Wyniki wyszukiwania - BazTech

1

Nowe podejście w izolowaniu i identyfikacji związków psychoaktywnych (dopalaczy) w materiale biologicznym

Musiał Jadwiga, Czarny Jakub, Powierska-Czarny Jolanta, Raczkowski Michał, Galant Natalia, Buszewski Bogusław, Gadzała-Kopciuch Renata

Wiadomości Chemiczne

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2025

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[Z] 79, 11-12

1221--1237

EN

To address the challenges facing toxicology laboratories and law enforcement agencies related to the need to rapidly identify psychoactive substances, particularly new psychoactive substances (NPS), commonly known as legal highs, in biological materials (blood, urine, and hair) to enable appropriate treatment to save the patient's health or life. To support timely medical intervention and facilitate the inclusion of emerging NPS on prohibited-substance lists, we developed and validated highthroughput analytical methods using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). These methods enable the simultaneous detection of more than 500 psychoactive compounds, drugs, and metabolites in blood, urine, and hair within 30 minutes. Because NPS often include numerous isomers and structurally similar compounds, chromatographic separation was optimized by monitoring selected pairs of multiple-reaction monitoring (MRM) transitions for each analyte. Careful optimization of mass-spectrometer parameters and MRM selection ensured unambiguous identification. Sample preparation employed both liquid-liquid and solid-liquid extraction, and calibration curves were prepared in matrix with finalstage dilution to minimize matrix effects and enhance analyte recovery. The validated methods allow parallel analysis of multiple biological matrices from a single patient, supporting studies of NPS metabolism and retrospective ingestion assessment. They have successfully passed proficiency testing, are implemented for routine casework at the Institute of Forensic Genetics in Bydgoszcz, accredited by the Polish Center for Accreditation, and are the subject of a pending patent application.

2

Structural and surface characterization of adsorbents applied in liquid chromatography

Lech-Przywara Regina, Galek Tomasz, Przywara Mateusz, Zapała Lidia, Zapała Wojciech

Advances in Science and Technology. Research Journal

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2025

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Vol. 19, no. 9

292--309

EN

A detailed analysis of the four commercial stationary phases often applied in liquid chromatography was performed using the following: SEM-EDS techniques and specific surface area and porosity analysis methods (multipoint BET, BJH, DH and DFT). The SEM-EDS results confirmed that the main component of all adsorbents examined is silica (SiO₂), while differences in oxygen content indicate varied approaches to surface modification, ranging from the strongly hydrophilic phase of TSK Gel Amide-80 to the hydrophobic Nucleodur C18 Gravity. Besides, the presence of trace amounts of metals may influence the additional analyte-adsorbent interaction of different nature. A comparison of specific adsorbent surface area data obtained using the multipoint BET method with the manufacturers values revealed significant discrepancies in the cases of TSK Gel Amide 80 and Nucleodur C18 Gravity, which may be the result of differences in pore accessibility and measurement methods. However, the Eurospher II 100-5 HILIC and Purospher STAR NH₂ phases showed good agreement with the manufacturers data. The porous structure of the phase studied shows significant differences: TSK Gel Amide 80 is characterized by mesopores with a uniform distribution, which favor the retention of larger molecules; Eurospher II 100-5 HILIC is microporous and selective for small, polar analytes; Nucleodur C18 Gravity has a structure typical of reversed phase materials; and Purospher STAR NH₂ exhibits the highest porosity, which favors the retention of large molecules, although it can also lead to the retention of undesirable analytes.

3

Analysis of selected factors influencing the course of the process in liquid chromatography

Lech-Przywara Regina, Zapała Wojciech

Advances in Science and Technology. Research Journal

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2025

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Vol. 19, no. 6

1--16

EN

This study examines the influence of temperature, eluent modifier type and concentration, and mobile phase flow velocity on the separation efficiency of caffeine (CAF) and phenol (PH) in Hypersil GOLD HILIC and Shodex SILICA 5NH 4D chromatographic columns. A thermodynamic analysis demonstrated that the adsorption processes of these compounds are primarily exothermic and depending on the eluent type. Acetonitrile-water (ACN:H₂O) systems provided superior selectivity between caffeine and phenol compared to methanol-water (MeOH:H₂O) systems, with selectivity improving as temperature increased in ACN:H₂O systems. Variations in eluent modifier concentration significantly impacted retention times, suggesting diverse interaction mechanisms between the analyzed compounds and the stationary phase. Furthermore, studies on column efficiency indicated that faster eluent flow reduced separation efficiency, as evidenced by HETP values. The optimal flow rates were determined to range between 0.2 and 1.25 ml/min, depending on the column tested.

