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Separations
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HPLC: A Key Tool for Analytical Chemistry
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HPLC: A Key Tool for Analytical Chemistry

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

Deadline for manuscript submissions: closed (10 May 2023) | Viewed by 12362

Special Issue Editor

Dr. Salvatore Barreca

E-Mail Website
Guest Editor
ARPA Lombardia, UOC Lab Milano, Sede Lab Monza & Brianza, Via Solferino 16, I-20900 Monza, MB, Italy
Interests: analytical chemistry; UHPLC; separation techniques; hyphenated techniques; separated components
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Over the last twenty years, high-pressure liquid chromatography (HPLC, UHPLC) hyphenated with several different detectors, has become one of the most useful methods worldwide for the separation and analysis of complex mixtures in many scientific fields, especially, analytical chemistry.

The ongoing evolution of HPLC has included advances in components such as stationary phases used in separation columns, green solvents, detection systems, data handling systems, and sample preparation.

This Special Issue of Separations “HPLC- A Key Tool on Analytical Chemistry” will illustrate the latest research and advancements in HPLC/UHPLC technology and applications. 

This Special Issue accepts contributions that cover all research aspects related to analytical chemistry, and several scientific macro-areas can also be included, such as green analytical chemistry, environmental chemistry and pharmacy, chemometrics, and food and nutrition.

Dr. Salvatore Barreca
Guest Editor

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. Separations is an international peer-reviewed open access monthly 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 2600 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

  • Analytical chemistry
  • UHPLC
  • Separation techniques
  • Hyphenated techniques
  • Separated components

Published Papers (5 papers)

