dimethylurea Isomers in Environmental Samples by Supercritical Fluid Chromatography–Tandem Mass Spectrometry
by Denis V. Ovchinnikov, Sergey A. Vakhrameev, Danil I. Falev, Nikolay V. Ul’yanovskii and Dmitry S. Kosyakov
Molecules 2022, 27(15), 5025; https://doi.org/10.3390/molecules27155025 - 7 Aug 2022
Cited by 2 | Viewed by 1655
Abstract
When released to the environment, the rocket fuel unsymmetrical dimethylhydrazine (UDMH) undergoes oxidative transformations, resulting in the formation of an extremely large number of nitrogen-containing transformation products, including isomeric compounds which are difficult to discriminate by common chromatography techniques. In the present work, [...] Read more.
When released to the environment, the rocket fuel unsymmetrical dimethylhydrazine (UDMH) undergoes oxidative transformations, resulting in the formation of an extremely large number of nitrogen-containing transformation products, including isomeric compounds which are difficult to discriminate by common chromatography techniques. In the present work, supercritical fluid chromatography–tandem mass spectrometry (SFC-MS/MS) was proposed for resolving the problem of fast separation and simultaneous quantification of 1-formyl-2,2-dimethylhydrazine (FADMH) as one of the major UDMH transformation products, and its isomers—1,1-dimethylurea (UDMU) and 1,2-dimethylurea (SDMU). 2-Ethylpyridine stationary phase provided baseline separation of analytes in 1.5 min without the distortion of the chromatographic peaks. Optimization of SFC separation and MS/MS detection conditions allowed for the development of rapid, sensitive, and “green” method for the simultaneous determination of FADMH, UDMU, and SDMU in environmental samples with LOQs of 1–10 µg L−1 and linear range covering three orders of magnitude. The method was validated and successfully tested on the real extracts of peaty and sandy soils polluted with rocket fuel and UDMH oxidation products. It was shown that both UDMU and SDMU are formed in noticeable amounts during UDMH oxidation. Despite relatively low toxicity, UDMU can be considered one of the major UDMH transformation products and a potential marker of soil pollution with toxic rocket fuel. Full article
(This article belongs to the Special Issue Chromatography—The Ultimate Analytical Tool II)
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Review

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19 pages, 368 KiB  
Review
Recent Advances in Mycotoxin Determination in Fish Feed Ingredients
by Sofia Vardali, Christina Papadouli, George Rigos, Ioannis Nengas, Panagiota Panagiotaki and Eleni Golomazou
Molecules 2023, 28(6), 2519; https://doi.org/10.3390/molecules28062519 - 9 Mar 2023
Cited by 4 | Viewed by 2615
Abstract
Low-cost plant-based sources used in aquaculture diets are prone to the occurrence of animal feed contaminants, which may in certain conditions affect the quality and safety of aquafeeds. Mycotoxins, a toxic group of small organic molecules produced by fungi, comprise a frequently occurring [...] Read more.
Low-cost plant-based sources used in aquaculture diets are prone to the occurrence of animal feed contaminants, which may in certain conditions affect the quality and safety of aquafeeds. Mycotoxins, a toxic group of small organic molecules produced by fungi, comprise a frequently occurring plant-based feed contaminant in aquafeeds. Mycotoxin contamination can potentially cause significant mortality, reduced productivity, and higher disease susceptibility; thus, its timely detection is crucial to the aquaculture industry. The present review summarizes the methodological advances, developed mainly during the past decade, related to mycotoxin detection in aquafeed ingredients, namely analytical, chromatographic, and immunological methodologies, as well as the use of biosensors and spectroscopic methods which are becoming more prevalent. Rapid and accurate mycotoxin detection is and will continue to be crucial to the food industry, animal production, and the environment, resulting in further improvements and developments in mycotoxin detection techniques. Full article
(This article belongs to the Special Issue Chromatography—The Ultimate Analytical Tool II)
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