4

Zjawiska międzyfazowe – 80 lat badań. Część 1., Adsorpcja i chromatografia cieczowa

Deryło-Marczewska Anna, Malinowska Irena, Goworek Jacek

Wiadomości Chemiczne

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2024

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[Z] 78, 9-10

1177--1221

EN

The paper presents the development of research on adsorption processes and thin-layer chromatography in the Department of Physical Chemistry of Maria Curie-Sklodowska University. The studies on chromatography and adsorption were initiated by prof. Andrzej Waksmundzki and his student prof. Jarosław Ościk at the turn of the 1940s and 1950s. Experimental studies in the area of adsorption included adsorption systems such as adsorbent – solutions of non-electrolytes in the entire concentration range, adsorbent – single- and multi-component diluted solutions, and measurements of adsorption equilibrium and kinetics. Methods for the synthesis and modification of various types of materials (silicas, carbons, clays, polymers, composites, nanomaterials) and methods for characterizing the structural and surface properties of adsorbents were developed, and a very effective method for measuring adsorption kinetics was developed. Experimental adsorption data, isotherms and concentration profiles, were analysed using various models and equations.

5

Metoda oznaczania kwasu cyjanurowego (1,3,5-triazinano-2,4,6-trionu; 1,3,5-triazyno-2,4,6-triolu) w powietrzu na stanowiskach pracy

Kowalska Joanna, Szewczyńska Małgorzata

Podstawy i Metody Oceny Środowiska Pracy

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2024

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Nr 2 (120)

131-142

PL

W artykule przedstawiono i omówiono wyniki oznaczania kwasu cyjanurowego (CYA) w powietrzu na stanowiskach pracy. Pobieranie próbek powietrza polega na zatrzymaniu obecnej w powietrzu substancji na filtrze z poli(chlorku winylu). Po wymyciu zatrzymanej substancji mieszaniną metanolu z buforem fosforanowym analizuje się otrzymane roztwory techniką chromatografii cieczowej z detekcją spektrofotometryczną. Najmniejsze stężenie frakcji wdychalnej kwasu cyjanurowego, jakie można oznaczyć przedstawioną metodą, wynosi 1 mg/m3 (dla próbki powietrza o objętości 120 l). Zakres tematyczny artykułu obejmuje zagadnienia zdrowia oraz bezpieczeństwa i higieny środowiska pracy będące przedmiotem badań z zakresu nauk o zdrowiu oraz inżynierii środowiska.

EN

The article presents and discusses the results of determining cyanuric acid (CYA) in the air at workplaces. Air sampling consists of trapping the substance present in the air on a poly(vinyl chloride) filter. After elution of the trapped substance with a mixture of methanol and phosphate buffer, the obtained solutions are analysed by liquid chromatography with spectrophotometric detection. The lowest concentration of the inhalable fraction of CYA that can be determined is 1 mg/m,3 (for an air sample of 120 l). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.

6

Możliwości wykorzystania mobilnych urządzeń do analiz chromatograficznych

Sok Paulina

Laboratorium - Przegląd Ogólnopolski

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2024

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nr 3

61--65

PL

Przenośne systemy chromatograficzne odgrywają kluczową rolę w różnych gałęziach przemysłu, szczególnie w ochronie środowiska oraz kontroli jakości farmaceutycznej. Elastyczność, kompatybilność oraz możliwość transportu sprawiają, że urządzenia te doskonale sprawdzają się w przypadku konieczności wykonania szybkich analiz terenowych oraz testów mobilnych. W niniejszym artykule przytoczono zagadnienia dotyczące mobilnej chromatografii gazowej, cieczowej, a także wspomniano krótko o chromatografii jonowej. Ponadto zostały zaprezentowane wybrane rozwiązania techniczne oraz aparaturowe umożliwiające wykonanie analizy w czasie rzeczywistym.

EN

Portable chromotography plays a key role in o variety of industries, particularly in environmental protection and pharmaceutical quality control. Flexibility, compatibility and transportability make these devices excellent for rapid field analysis and mobile testing. In this article, the issues of gas and liquid portable chromatography are mentioned, and portable ion chromatography is briefly outlined. Moreover, selected technical and equipment solutions for real-time analysis are presented.

