Monitoring plasma concentrations of β-lactam antibiotics is crucial, particularly in critically ill patients, where variations in concentrations can lead to treatment failure or adverse events. Standardized antimicrobial regimens may not be effective for all patients, especially in special groups with altered physiological parameters. Pharmacokinetic/pharmacodynamic (PK/PD) studies highlight the time-dependent antibacterial activity of these antibiotics, emphasizing the need for personalized dosing. Therapeutic drug monitoring (TDM) is essential, requiring rapid and accurate analytical methods for precise determination of drugs in biological material (typically plasma or serum). This study presents a novel capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) method designed for the simultaneous quantification of five penicillin antibiotics, two cephalosporins, one carbapenem, and two β-lactamase inhibitors in a single run. The method involves a simple sample pretreatment-precipitation with organic solvent-and has a run time of 20 min. Optimization of CZE separation conditions revealed that 20 mM ammonium hydrogen carbonate (NH4HCO3) serves as the optimal background electrolyte (BGE). Positive electrospray ionization (ESI) mode, with isopropyl alcohol (IP)/10 mM ammonium formate water solution (50/50, v/v) as the sheath liquid, was identified as the optimal condition for MS detection. Method validation according to the Food and Drug Administration (FDA) guideline for development of bioanalytical methods demonstrated satisfactory selectivity, linearity, recovery, robustness, and stability. The method's practicality was evaluated using the Blue Applicability Grade Index (BAGI), yielding a score of 77.5. Moreover, the greenness of the proposed method was evaluated by two commonly used metric tools-Analytical GREEnness (AGREE) and Green Analytical Procedure Index (GAPI). The developed CZE-MS/MS method offers a practical and reliable approach for quantifying a broad spectrum of β-lactam antibiotics in plasma. Its ability to simultaneously quantify multiple analytes in a single run, coupled with a straightforward sample pretreatment, positions it as a valuable and prospective tool for TDM in critically ill patients.

• Publikační typ
• časopisecké články MeSH

Short-chain fatty acids (SCFAs) are the main metabolites produced by bacterial fermentation of non-digestible carbohydrates in the gastrointestinal tract. They can be seen as the major flow of carbon from the diet, through the microbiome to the host. SCFAs have been reported as important molecules responsible for the regulation of intestinal homeostasis. Moreover, these molecules have a significant impact on the immune system and are able to affect inflammation, cardiovascular diseases, diabetes type II, or oncological diseases. For this purpose, SCFAs could be used as putative biomarkers of various diseases, including cancer. A potential diagnostic value may be offered by analyzing SCFAs with the use of advanced analytical approaches such as gas chromatography (GC), liquid chromatography (LC), or capillary electrophoresis (CE) coupled with mass spectrometry (MS). The presented review summarizes the importance of analyzing SCFAs from clinical and analytical perspective. Current advances in the analysis of SCFAs focused on sample pretreatment, separation strategy, and detection methods are highlighted. Additionally, it also shows potential areas for the development of future diagnostic tools in oncology and other varieties of diseases based on targeted metabolite profiling.

• Publikační typ
• časopisecké články MeSH
• přehledy MeSH

Úvod: Polyfarmácia (polyfarmakoterapia) je závažným problémom u seniorov, cieľom práce bolo porovnať farmakoterapiu a polyfarmáciu u seniorov v sociálnych zariadeniach v rokoch 2001 a 2019. Metodika: K 31. decembru 2001 sme zisťovali údaje o farmakoterapii 151 obyvateľov dvoch domovov dôchodcov (priemerný vek 75,1 rokov, 68,9 % žien). Výsledky sme porovnali s farmakoterapiou obyvateľov dvoch zariadení pre seniorov k 31. októbru 2019 (237 seniorov, priemerný vek 80,5 rokov, 73,4 % žien). Podľa zdravotných záznamov sme porovnávali pravidelne užívané lieky u všetkých obyvateľov, užívanie liekov podľa veku a pohlavia, užívanie 0 - 4 liekov, 5 - 9 liekov, 5 a viac liekov, 10 a viac liekov, skupiny liekov podľa ATC klasifikácie. Pri štatistickom spracovaní sme použili t‐test a chí-kvadrátový test. Výsledky: V roku 2001 obyvatelia pravidelne užívali spolu 891 liekov, o 18 rokov neskôr užívali obyvatelia spolu 2099 liekov. Pozorovali sme signifikantné zvýšenie priemerného počtu pravidelne užívaných liekov jedným obyvateľom o viac ako polovicu (z 5,90 liekov na 8,86 liekov); u žien z 6,11 liekov na 9,24 liekov a u mužov z 5,45 liekov na 7,81 liekov. Počet obyvateľov s polyfarmáciou (pravidelné užívanie ≥ 5 liekov) sa zvýšil takmer o štvrtinu (z 70,2 % na 87,3 %) a počet seniorov s excesívnou polyfarmáciou (pravidelné užívanie ≥ 10 liekov) vzrástol 4,6 násobne (z 9,3 % na 43,5 %). Záver: Naša práca potvrdila, že v priebehu 18 rokov sa u seniorov v inštitúciách sociálneho typu zvýšil počet užívaných liekov. Poukazuje aj na trend zvyšovania polyfarmácie a excesívnej polyfarmácie u seniorov, osobitne vo veku 75+ rokov a u žien.

