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Chromatography-the Ultimate Analytical Tool

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

Deadline for manuscript submissions: closed (31 January 2022) | Viewed by 27216

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Prof. Dr. Victoria Samanidou

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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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Dr. Natasa Kalogiouri

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Assistant 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

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Dear Colleagues,

Since its introduction by the Russian botanist Mikhail Semyonovich Tsvet chromatography has been the most powerful analytical tool in Analytical Chemistry.

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 for most types of samples and most kinds of analytes. Not to mention that older varieties like paper chromatography and thin-layer chromatography were pioneer analytical techniques in many laboratories.

Especially when hyphenated to spectrometric techniques, chromatography also allows 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 give their lights 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
Guest Editor

Dr. Natasa Kalogiouri
Assistant Guest Editor

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Keywords

Chromatography
HPLC
TLC
GC
SFC
Paper chromatography
Liquid chromatography
Preparative chromatography
Supercritical chromatography
Thin-layer chromatography

Published Papers (10 papers)

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Research

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9 pages, 1376 KiB

Open AccessArticle

A Rapid LC-MS/MS-PRM Assay for Serologic Quantification of Sialylated O-HPX Glycoforms in Patients with Liver Fibrosis

by Aswini Panigrahi, Julius Benicky, Renhuizi Wei, Jaeil Ahn, Radoslav Goldman and Miloslav Sanda

Molecules 2022, 27(7), 2213; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27072213 - 29 Mar 2022

Cited by 3 | Viewed by 1699

Abstract

Development of high throughput robust methods is a prerequisite for a successful clinical use of LC-MS/MS assays. In earlier studies, we reported that nLC-MS/MS measurement of the O-glycoforms of HPX is an indicator of liver fibrosis. In this study, we show that a microflow LC-MS/MS method using a single column setup for capture of the analytes, desalting, fast gradient elution, and on-line mass spectrometry measurements, is robust, substantially faster, and even more sensitive than our nLC setup. We demonstrate applicability of the workflow on the quantification of the O-HPX glycoforms in unfractionated serum samples of control and liver disease patients. The assay requires microliter volumes of serum samples, and the platform is amenable to one hundred sample injections per day, providing a valuable tool for biomarker validation and screening studies. Full article

(This article belongs to the Special Issue Chromatography-the Ultimate Analytical Tool)

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15 pages, 2517 KiB

Open AccessArticle

Simultaneous Determination of Caffeine and Paracetamol in Commercial Formulations Using Greener Normal-Phase and Reversed-Phase HPTLC Methods: A Contrast of Validation Parameters

by Prawez Alam, Faiyaz Shakeel, Abuzer Ali, Mohammed H. Alqarni, Ahmed I. Foudah, Tariq M. Aljarba, Faisal K. Alkholifi, Sultan Alshehri, Mohammed M. Ghoneim and Amena Ali

Molecules 2022, 27(2), 405; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27020405 - 09 Jan 2022

Cited by 19 | Viewed by 2687

Abstract

There has been no assessment of the greenness of the described analytical techniques for the simultaneous determination (SMD) of caffeine and paracetamol. As a result, in comparison to the greener normal-phase high-performance thin-layer chromatography (HPTLC) technique, this research was conducted to develop a rapid, sensitive, and greener reversed-phase HPTLC approach for the SMD of caffeine and paracetamol in commercial formulations. The greenness of both techniques was calculated using the AGREE method. For the SMD of caffeine and paracetamol, the greener normal-phase and reversed-phase HPTLC methods were linear in the 50–500 ng/band and 25–800 ng/band ranges, respectively. For the SMD of caffeine and paracetamol, the greener reversed-phase HPTLC approach was more sensitive, accurate, precise, and robust than the greener normal-phase HPTLC technique. For the SMD of caffeine paracetamol in commercial PANEXT and SAFEXT tablets, the greener reversed-phase HPTLC technique was superior to the greener normal-phase HPTLC approach. The AGREE scores for the greener normal-phase and reversed-phase HPTLC approaches were estimated as 0.81 and 0.83, respectively, indicated excellent greenness profiles for both analytical approaches. The greener reversed-phase HPTLC approach is judged superior to the greener normal-phase HPTLC approach based on numerous validation parameters and pharmaceutical assays. Full article

(This article belongs to the Special Issue Chromatography-the Ultimate Analytical Tool)

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11 pages, 3185 KiB

Open AccessArticle

Application of Skyline for Analysis of Protein–Protein Interactions In Vivo

by Arman Kulyyassov

Molecules 2021, 26(23), 7170; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26237170 - 26 Nov 2021