7

Validation of the rapid and simple LC-MS/MS method for the quantification of pregabalin in plasma of acutely poisoned patients

Antunovic Marko, Dzudovic Jelena, Kilibarda Vesna, Vucinic Slavica, Djordjevic Snezana

Acta Chromatographica

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2024

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Vol. 36, no. 2

106--113

EN

Pregabalin is a gabapentinoid approved for the treatment of general anxiety disorder, neuropathic pain and as adjunctive therapy for focal seizures in patients with epilepsy. In addition, there are a number of conditions for which pregabalin is prescribed off-label. Along with the widespread use there are a significant number of reports describing the misuse of pregabalin over the last decade. Over time, it became clear that pregabalin should become part of routine testing in toxicology laboratories. The aim of this paper was to present validation of a LC-MS/MS method for the quantification of pregabalin in plasma of acutely poisoned patients. Simple sample preparation step and rapid chromatographic separation shortened the overall analysis time, which was the goal of method development. The presence of pregabalin was confirmed with three ion transitions, ensuring high selectivity of the validated method. The statistical data obtained showed good precision and accuracy over a wide concentration range. No endogenous or other interference was detected, and there was no matrix effect influence with this method. The LC-MS/MS method was applied to quantify pregabalin in plasma samples of patients admitted to the emergency department due to a possible acute pregabalin overdose. Different concentrations were found, and we report, to the best of our knowledge, the highest plasma concentration of pregabalin in the plasma of a patient with acute poisoning. In conclusion, we developed a fast and simple LC-MS/MS method for reliable determination of pregabalin and demonstrated the developed method was suitable for routine use in clinical toxicology setting.

8

Kwas benzoesowy. Metoda oznaczania w powietrzu na stanowiskach pracy

Szewczyńska Małgorzata, Wasilewski Paweł

Podstawy i Metody Oceny Środowiska Pracy

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2023

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Nr 3 (117)

137-154

PL

Kwas benzoesowy jest organicznym związkiem należącym do grupy aromatycznych kwasów karboksylowych. Wykorzystuje się go głównie do produkcji fenolu, kaprolaktamu i soli benzoesowych, jako konserwant spożywczy i farmaceutyczny oraz przy produkcji herbicydów, środków owadobójczych i bakteriobójczych. Zgodnie z rozporządzeniem Parlamentu Europejskiego i Rady (WE 1272/2008) kwas benzoesowy został sklasyfikowany jako substancja działająca szkodliwie na płuca, drażniąca skórę i powodująca uszkodzenie oczu. Celem badań było opracowanie metody oznaczania kwasu benzoesowego do oceny narażenia zawodowego w zakresie 1/10 ÷ 2 zaproponowanej wartości NDS. Metoda polega na pobraniu frakcji wdychalnej kwasu benzoesowego zawartej w powietrzu na filtr z włókna szklanego pokryty węglanem(IV) sodu, desorpcji roztworem metanolu w wodzie, a następnie oznaczeniu zawartości kwasu benzoesowego w próbce z zastosowaniem chromatografii cieczowej z detektorem diodowym (UHPLC-DAD). Podczas wykonywania badań spełniono wymagania walidacyjne przedstawione w normie europejskiej PN-EN 482. Metoda umożliwia oznaczanie kwasu benzoesowego w powietrzu w stężeniach 0,05 ÷ 1 mg/m3. Zakres tematyczny artykułu obejmuje zagadnienia zdrowia oraz bezpieczeństwa i higieny środowiska pracy będące przedmiotem badań z zakresu nauk o zdrowiu oraz inżynierii środowiska.

EN

Benzoic acid is an organic compound that belongs to the group of aromatic carboxylic acids. It is mainly used in the production of phenol, caprolactam and benzoic salts, as a food and pharmaceutical preservative, and in the production of herbicides, insecticides and bactericides. According to the Regulation of the European Parliament and of the Council (WE 1272/2008), benzoic acid is classified as a substance that is harmful to the lungs, irritates the skin and causes eye damage. The aim of the study was to develop a method for the determination of benzoic acid for the assessment of occupational exposure within 1/10–2 of the proposed MAC value. The method involves taking the inhalable fraction of airborne benzoic acid onto a glass fiber filter coated with sodium carbonate(IV), desorption with a solution of methanol in water and then determining the benzoic acid content of the sample by the use of liquid chromatography with diode array detector (UHPLC-DAD). Validation requirements presented in European standard PN-EN 482 were fulfilled during the tests. The method enables determination of benzoic acid in air at concentrations of 0.05 to 1 mg/m3 . The method for determining benzoic acid has been recorded in the form of an analytical procedure (see Appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.

