Application of Analytical Chemistry in Exercise Physiology and Pharmacology

Topic Information

Dear Colleagues,

It is our great pleasure to announce a new Separations Special Issue entitled “Application of Analytical Chemistry in Exercise Physiology and Pharmacology”. The development of analytical chemistry in recent years has been highly noticeable, and new techniques and new methods of application have been introduced into different research areas. Hence, the aim of this proposed Special Issue is to collect updated knowledge about the effectiveness of analytical chemistry in various areas of physiology and pharmacology. We encourage the global scientific community to publish, in open access form, both original papers and high-quality reviews that look at this topic. This Special Issue can be a place to share your own experiences and challenges in developing methods for monitoring exercise physiology and identifying various pharmacological agents that have positive or negative effects on the human body. The determination of both endogenous and exogenous compounds in various biological samples can provide information about the health status of individuals, the level of training effectiveness, the use of prohibited agents, the action of drugs, and many other areas for which you have found a practical application. It is worth sharing this knowledge.

Dr. Andrzej Pokrywka
Prof. Dr. Dorota Kwiatkowska
Topic Editors

Keywords

Participating Journals

Journal Name	Impact Factor	CiteScore	Launched Year	First Decision (median)	APC
Antioxidants antioxidants	7.0	8.8	2012	13.9 Days	CHF 2900	Submit
Biomolecules biomolecules	5.5	8.3	2011	16.9 Days	CHF 2700	Submit
Molecules molecules	4.6	6.7	1996	14.6 Days	CHF 2700	Submit
Pharmaceutics pharmaceutics	5.4	6.9	2009	14.2 Days	CHF 2900	Submit
Separations separations	2.6	2.5	2014	13.6 Days	CHF 2600	Submit

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Published Papers (6 papers)

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17 pages, 1644 KiB  

Open AccessArticle

A One-Step Sample Processing Method in Combination with HPLC-MS/MS for the Simultaneous Quantification of Atorvastatin, Ezetimibe and Three Metabolites including o-Hydroxyl Atorvastatin, p-Hydroxyl Atorvastatin, and Ezetimibe-Glucuronide in Human Plasma

by T. Nguyen Nguyen Le, Nai Ngoc Chuong and Tuan Duc Nguyen

Separations 2023, 10(7), 409; https://0-doi-org.brum.beds.ac.uk/10.3390/separations10070409 - 17 Jul 2023

Cited by 1 | Viewed by 1113

Abstract

A simple and sensitive liquid chromatography–tandem mass spectrometry (LC-MS/MS) method has been developed for the simultaneous determination of atorvastatin (ATOR), ezetimibe (EZM), and their three metabolites, including o-hydroxyl atorvastatin (o-OH ATOR), p-hydroxyl atorvastatin (p-OH ATOR), and ezetimibe–glucuronide [...] Read more.

A simple and sensitive liquid chromatography–tandem mass spectrometry (LC-MS/MS) method has been developed for the simultaneous determination of atorvastatin (ATOR), ezetimibe (EZM), and their three metabolites, including o-hydroxyl atorvastatin (o-OH ATOR), p-hydroxyl atorvastatin (p-OH ATOR), and ezetimibe–glucuronide (EZM-G) in human plasma using benzyl paraben (BP) as the internal standard (IS). The analytes and IS were ionized using ESI positive ion mode (ATOR, o-OH ATOR, and p-OH ATOR), ESI negative ion mode (EZM, EZM-G, and BP), and operated in multiple reaction monitoring (MRM) mode. They were then extracted via salting-out assisted liquid–liquid extraction with acetonitrile and analyzed via liquid chromatography on a reversed-phase chromatographic column (50 mm × 4.6 mm; 3.5 µm) using a mixture of acetonitrile and an acetic acid solution (0.5%) as the mobile phase, showing high extraction efficiency (>70%), and a minimized matrix effect. The method was satisfactorily validated, and it showed excellent linearity over wide concentration ranges of 0.06–15 ng/mL, 0.6–150 ng/mL, 0.4–100 ng/mL, 0.12–30 ng/mL, and 0.05–3 ng/mL for EZM, EZM-G, ATOR, o-OH ATOR, and p-OH ATOR, respectively. Full article

(This article belongs to the Topic Application of Analytical Chemistry in Exercise Physiology and Pharmacology)

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12 pages, 2051 KiB  

Open AccessArticle

Self-Declared and Measured Prevalence of Glucocorticoid Use in Polish Athletes

by Andrzej Pokrywka, Daria Berezovska, Sylwia Lewandowska-Pachecka, Jarosław Krzywański, Michał Rynkowski, Mariola Wicka, Dorota Kwiatkowska and Raphael Faiss

Separations 2023, 10(3), 204; https://0-doi-org.brum.beds.ac.uk/10.3390/separations10030204 - 15 Mar 2023

Viewed by 1500

Abstract

Glucocorticoids (GCs) are included in the list of prohibited substances and methods in sport published annually by the World Anti-Doping Agency (WADA). In its 2022 update, the WADA list prohibits all injectable routes of administration of GCs for use during in-competition periods. Previously, [...] Read more.