Introduction: Polypharmacy (polypharmacotherapy) is a serious problem among seniors. The aim of the work was to compare pharmacotherapy and polypharmacy among seniors in social facilities in 2001 and 2019. Methodology: As of December 31, 2001, we collected data on the pharmacotherapy of 151 residents of two retirement homes (average age 75.1 years, 68.9% women). We compared the results with the pharmacotherapy of residents of two facilities for seniors as of October 31, 2019 (237 seniors, average age 80.5 years, 73.4% women). According to the medical records, we determined and compared the regularly used medicines of all residents, the use of medicines by age and sex, the use of 0-4 medicines, 5-9 medicines, 5 or more medicines, 10 or more medicines and the groups of medicines according to the ATC classification. For statistical processing, we used the t-test and chi-square test. Results: In 2001, residents regularly used a total of 891 medicines, 18 years later, they used a total of 2099 medicines. We observed a significant increase in the average number of regularly used medications per resident by more than a half (from 5.90 medications to 8.86 medications), in women from 6.11 drugs to 9.24 drugs and in men from 5.45 drugs to 7.81 drugs. The number of residents with polypharmacy (regular use of ≥ 5 drugs) increased by almost a quarter (from 70.2% to 87.3%), and the number of seniors with excessive polypharmacy (regular use of ≥ 10 drugs) increased 4.6 times (from 9, 3% to 43.5%). Conclusion: Our work confirmed that over the course of 18 years, the number of medications used by seniors in social-type institutions has increased. It also points to the trend of increasing polypharmacy and excessive polypharmacy among seniors, especially at the age of 75+ and among women.

• MeSH
• domovy pro seniory * MeSH
• lidé MeSH
• polyfarmacie * MeSH
• senioři nad 80 let MeSH
• senioři MeSH
• Check Tag
• lidé MeSH
• mužské pohlaví MeSH
• senioři nad 80 let MeSH
• senioři MeSH
• ženské pohlaví MeSH
• Geografické názvy
• Slovenská republika MeSH

Prezentovaná práca sa zameriava na vývoj a validáciu analytickej metódy na báze kapilárnej zónovej elektroforézy v spojení s UV detekciou pre simultánne stanovenie tramadolu a paracetamolu vo farmaceutických a biologických vzorkách. Základný elektrolyt bol tvorený 50 mM uhličitanom amónnym, ktorý predstavuje pomerne atypický elektrolytový systém. Vyvinutá metóda disponuje vhodnými validačnými parametrami ako linearita (koeficient determinácie r2 ≥ 0,995), selektivita alebo medza dôkazu na úrovni 0,25 – 0,5 μg/ml. Metóda bola charakterizovaná adekvátnymi hodnotami presnosti a správnosti, ktoré boli v súlade s kritériami validačných smerníc, či už pre matrice farmaceutického alebo biologického charakteru. Detekcia bola uskutočnená pri vlnovej dĺžke 200 nm. Daná metóda bola úspešne použitá pre potreby stanovenia tramadolu a paracetamolu v rozličných liekových formách a v biologickej matrici moču. Dosiahnuté výsledky indikujú potenciál začlenenia metódy do procesov kontroly kvality liečiv a/alebo bioanalýzy.