9

Zastosowanie chromatografii cieczowej do oznaczania antybiotyków aminoglikozydowych – główne strategie i wyzwania

Glinka Marta, Wasik Andrzej

Analityka : nauka i praktyka

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2023

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nr 3

24--31

PL

Artykuł opracowany na podstawie rozprawy doktorskiej dr inż. Marty Glinki pt.: Application of liquid chromatography for the determination of aminoglycoside antibiotics and the deve-lopment of polymer-based drug delivery systems for their controlled release nagrodzonej przez Komitet Chemii Analitycznej PAN 2023 roku w konkursie na najleosze prace doktorskie. Nagroda ufundowana przez firmę Perlan Technologies.

10

Elektrochemiczna symulacja metabolizmu leków psychotropowych z zastosowaniem chromatografii cieczowej i spektrometrii mas

Podgrudna Paulina, Goldner Valentin, Karst Uwe, Szultka-Młyńska Małgorzata

Analityka : nauka i praktyka

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2023

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nr 2

4--9

PL

Połączenie EC/MS znajduje szerokie zastosowanie w takich dziedzinach nauki, jak toksykologia czy kryminalistyka, między innymi w analizie dopingowej do przewidywania potencjalnych ludzkich metabolitów nielegalnych substancji. Jest to obiecująca metoda w analizie środowiskowej syntezie na skalę preparatywną ,charakterystyce cząsteczek docelowych, a także do syntezy docelowej metabolitów, adduktów DNA lub protein.

11

Analiza triklosanu i jego metabolitu izolowanego z moczu za pomocą ultrawysokosprawnej chromatografii cieczowej

Gembicka Karolina, Buszewski Bogusław, Gadzała-Kopciuch Renata

Analityka : nauka i praktyka

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2023

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nr 2

16--21

PL

Prowadzone badania opierały się na doborze selektywnej metody izolowania triklosanu i jego metabolitu z matrycy biologicznej oraz na analizie jakościowej i ilościowej z wykorzystaniem wysokosprawnej chromatografii cieczowej z detektorem spektrofometrycznym.

12

A new simple liquid chromatographic assay for gentamicin in presence of methylparaben and propylparaben

Ivković Branka, Milutinović Ivana, Čudina Olivera, Marković Bojan

Acta Chromatographica

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2023

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Vol. 35, no. 1

81--87

EN

Gentamicin sulfate is a potent broad spectrum aminoglycoside antibiotic which is used against Gram-positive and Gram-negative bacteria. A simple, isocratic HPLC method for separation, identification and determination of gentamicin and parabens (methylparaben and propylparaben) was developed and validated. To our knowledge there is no report about simultaneous determination of those three analytes in pharmaceutical products. The optimum chromatographic conditions were achieved on CN column with a mobile phase consisting of 0.15% triethylamine in 10 mM KH₂PO₄ aqueous solution (final pH 3.0 adjusted with H₃PO₄) and methanol in the ratio 70:30 (v/v), providing selective quantification of analytes within 5 min. The method was successfully validated according to ICH guidelines acceptance criteria in terms of selectivity, linearity, accuracy, precision and robustness. The linearity of the method was proved in defined concentrations ranges for gentamicin (0.32–1.04 mg mL⁻¹), methylparaben (0.0072–0.0234 mg mL⁻¹) and propylparaben (0.0008–0.0026 mg mL⁻¹). Relative standard deviations calculated for all analytes in precision testing were <2% (analysis repeatability) and <3% (intermediate precision). Recovery values were between 98.87% and 101.67%. Chromatographic parameters are not significantly influenced by small variations of column temperature, pH and molarity of KH₂PO₄. Finally, the method was successfully applied for quantitative determination of gentamicin and parabens in commercially available solution for injection. Proposed HPLC method is found to be promising in terms of simplicity, analysis times and non-use of derivatization and ion-pair agents.