Glucocorticoids (GCs) are included in the list of prohibited substances and methods in sport published annually by the World Anti-Doping Agency (WADA). In its 2022 update, the WADA list prohibits all injectable routes of administration of GCs for use during in-competition periods. Previously, GCs were prohibited in-competition when administered by oral, intravenous, intramuscular, or rectal routes, but local injections (in addition to topical applications) were allowed. This study first investigated the prevalence of GC use by athletes in Poland, declared in 2130 doping control forms, and the related 2130 urine samples analysed at the Polish Anti-Doping Laboratory. Second, the validity of the analytical methodology to detect GCs was evaluated with the updated WADA requirement for substance-specific minimum reporting levels and considering the proposed washout periods. Despite the new regulation in place, the use of 30 different GC preparations were declared in a total of 162 occurrences (8% of the tests) with therapeutic purposes. Laboratory analyses resulted in the presence of GCs in 16 occurrences with only two samples with a concentration triggering an adverse analytical finding. Our study allowed us to confirm that the applied methodology for the determination of GCs in urine samples (ultra-high-performance liquid chromatography–tandem mass spectrometry) remains fully valid after the latter regulation change while the challenge to assess the timing and administration route for GCs persists. Full article

(This article belongs to the Topic Application of Analytical Chemistry in Exercise Physiology and Pharmacology)

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15 pages, 5253 KiB  

Open AccessArticle

Investigation of the Excretion of Triamcinolone Acetonide and Its Metabolite

by Dorota Kwiatkowska, Mariola Wicka, Ewa Bulska and Pawel Kaliszewski

Separations 2023, 10(3), 164; https://0-doi-org.brum.beds.ac.uk/10.3390/separations10030164 - 27 Feb 2023

Cited by 3 | Viewed by 1142

Abstract

Triamcinolone acetonide (TA) is a synthetic corticosteroid commonly used in medical practice to treat various skin conditions, including eczema, dermatitis, and allergies. It is a highly potent derivative of triamcinolone, with a strength that is about eight times greater than prednisone. Although it [...] Read more.

Triamcinolone acetonide (TA) is a synthetic corticosteroid commonly used in medical practice to treat various skin conditions, including eczema, dermatitis, and allergies. It is a highly potent derivative of triamcinolone, with a strength that is about eight times greater than prednisone. Although it is sometimes used by athletes, it is important to note that the World Anti-Doping Agency (WADA) prohibits the use of glucocorticoids in competition when administered via injection, oral (including oromucosal, such as buccal, gingival, or sublingual), or rectal routes. However, they are allowed if administered otherwise, such as via inhalation or topical application to the skin. Anti-doping laboratories generally report Adverse Analytical Findings (AAF) for glucocorticoid group substances when their estimated concentration exceeds 30 ng/mL, with some exceptions such as triamcinolone acetonide, which has a reporting limit of 15 ng/mL. It is important to note that this only applies to the parent compound of specified metabolites. To address interpretation issues that can arise with other glucocorticoids, such as budesonide, the authors of this study investigated whether similar issues occur with triamcinolone acetonide. Specifically, they examined whether therapeutic doses of the commonly used medication Previsone could result in anti-doping rule violations due to the presence of triamcinolone acetonide and its metabolites in urine. The study involved ten healthy volunteers, and the analytical procedure was developed using liquid/liquid extraction, hydrolysis, and LC/MS/MS analysis. The results of the study showed that topical administration of therapeutic doses of Previsone does not pose a threat of anti-doping rules violation, as the excretion of the parent compound does not exceed the reporting limit in urine. Additionally, the concentration of 6β-hydroxy Triamcinolone acetonide was also well below the reporting limit. Full article

(This article belongs to the Topic Application of Analytical Chemistry in Exercise Physiology and Pharmacology)

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19 pages, 4976 KiB  

Open AccessEditor’s ChoiceArticle

Determination of 27 Glucocorticoids in Urine by Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry Using UniSpray^TM Source

by Mariola Wicka, Krzysztof Grucza, Aleksandra Drapała, Patryk Konarski and Dorota Kwiatkowska

Separations 2023, 10(3), 155; https://0-doi-org.brum.beds.ac.uk/10.3390/separations10030155 - 24 Feb 2023

Cited by 1 | Viewed by 1597

Abstract

Glucocorticoids (GCs) are a group of the most important and commonly used anti-inflammatory, antiallergenic, and immunosuppressive drugs. Like narcotics, they can be addictive if taken at increasing doses to achieve greater analgesic effects. The purpose of the study was to develop initial and [...] Read more.