Cited by 3 | Viewed by 2327

Abstract

Quantitative and qualitative analyses of cell protein composition using liquid chromatography/tandem mass spectrometry are now standard techniques in biological and clinical research. However, the quantitative analysis of protein–protein interactions (PPIs) in cells is also important since these interactions are the bases of many processes, such as the cell cycle and signaling pathways. This paper describes the application of Skyline software for the identification and quantification of the biotinylated form of the biotin acceptor peptide (BAP) tag, which is a marker of in vivo PPIs. The tag was used in the Proximity Utilizing Biotinylation (PUB) method, which is based on the co-expression of BAP-X and BirA-Y in mammalian cells, where X or Y are interacting proteins of interest. A high level of biotinylation was detected in the model experiments where X and Y were pluripotency transcription factors Sox2 and Oct4, or heterochromatin protein HP1γ. MRM data processed by Skyline were normalized and recalculated. Ratios of biotinylation levels in experiment versus controls were 86 ± 6 (3 h biotinylation time) and 71 ± 5 (9 h biotinylation time) for BAP-Sox2 + BirA-Oct4 and 32 ± 3 (4 h biotinylation time) for BAP-HP1γ + BirA-HP1γ experiments. Skyline can also be applied for the analysis and identification of PPIs from shotgun proteomics data downloaded from publicly available datasets and repositories. Full article

(This article belongs to the Special Issue Chromatography-the Ultimate Analytical Tool)

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18 pages, 3432 KiB

Open AccessArticle

A Validated Ultrasound-Assisted Extraction Coupled with SPE-HPLC-DAD for the Determination of Flavonoids in By-Products of Plant Origin: An Application Study for the Valorization of the Walnut Septum Membrane

by Natasa P. Kalogiouri and Victoria F. Samanidou

Molecules 2021, 26(21), 6418; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26216418 - 24 Oct 2021

Cited by 8 | Viewed by 2063

Abstract

Walnut byproducts have been shown to exert functional properties, but the literature on their bioactive content is still scarce. Among walnut byproducts, walnut septum is a dry ligneous diaphragm tissue that divides the two halves of the kernel, exhibiting nutritional and medicinal properties. These functional properties are owing to its flavonoid content, and in order to explore the flavonoid fraction, an ultrasound-assisted (UAE) protocol was combined with solid phase extraction (SPE) and coupled to high-performance liquid chromatography with diode array detection (HPLC-DAD) for the determination of flavonoids in Greek walnut septa membranes belonging to Chandler, Vina, and Franquette varieties. The proposed UAE-SPE-HPLC-DAD method was validated and the relative standard deviations (RSD%) of the within-day and between-day assays were lower than 6.2 and 8.5, respectively, showing good precision, and high accuracy ranging from 90.8 (apigenin) to 97.5% (catechin) for within-day assay, and from 88.5 (myricetin) to 96.2% (catechin) for between-day assay. Overall, seven flavonoids were determined (catechin, rutin, myricetin, luteolin, quercetin, apigenin, and kaempferol) suggesting that the walnut septum is a rich source of bioactive constituents. The quantification results were further processed using ANOVA analysis to examine if there are statistically significant differences between the concentration of each flavonoid and the variety of the walnut septum. Full article

(This article belongs to the Special Issue Chromatography-the Ultimate Analytical Tool)

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11 pages, 1685 KiB

Open AccessArticle

Development of HPLC Method for Catechins and Related Compounds Determination and Standardization in Miang (Traditional Lanna Fermented Tea Leaf in Northern Thailand)

by Sunanta Wangkarn, Kate Grudpan, Chartchai Khanongnuch, Thanawat Pattananandecha, Sutasinee Apichai and Chalermpong Saenjum

Molecules 2021, 26(19), 6052; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26196052 - 06 Oct 2021

Cited by 16 | Viewed by 3859

Abstract

High performance liquid chromatography (HPLC) for catechins and related compounds in Miang (traditional Lanna fermented tea leaf) was developed to overcome the matrices during the fermentation process. We investigated a variety of columns and elution conditions to determine seven catechins, namely (+)-catechin, (−)-gallocatechin, (−)-epigallocatechin, (−)-epicatechin, (−)-epigallocatechin gallate, (−)-gallocatechin gallate, (−)-epicatechin gallate, as well as gallic acid and caffeine, resulting in the development of reproducible systems for analyses that overcome sample matrices. Among the three reversed-phase columns, column C (deactivated, with extra dense bonding, double endcapped monomeric C18, high-purity silica at 3.0 mm × 250 mm and a 5 µm particle size) significantly improved the separation between Miang catechins in the presence of acid in the mobile phase within a shorter analysis time. The validation method showed effective linearity, precision, accuracy, and limits of detection and quantitation. The validated system was adequate for the qualitative and quantitative measurement of seven active catechins, including gallic acid and caffeine in Miang, during the fermentation process and standardization of Miang extracts. The latter contain catechins and related compounds that are further developed into natural active pharmaceutical ingredients (natural APIs) for cosmeceutical and nutraceutical products. Full article