13

The Sensitive Method of Determination of Hazardous Phthlates in Polymeric Building Materials by High Performance Liquid Chromatography

Kaniowska Elżbieta, Kaczmarczyk Grzegorz

Rocznik Ochrona Środowiska

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2022

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Tom 24

190--201

EN

Polymeric building materials and equipment for indoor use in spaces intended for people may, in an essential way, contribute to the deterioration of wholesome quality of life. Phthalates, present in many products, constitute an omnipresent group of compounds used widely as plasticisers. The research results show that these substances may negatively impact human health, and thus European Union has implemented several regulatory measures restricting their use. Manufacturers and suppliers must comply with these regulations. As a result, it is necessary to investigate and determine the contents of phthalates in these materials. This paper presents the analytic profile of the method of marking phthalates extracted from polyvinyl chloride using HPLC chromatography with UV-VIS detection and selected results obtained in examinations of materials used in interior design. The results of described examinations of phthalates content indicate that not all materials recommended by manufacturers may be used indoors in spaces intended for people. The method was verified for its suitability for routine analyses of materials made of PVC and submitted for attestation. The elaborated method can be used to determine the banned phthalates’ presence in PVC. The method allows for detecting these phthalates at the level required by the REACH regulation, and its validation parameters are highly satisfactory considering a very complex matrix.

14

Zastosowanie chromatografii gazowej i cieczowej w badaniach produktów ciekłych pirolizy mikrofalowej

Burnus Zygmunt, Markowski Jarosław

Nafta-Gaz

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2022

|

R. 78, nr 1

64--79

PL

W niniejszej pracy zbadano możliwości wykorzystania technik chromatografii gazowej GC-FID oraz GC-MS wspomaganych klasyczną chromatografią cieczową LC do badania składników biooleju pochodzącego z pirolizy biomasy stałej. Badania biomasy i produktów jej przerobu mają na celu rozwój technologii paliw proekologicznych i/lub zawierających frakcje otrzymywane z biomasy lub surowców odpadowych. Celem tych działań jest stopniowe zwiększanie wykorzystania źródeł energii pochodzących z surowców odnawialnych przy jednoczesnym ograniczaniu zastosowania surowców kopalnych. Jest to jedno z działań, których efektem ma być ograniczenie emisji GHG. Działanie to jest związane z wytycznymi dyrektyw Unii Europejskiej nakazujących wzrost udziału odnawialnych źródeł energii w transporcie oraz energetyce. Są to dyrektywy 2003/30/WE oraz 2009/28/WE, dotyczące promowania użycia biopaliw lub innych paliw odnawialnych w transporcie oraz wzrostu udziału pozyskiwania energii ze źródeł odnawialnych w różnych sektorach krajów Wspólnoty Europejskiej. Energetyczne wykorzystanie biomasy to jeden z głównych obszarów zainteresowania polityki energetycznej Polski, zbieżnej z celami polityki wyznaczonymi przez Unię Europejską. W niniejszym artykule dokonano przeglądu literatury w zakresie rodzajów biomasy występującej w Polsce oraz zastosowania technik chromatografii gazowej i cieczowej (Py-GC, GC-MS, GC-FID) w badaniu ciekłych produktów procesu pirolizy biomasy. Opracowano warunki chromatograficzne badania produktów ciekłych pirolizy biomasy stałej przy wykorzystaniu reaktora mikrofalowego do pirolizy jako elementu aparatury umożliwiającego badania technikami chromatograficznymi. Przy zastosowaniu dobranych warunków analitycznych wykonano badania ciekłych produktów pirolizy biomasy: miskantu olbrzymiego, słomy, trocin sosnowych, łusek słonecznika i ziaren kawy. Zidentyfikowano składniki biooleju pochodzącego z pirolizy biomasy i zaproponowano metodę oznaczania ilościowego składników biooleju. Wykazano możliwość jednoczesnego zastosowania różnych technik chromatografii gazowej w celu poznania składu chemicznego biooleju pochodzącego z pirolizy mikrofalowej różnego rodzaju biomasy stałej.