The aim of the present study is the development and validation of a simple method based on capillary zone electrophoresis coupled with UV detection for simultaneous determination of tramadol and paracetamol in pharmaceutical and biological samples. The background electrolyte was composed of 50 mM ammonium carbonate, which is a type of a non-conventional electrolyte system. The developed method was characterized by suitable validation parameters, such as linearity (coefficient of determination r2 ≥ 0,995), selectivity or the limit of detection at the level of 0.25 – 0.5 μg/ml. Acceptable values of accuracy and precision were obtained, which were in good agreement with the recommended validation guidelines for analysis of pharmaceutical and biological samples. Detection was performed at a wavelength of 200 nm. The developed method was successfully applied to determine tramadol and paracetamol in various dosage forms and in urine biological samples. Achieved results indicate a potential of the method to be integrated in the common quality control processes of drugs and/or in bioanalysis.

• MeSH
• analýza moči metody   MeSH
• elektroforéza * metody   MeSH
• léčivé přípravky analýza   MeSH
• lidé MeSH
• paracetamol * analýza   MeSH
• tramadol * analýza   MeSH
• Check Tag
• lidé MeSH

Oxandrolone, a synthetic testosterone analog, is used for the treatment of several diseases associated with weight loss. Unfortunately, oxandrolone is abused by many athletes and bodybuilders due to its strong anabolic effect. We have developed and validated a highly sensitive and rapid on-line SPE-UHPLC-MS/MS method for the determination of oxandrolone and simultaneous identification of its major metabolite 17-epi-oxandrolone in urine matrices. Enrichment of the analytes via an integrated solid-phase extraction was achieved using an Acquity UPLC BEH C18 Column. Subsequently, the chromatographic separation of the on-line preconcentrated sample fraction was achieved using an Acquity HSS T3 C18 Column. For the structural identification of these analytes, a high-resolution mass spectrometer Synapt-G2Si coupled to the Acquity M-class nano-LC system with ionKey source was used. A highly sensitive determination of oxandrolone was achieved using a tandem quadrupole mass spectrometer XEVO TQD. The method was successfully validated in the linear range of oxandrolone from 81.63 pg·mL-1 (limit of quantification, LOQ) to 5000 pg·mL-1 in the human urine matrix. It was applied to the analysis of real urine samples obtained from a healthy volunteer after the oral administration of one dose (10 mg) of oxandrolone. Concentration vs. time dependence was tested in the time interval of 4 h-12 days (after oral administration) to demonstrate the ability of the method to detect the renal elimination of oxandrolone from the human body. Favorable performance parameters along with successful application indicate the usefulness of the proposed method for its routine use in antidoping control labs.

• MeSH
• analýza moči metody   MeSH
• extrakce na pevné fázi metody   MeSH
• lidé MeSH
• oxandrolon izolace a purifikace   metabolismus   moč   MeSH
• tandemová hmotnostní spektrometrie metody   MeSH
• vysokoúčinná kapalinová chromatografie metody   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH

Práca sa zameriava na vývoj jednoduchej analytickej metódy na báze kapilárnej zónovej elektroforézy v spojení s UV-detekciou pre simultánne stanovenie tiamínu a pyridoxínu vo vzorkách farmaceutického a potravinárskeho charakteru. Separácia tiamínu a pyridoxínu prebiehala v elektrolytovom systéme 25 mmol ∙ l–1 GABA + 50 mmol ∙ l–1 HAc+ 0,05% m-HEC. Detekcia bola uskutočnená pri vlnovej dĺžke 260 nm. Medza detekcie pre tiamín bola 0,059 µg ∙ ml–1 a pre pyridoxín 0,23 µg ∙ ml–1. Tieto hodnoty naznačujú, že metóda je vhodná na stanovenie relatívne nízkych koncentrácií tiamínu a pyridoxínu. Uvedená CZE-UV metóda umožnila efektívne stanovenie obsahu dvojice vitamínov v piatich výživových doplnkoch a jedenástich energetických nápojoch a vitamínových vodách.