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Research

13 pages, 1563 KiB  
Article
HPLC-DAD Development and Validation Method for Short-Chain Fatty Acids Quantification from Chicken Feces by Solid-Phase Extraction
by Lenin Rodolfo Díaz-Corona, Karina Jeanette Parra-Saavedra, Renata Sofia Mora-Alonzo, María Esther Macías-Rodríguez, Alma H. Martínez-Preciado, Santiago José Guevara-Martínez, Adalberto Zamudio-Ojeda and Adriana Macaria Macias-Lamas
Separations 2023, 10(5), 308; https://0-doi-org.brum.beds.ac.uk/10.3390/separations10050308 - 13 May 2023
Cited by 1 | Viewed by 2124
Abstract
A solid-phase extraction (SPE) process, followed by an HPLC-DAD method, was developed and validated to quantify short-chain fatty acids (SCFAs) and applied to analyze chicken feces samples. This study aimed to report the use of the STRATATM-X-A 96 Well Plate SPE [...] Read more.
A solid-phase extraction (SPE) process, followed by an HPLC-DAD method, was developed and validated to quantify short-chain fatty acids (SCFAs) and applied to analyze chicken feces samples. This study aimed to report the use of the STRATATM-X-A 96 Well Plate SPE cartridge method as the first step in quantifying SCFAs. A stationary reverse-phase Luna Omega C18 column kept at 40 °C was used, with a gradient elution mobile phase (H2SO4 and Acetonitrile, 98:2), a flow rate of 1.2 mL/min, and detection at 210 nm. A mixture of acetic, propionic, and butyric acid was used as thestandard. The method showed a linear relationship, with a coefficient of determination of R2 = 0.9987, R2 = 0.9985, and R2 = 0.9966 for acetic, propionic, and butyric acid, respectively. Concerning sensitivity, an LOD and LOQ of 0.14, 0.14, 0.14 mg/mL and 0.44, 0.45, 0.43 mg/mL were obtained for acetic, propionic, and butyric acid, respectively. According to the sample analysis, the accuracy was 76.05, 95.60, and 81.56% for acetic, propionic, and butyric acid, respectively. The developed method is simple, fast, linear, sensitive, accurate, precise, and robust for the quantification of SCFAs. This could serve as an alternative to conventional methodologies for the determination of these critical components in the intestinal health of chicken feces. Full article
(This article belongs to the Special Issue HPLC: A Key Tool for Analytical Chemistry)
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21 pages, 2112 KiB  
Article
Box–Behnken Design Based Development of UV-Reversed Phase High Performance Liquid Chromatographic Method for Determination of Ascorbic Acid in Tablet Formulations
by Syed Najmul Hejaz Azmi, Umaima Al Hoqani, Juhaina Obaid Said Al Mamari, Buthaina Mohamed Salim Al Mamari, Balaqis Sultan Ali Rashid Al Jassasi, Aziza Saleh Saif Al Rubaiai, Nafisur Rahman, Mohd Nasir, Sk Manirul Haque, Shah Alam Khan, Qamar Uddin Ahmed and Zainul Amiruddin Zakaria
Separations 2022, 9(11), 361; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9110361 - 09 Nov 2022
Cited by 4 | Viewed by 2063
Abstract
A simple, sensitive, accurate and inexpensive UV-reversed-phase high-performance liquid chromatographic method was developed for the determination of ascorbic acid in tablet formulations. The method was based on the separation of ascorbic acid using a mobile phase of an acetonitrile-NaH2PO4-H [...] Read more.
A simple, sensitive, accurate and inexpensive UV-reversed-phase high-performance liquid chromatographic method was developed for the determination of ascorbic acid in tablet formulations. The method was based on the separation of ascorbic acid using a mobile phase of an acetonitrile-NaH2PO4-H3PO4 buffer solution (pH = 3) (5:95 v/v) with a UV detection wavelength of 245 nm and a flow rate of 0.8 mL min−1 at ambient column temperature. The variables of the proposed method, such as acetonitrile fraction (%), flow rate (mL min−1) and column temperature (°C), were optimized on the peak area by response surface methodology via the Box–Behnken design. The mobile phase was passed isocratically, and the separation of ascorbic acid was performed at the retention time of 4.1 min. A calibration graph was obtained and found to be linear in the concentration range of 10–180 µg mL−1. The method suitability was assessed and an asymmetry factor of 1.15 was obtained. The proposed method was successfully applied for the determination of ascorbic acid in tablet formulations and statistically compared with the results of the reference method. The performance of the proposed method was excellent and in agreement with the reference method. The recovery percentage of the proposed and reference methods was in the range of 99.98–100.04% and showed compliance (100 ± 2%) with regulatory guidelines. Full article
(This article belongs to the Special Issue HPLC: A Key Tool for Analytical Chemistry)
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10 pages, 895 KiB  
Article
Development and Validation of HPLC-DAD Method for the Determination of Favipiravir and Studying the Impact of Vitamin C on the Pharmacokinetics of COVID-19 Antiviral Drug Favipiravir
by Mohammad Hailat, Israa Al-Ani, Zainab Zakareia, Ramadan Al-Shdefat, Osaid Al-Meanazel, Md. Khalid Anwer, Mohammed Hamad, Walid Abu Rayyan, Riad Awad and Wael Abu Dayyih
Separations 2022, 9(10), 303; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9100303 - 11 Oct 2022
Cited by 6 | Viewed by 1999
Abstract
A novel, sensitive, and low-cost HPLC method for the rapid determination of favipiravir (FVR) in rat plasma was developed and validated, and the effect of vitamin C on FVR pharmacokinetic parameters was investigated. FVR and oxcarbazepine (IS) were separated using a mobile phase [...] Read more.