(This article belongs to the Special Issue Chromatography-the Ultimate Analytical Tool)

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14 pages, 1729 KiB

Open AccessArticle

A Rapid HPLC-UV Protocol Coupled to Chemometric Analysis for the Determination of the Major Phenolic Constituents and Tocopherol Content in Almonds and the Discrimination of the Geographical Origin

by Natasa P. Kalogiouri, Petros D. Mitsikaris, Dimitris Klaoudatos, Athanasios N. Papadopoulos and Victoria F. Samanidou

Molecules 2021, 26(18), 5433; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26185433 - 07 Sep 2021

Cited by 8 | Viewed by 2431

Abstract

Reversed phase-high-pressure liquid chromatographic methodologies equipped with UV detector (RP-HPLC-UV) were developed for the determination of phenolic compounds and tocopherols in almonds. Nineteen samples of Texas almonds originating from USA and Greece were analyzed and 7 phenolic acids, 7 flavonoids, and tocopherols (−α, −β + γ) were determined. The analytical methodologies were validated and presented excellent linearity (r² > 0.99), high recoveries over the range between 83.1 (syringic acid) to 95.5% (ferulic acid) for within-day assay (n = 6), and between 90.2 (diosmin) to 103.4% (rosmarinic acid) for between-day assay (n = 3 × 3), for phenolic compounds, and between 95.1 and 100.4% for within-day assay (n = 6), and between 93.2–96.2% for between-day assay (n = 3 × 3) for tocopherols. The analytes were further quantified, and the results were analyzed by principal component analysis (PCA), and agglomerative hierarchical clustering (AHC) to investigate potential differences between the bioactive content of almonds and the geographical origin. A decision tree (DT) was developed for the prediction of the geographical origin of almonds proposing a characteristic marker with a concentration threshold, proving to be a promising and reliable tool for the guarantee of the authenticity of the almonds. Full article

(This article belongs to the Special Issue Chromatography-the Ultimate Analytical Tool)

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19 pages, 3029 KiB

Open AccessArticle

The Evaluation of Multiple Linear Regression–Based Limited Sampling Strategies for Mycophenolic Acid in Children with Nephrotic Syndrome

by Joanna Sobiak, Matylda Resztak, Maria Chrzanowska, Jacek Zachwieja and Danuta Ostalska-Nowicka

Molecules 2021, 26(12), 3723; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26123723 - 18 Jun 2021

Cited by 7 | Viewed by 2386

Abstract

We evaluated mycophenolic acid (MPA) limited sampling strategies (LSSs) established using multiple linear regression (MLR) in children with nephrotic syndrome treated with mycophenolate mofetil (MMF). MLR-LSS is an easy-to-determine approach of therapeutic drug monitoring (TDM). We assessed the practicability of different LSSs for the estimation of MPA exposure as well as the optimal time points for MPA TDM. The literature search returned 29 studies dated 1998–2020. We applied 53 LSSs (n = 48 for MPA, n = 5 for free MPA [fMPA]) to predict the area under the time-concentration curve (AUC_pred) in 24 children with nephrotic syndrome, for whom we previously determined MPA and fMPA concentrations, and compare the results with the determined AUC (AUC_total). Nine equations met the requirements for bias and precision ±15%. The MPA AUC in children with nephrotic syndrome was predicted the best by four time-point LSSs developed for renal transplant recipients. Out of five LSSs evaluated for fMPA, none fulfilled the ±15% criteria for bias and precision probably due to very high percentage of bound MPA (99.64%). MPA LSS for children with nephrotic syndrome should include blood samples collected 1 h, 2 h and near the second MPA maximum concentration. MPA concentrations determined with the high performance liquid chromatography after multiplying by 1.175 may be used in LSSs based on MPA concentrations determined with the immunoassay technique. MPA LSS may facilitate TDM in the case of MMF, however, more studies on fMPA LSS are required for children with nephrotic syndrome. Full article

(This article belongs to the Special Issue Chromatography-the Ultimate Analytical Tool)

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41 pages, 9466 KiB

Open AccessArticle

Counteracting the Ramifications of UVB Irradiation and Photoaging with Swietenia macrophylla King Seed

by Camille Keisha Mahendra, Syafiq Asnawi Zainal Abidin, Thet Thet Htar, Lay-Hong Chuah, Shafi Ullah Khan, Long Chiau Ming, Siah Ying Tang, Priyia Pusparajah and Bey Hing Goh

Molecules 2021, 26(7), 2000; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26072000 - 01 Apr 2021