Glucocorticoids (GCs) are a group of the most important and commonly used anti-inflammatory, antiallergenic, and immunosuppressive drugs. Like narcotics, they can be addictive if taken at increasing doses to achieve greater analgesic effects. The purpose of the study was to develop initial and confirmation testing analytical methods that would allow for the identification of glucocorticoid class substances in human urine to be used for routine analyses for the purposes of prosecution in the case of abuse, for clinical toxicology, medical jurisprudence, as well as for routine testing of athletes for the presence of prohibited substances in sports by means of ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) using a new generation ionization source UniSprayTM (U.S). This new method allows for the simultaneous detection of 27 glucocorticoids in human urine using LC-MS/MS. The tests conducted yielded relatively low LOD and LOQ values, ranging from 0.06 ng/mL to 0.14 ng/mL and 0.75 ng/mL for LOD and LOQ, respectively. Full article

(This article belongs to the Topic Application of Analytical Chemistry in Exercise Physiology and Pharmacology)

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9 pages, 1526 KiB  

Open AccessArticle

Determination of Ecdysterone in Dietary Supplements and Spinach by Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry

by Krzysztof Grucza, Mariola Wicka, Aleksandra Drapała and Dorota Kwiatkowska

Separations 2022, 9(1), 8; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9010008 - 29 Dec 2021

Cited by 9 | Viewed by 3919

Abstract

Ecdysterone is a naturally occurring steroid hormone of the ecdysteroid class. This group is widely marketed to athletes in dietary supplements as a “natural anabolic agent”, advertised to increase strength and muscle mass during resistance training, reduce fatigue and ease recovery. The aim [...] Read more.

Ecdysterone is a naturally occurring steroid hormone of the ecdysteroid class. This group is widely marketed to athletes in dietary supplements as a “natural anabolic agent”, advertised to increase strength and muscle mass during resistance training, reduce fatigue and ease recovery. The aim of the study was to develop and validate a straightforward approach for identifying ecdysterone in dietary supplements by means of ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). Furthermore, due to the fact that ecdysterone is one of the compounds naturally occurring in spinach, the fit-for-purpose method for extraction and identification of ecdysterone in spinach is proposed. The validity of the developed method was confirmed with the use of a reference standard and the limit of detection (LOD) for ecdysterone was established at 1 mg/g supplement. The presence of ecdysterone was confirmed in all tested supplements at estimated concentrations ranging between 5 mg/g and 383 mg/g. Full article

(This article belongs to the Topic Application of Analytical Chemistry in Exercise Physiology and Pharmacology)

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20 pages, 3522 KiB  

Open AccessArticle

Determination of the Dissociation Constants of 16 Active Ingredients in Medicinal Herbs Using a Liquid–Liquid Equilibrium Method

by Wanying Wang, Baixiu Zheng, Jiahao Wu, Weisong Lv, Peiying Lin and Xingchu Gong

Separations 2021, 8(4), 49; https://doi.org/10.3390/separations8040049 - 14 Apr 2021

Cited by 5 | Viewed by 2510

Abstract

The dissociation constant is an important physicochemical property of drug molecules that affects the pharmacokinetic and pharmacodynamic properties of drugs. In this study, the distribution coefficients of 16 active ingredients extracted from herbal materials were determined at different pH values in liquid–liquid equilibrium [...] Read more.

The dissociation constant is an important physicochemical property of drug molecules that affects the pharmacokinetic and pharmacodynamic properties of drugs. In this study, the distribution coefficients of 16 active ingredients extracted from herbal materials were determined at different pH values in liquid–liquid equilibrium systems; the active ingredients were sinomenine, aescin A, aescin B, aescin C, aescin D, chlorogenic acid, neochlorogenic acid, cryptochlorogenic acid, isochlorogenic acid A, isochlorogenic acid B, isochlorogenic acid C, baicalin, wogonoside, calycosin-7-glucoside, astraisoflavan-7-O-β-D-glucoside, and isomucronulatol 7-O-glucoside. The dissociation constants of these active ingredients were calibrated and compared with reported values. The dissociation constants obtained were close to those reported in other studies, which means that the results of this work are reliable. Full article

(This article belongs to the Topic Application of Analytical Chemistry in Exercise Physiology and Pharmacology)

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