A novel, sensitive, and low-cost HPLC method for the rapid determination of favipiravir (FVR) in rat plasma was developed and validated, and the effect of vitamin C on FVR pharmacokinetic parameters was investigated. FVR and oxcarbazepine (IS) were separated using a mobile phase of 50% acetonitrile and 50% water (with 0.25% trifluoroacetic acid) at 1.0 mL/min flow rate and detected at λmax 289 nm. The intra- and interday values for FVR in plasma were less than 15%, with low, medium, and high QC levels for the relative recovery rate, according to ICH guidelines. Cmax values in the control and experimental groups were 558 ± 124.42 and 979.13 ± 138.10 ng/mL, respectively; t1/2 values were 7.15 ± 1.60 and 9.09 ± 1.14 h, AUC(0-t) values were 5697.70 ± 536.58 and 7381.62 ± 1577.58 ng.h/mL, and AUC(0-∞) values were 5697.70 ± 536.58 and 8192.36 ±  1721.67, respectively. According to the results, the experimental group’s Cmax of FVR was 75.17% higher than the control group’s, the Vz/F was lower, and the t1/2 was 1.86 h longer. The technique developed for determining FVR in plasma was useful for FVR pharmacokinetics and food–drug interaction investigations. Full article
(This article belongs to the Special Issue HPLC: A Key Tool for Analytical Chemistry)
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10 pages, 217 KiB  
Article
Study on the Stability of Antibiotics, Pesticides and Drugs in Water by Using a Straightforward Procedure Applying HPLC-Mass Spectrometric Determination for Analytical Purposes
by Salvatore Barreca, Carola Forni, Luisa Colzani, Laura Clerici, Daniela Daverio and Pierluisa Dellavedova
Separations 2021, 8(10), 179; https://0-doi-org.brum.beds.ac.uk/10.3390/separations8100179 - 09 Oct 2021
Cited by 10 | Viewed by 2000
Abstract
The stability of analytes is a critical point in chemical analysis, especially in the field of trace levels residue analysis. Nowadays, due to advances in analytical technology and in separation sciences, the analyses of water have been improved. Unfortunately, in this context, one [...] Read more.
The stability of analytes is a critical point in chemical analysis, especially in the field of trace levels residue analysis. Nowadays, due to advances in analytical technology and in separation sciences, the analyses of water have been improved. Unfortunately, in this context, one of the most critical issues in water analysis include compound stability from sampling station to laboratory procedures. This study was carried out to explore the stability of several compounds in water from sampling to analysis concerning analytes reported in implementing decision 2018/840—Watch List. During method development and validation, the stability of compounds was investigated to detect the best operating conditions concerning sampling, extraction and analysis. In this paper, we report a study on the stability of antibiotics, pesticides and drugs in water determined using a straight-forward procedure applying mass spectrometric detection for analytical purposes. The laboratory tests were performed in Milli-Q water and surface water by analyzing samples through direct injection, solvent mixture (Water/ACN) and solid phase extraction system from time 0 to 168 h. All the analytes of the WL are stable in aqueous solutions with the addition of at least 25% ACN even after 168 h, and the analytes have shown a matrix effect on recovery of some analytes such as Famoxadone from sampling results (recovery in surface water 72%). For all the analytes investigated, recoveries were between 70 and 130% by using SPE procedures before UHPLC-MS/MS analysis, which is in good agreement with method validation procedures. Full article
(This article belongs to the Special Issue HPLC: A Key Tool for Analytical Chemistry)
12 pages, 282 KiB  
Article
Analysis of Selected Mycotoxins in Maize from North-West South Africa Using High Performance Liquid Chromatography (HPLC) and Other Analytical Techniques
by Theodora Ijeoma Ekwomadu, Toluwase Adeseye Dada, Stephen Abiola Akinola, Nancy Nleya and Mulunda Mwanza
Separations 2021, 8(9), 143; https://0-doi-org.brum.beds.ac.uk/10.3390/separations8090143 - 03 Sep 2021
Cited by 15 | Viewed by 2496
Abstract
Contamination of foods by mycotoxins is linked to various health and economic implications. This study evaluated the incidence of mycotoxins in commercial and small-scale maize and evaluated potential health risks for consumers based on South African and international regulations. The sensitivity/specificity of HPLC [...] Read more.
Contamination of foods by mycotoxins is linked to various health and economic implications. This study evaluated the incidence of mycotoxins in commercial and small-scale maize and evaluated potential health risks for consumers based on South African and international regulations. The sensitivity/specificity of HPLC over other analytical methods used was also ascertained. In total, 100 maize samples were analyzed using immuno-affinity column for extraction and clean-up, thin layer chromatography (TLC), HPLC, and enzyme linked immunosorbent assay (ELISA) for quantification. Results revealed that fumonisinB1 was the most contaminant mycotoxin in both small-scale and commercial samples with incidence rates of 100% and 98.6%, respectively. Aflatoxins contamination occurred at incidences of 26.7% in small-scale and 25.0% in commercial samples. Furthermore, ochratoxin A had high incidence rates of 97.8% and 93.0% and ranged from 3.60–19.44 µg/kg and 1.60–9.89 µg/kg, respectively, in small-scale and commercial samples, while ZEA occurred in 50% and 55% of small-scale and commercial samples, respectively. Results demonstrate that maize, especially from small-scale farmers, may contribute to dietary exposure to mycotoxins. Farmers and consumers should be alerted to the dangers of mycotoxins contamination in maize with resultant health risks. Additionally, HPLC method was also found to be more specific for mycotoxin detection than ELISA. Full article
(This article belongs to the Special Issue HPLC: A Key Tool for Analytical Chemistry)
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