Cited by 6 | Viewed by 2837

Abstract

In this day and age, the expectation of cosmetic products to effectively slow down skin photoaging is constantly increasing. However, the detrimental effects of UVB on the skin are not easy to tackle as UVB dysregulates a wide range of molecular changes on the cellular level. In our research, irradiated keratinocyte cells not only experienced a compromise in their redox system, but processes from RNA translation to protein synthesis and folding were also affected. Aside from this, proteins involved in various other processes like DNA repair and maintenance, glycolysis, cell growth, proliferation, and migration were affected while the cells approached imminent cell death. Additionally, the collagen degradation pathway was also activated by UVB irradiation through the upregulation of inflammatory and collagen degrading markers. Nevertheless, with the treatment of Swietenia macrophylla (S. macrophylla) seed extract and fractions, the dysregulation of many genes and proteins by UVB was reversed. The reversal effects were particularly promising with the S. macrophylla hexane fraction (SMHF) and S. macrophylla ethyl acetate fraction (SMEAF). SMHF was able to oppose the detrimental effects of UVB in several different processes such as the redox system, DNA repair and maintenance, RNA transcription to translation, protein maintenance and synthesis, cell growth, migration and proliferation, and cell glycolysis, while SMEAF successfully suppressed markers related to skin inflammation, collagen degradation, and cell apoptosis. Thus, in summary, our research not only provided a deeper insight into the molecular changes within irradiated keratinocytes, but also serves as a model platform for future cosmetic research to build upon. Subsequently, both SMHF and SMEAF also displayed potential photoprotective properties that warrant further fractionation and in vivo clinical trials to investigate and obtain potential novel bioactive compounds against photoaging. Full article

(This article belongs to the Special Issue Chromatography-the Ultimate Analytical Tool)

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14 pages, 1349 KiB

Open AccessArticle

Simultaneous Determination of Polyamines and Steroids in Human Serum from Breast Cancer Patients Using Liquid Chromatography–Tandem Mass Spectrometry

by Yu Ra Lee, Ji Won Lee, Jongki Hong and Bong Chul Chung

Molecules 2021, 26(4), 1153; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26041153 - 21 Feb 2021

Cited by 10 | Viewed by 2338

Abstract

A simultaneous quantitative profiling method for polyamines and steroids using liquid chromatography–tandem mass spectrometry was developed and validated. We applied this method to human serum samples to simultaneously evaluate polyamine and steroid levels. Chemical derivatization was performed using isobutyl chloroformate to increase the sensitivity of polyamines. The method was validated, and the matrix effects were in the range of 78.7–126.3% and recoveries were in the range of 87.8–123.6%. Moreover, the intra-day accuracy and precision were in the ranges of 86.5–116.2% and 0.6–21.8%, respectively, whereas the inter-day accuracy and precision were in the ranges of 82.0–119.3% and 0.3–20.2%, respectively. The linearity was greater than 0.99. The validated method was used to investigate the differences in polyamine and steroid levels between treated breast cancer patients and normal controls. In our results, N-acetyl putrescine, N-acetyl spermidine, cadaverine, 1,3-diaminopropane, and epitestosterone were significantly higher in the breast cancer patient group. Through receiver operating characteristic curve analysis, all metabolites that were significantly increased in patient groups with areas under the curve >0.8 were shown. This mass spectrometry-based quantitative profiling method, used for the investigation of breast cancer, is also applicable to androgen-dependent diseases and polyamine-related diseases. Full article

(This article belongs to the Special Issue Chromatography-the Ultimate Analytical Tool)

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Review

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29 pages, 376 KiB

Open AccessReview

Metabolic Profiling and Quantitative Analysis of Cerebrospinal Fluid Using Gas Chromatography–Mass Spectrometry: Current Methods and Future Perspectives

by Alisa Pautova, Natalia Burnakova and Alexander Revelsky

Molecules 2021, 26(12), 3597; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26123597 - 11 Jun 2021

Cited by 10 | Viewed by 3073

Abstract

Cerebrospinal fluid is a key biological fluid for the investigation of new potential biomarkers of central nervous system diseases. Gas chromatography coupled to mass-selective detectors can be used for this investigation at the stages of metabolic profiling and method development. Different sample preparation conditions, including extraction and derivatization, can be applied for the analysis of the most of low-molecular-weight compounds of the cerebrospinal fluid, including metabolites of tryptophan, arachidonic acid, glucose; amino, polyunsaturated fatty and other organic acids; neuroactive steroids; drugs; and toxic metabolites. The literature data analysis revealed the absence of fully validated methods for cerebrospinal fluid analysis, and it presents opportunities for scientists to develop and validate analytical protocols using modern sample preparation techniques, such as microextraction by packed sorbent, dispersive liquid–liquid microextraction, and other potentially applicable techniques. Full article

(This article belongs to the Special Issue Chromatography-the Ultimate Analytical Tool)

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