The paper is focused on development of a simple analytical method based on capillary zone electrophoresis in combination with UV-detection for simultaneous detemination of thiamine and pyridoxine in pharmaceutical and food samples. The separation of thiamine and pyridoxine was performed in a background electrolyte composed of 25 mmol ∙ l–1 GABA + 50 mmol ∙ l–1 HAc+ 0.05% m-HEC. The UV detector was set at the constant wavelength of 260 nm. Limit of detection was 0.059 µg ∙ ml–1 for thiamine and 0.23 µg ∙ ml–1 for pyridoxine. These levels suggest that relatively low quantities of thiamine and pyridoxine can be detected. The presented CZE-UV method enabled effective determination of the two vitamins in 5 food supplements and 11 energy drinks and vitamin waters.

• Klíčová slova
• UV detekce,
• MeSH
• elektroforéza kapilární metody   MeSH
• potravní doplňky * analýza   MeSH
• pyridoxin analýza   MeSH
• řízení kvality MeSH
• thiamin analýza   MeSH

Reliable, fast, simple and low-cost analytical procedure based on radionuclide X-ray fluorescence spectrometry (RRFS) was proposed to identify and determine heavy metals in various antitussive preparations of synthetic and biological origin. Various materials (tablet dosage forms, granules, plants) can be analyzed directly without the need of isolation of the analyzed compounds from their matrices so that errors in the analytical process are minimized. External matrices, such as Medicago sativa L. , benzoic acid, and dextran were proposed to quantify heavy metals in some problematic materials ( Farfarereae folium , effervescent tablets of medicine ACC long, hard capsules of various homeopathics, respectively) that had not allowed homogeneous implementation of standard addition of analyzed elements into the standardized tablet forms used for the RRFS analysis. The appropriate external matrices were consistent with the original ones in terms of matrix effects (e.g., background noise produced and approximate levels of naturally occurring heavy metals studied), and they allowed to prepare well defined tablets including required amounts of the standard additions of heavy metals providing proper calibration parameters. The RRFS method applied for the original or external matrices enabled an effective and economic control of antitussive preparations for selected heavy metals contents evaluated according to the established directives and laws. Hence, it is recommended for a routine use in quality control laboratories.

• MeSH
• antitusika analýza   chemie   MeSH
• fluorescenční spektrometrie metody   MeSH
• kontaminace léku * MeSH
• kontrola léčiv a omamných látek * MeSH
• léčivé rostliny chemie   MeSH
• rostlinné extrakty * analýza   chemie   MeSH
• těžké kovy analýza   MeSH

Chronic obstructive pulmonary disease (COPD) is a slowly progressive, largely non-reversible pulmonary disease that is characterized by airflow limitation. The disease encompasses multiple structural and functional components, but inflammation is at the core of the disease affecting both the lungs and other organs. A number of studies have shown an increased oxidant burden and con-sequently increased markers of oxidative stress in the air-spaces, breath, blood and urine in patients with COPD. The presence of oxidative stress has important conse-quences for the pathogenesis of COPD. Excess reactive oxygen species (ROS) production is regarded as one of the causes of COPD, as it is known to damage tissues. As for antioxidants, there are various enzymes eliminating over-produced ROS. Superoxide dismutase (SOD) can be clas-sified into copper/zinc-SOD (CuZn-SOD), manganese-SOD (Mn-SOD) and iron-SOD (Fe-SOD), depending on differences in metals that are necessary for the activity. Trace elements such as Zn, Se, Mn, Cu and Fe are consid-ered to be essential for living organisms, and their supple-mentation effectively suppresses oxidative stress, inflam-mation and fibrosis, suggesting that the essential elements can potentially be used as therapeutic agents in the treat-ment of pulmonary inflammatory diseases. Trace elements concentrations in COPD patients are related to the role of each of the elements in the immune system.

• MeSH
• chronická obstrukční plicní nemoc * terapie   MeSH
• klinická studie jako téma MeSH
• lidé MeSH
• mangan analýza   krev   terapeutické užití   MeSH
• měď analýza   krev   terapeutické užití   MeSH
• selen analýza   krev   terapeutické užití   MeSH
• stopové prvky analýza   krev   terapeutické užití   MeSH
• zinek analýza   krev   terapeutické užití   MeSH
• Check Tag
• lidé MeSH

• MeSH
• chromatografie kapalinová MeSH
• hmotnostní spektrometrie MeSH

• Konspekt
• Farmacie. Farmakologie
• NLK Obory
• farmacie a farmakologie
• NLK Publikační typ
• učebnice vysokých škol