EN

In this work, the possibilities of implementation of the GC-FID and GC-MS gas chromatography techniques supported by classic LC liquid chromatography to study the components of bio-oil derived from the pyrolysis of solid biomass were examined. Research on biomass and its processing products is aimed at the development of pro-ecological fuels and / or fuels containing fractions obtained from biomass or waste materials. The aim of these activities is to gradually increase the use of energy sources derived from renewable raw materials and limiting the use of fossil raw materials. It is one of the ways to reduce GHG emissions. This action is related to the guidelines of the European Union Directives describing an increase in the share of renewable energy sources in transport and energy – Directives 2003/30/EC and 2009/28/EC – the promotion of the use of biofuels or other renewable fuels in transport and the increase in the share of energy obtained from renewable sources in various sectors of the European Community. The use of energy obtained from biomass is one of the main areas of interest in Poland's energy policy, consistent with the policy objectives set by the European Union. This article describes the types of biomass found in Poland and the use of gas and liquid chromatography techniques (Py-GC, GC-MS, GC-FID) in the study of liquid products of the biomass pyrolysis process. The chromatographic conditions for testing liquid products of solid biomass pyrolysis with the use of a microwave pyrolysis reactor as an element of the apparatus enabling the research with chromatographic techniques were developed. Using selected analytical conditions, tests were carried out on liquid products of biomass pyrolysis: giant miscanthus, straw, pine sawdust, sunflower husks and coffee grounds. The components of bio-oil derived from biomass pyrolysis were identified and a method for the quantification of bio-oil components was proposed. The possibility of the simultaneous application of various gas chromatography techniques to understand the chemical composition of bio-oil from microwave pyrolysis of various types of solid biomass was demonstrated.

15

The Effect of an Accidental Carrier Rocket Crash on Soil and Vegetation Cover

Maikanov Balgabay S., Auteleyeva Laura T., Zhubatov Zhailaubay K., Terlikbayev Askar A., Kamsaev Kanat M.

Journal of Ecological Engineering

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2022

|

Vol. 23, nr 2

176--184

EN

The dynamics of the consequences of the Proton-M carrier rocket crash on the soil and vegetation cover in the area where its parts fell were studied in 2007-2014. Analytical methods such as liquid chromatography with electrochemical and spectrophotometric detection were used. In 2007, four soil detoxifications were performed. A second study in 2009 showed a sharp increase in the area of contamination of plants by UDMH (unsymmetrical dimethylhydrazine) and NDMA (N-Nitrosodimethylamine). In 2010, the situation shifted in the opposite direction. Toxicants in plants were absent for three years (2010-2012) but reappeared in 2013 and 2014. The accidental crash of the Proton-M carrier rocket led to the destruction of the soil and vegetation cover, ignition of vegetation, and soil contamination. In the area where the rocket parts fell, the UDMH content in the soil was 1.4–5,200 times higher than the threshold limit value. The fall of the carrier rocket increased the area of soil contamination with UDMH to 3,600 m2, with NDMA to 917 m2, and with nitrate ions to 8,314 m2. The reappearance of heptyl and nitrous compounds in plants and soil was detected four years after repeated detoxification of the soil.

16

Chromatografia nadkrytyczna w przemyśle farmaceutycznym

Fularczyk Tymoteusz, Bulska Ewa

Analityka : nauka i praktyka

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2022

|

nr 2

40--46

PL

Odkrycie kolejnego stanu skupienia, czyli cieczy w stanie nadkrytycznym, pozwoliło na rozwój nowej techniki chromatograficznej (chromatografia nadkrytyczna). Dzięki szczególnym właściwościom cieczy w stanie nadkrytycznym możliwe stało się opracowanie techniki łączącej zalety chromatografii gazowej i wysokosprawnej chromatografii cieczowej.

17

Liquid chromatographic enantioseparation, determination, bioassay and isolation of enantiomers of Ketorolac : a review

Bhushan Ravi

Acta Chromatographica

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2022

|

Vol. 34, no. 3

220--236

EN

Ketorolac (Ket) is a potent non-narcotic analgesic drug (among the nonsteroidal anti-inflammatory drugs). The physiological activity of Ket resides with (S)-(-)-Ket while the drug is marketed and administered as a racemic mixture. Therefore, it is desirable that the pharmacokinetics is measured and quantified for enantiomers individually and not as a total drug. The present paper is focused on relevant literature on LC enantioseparation of (RS)-Ket along with bioassay, pharmacokinetic and clinical studiem within the discipline of analytical chemistry. HPLC and Thin layer chromatography (TLC) methods using both direct and indirect approaches are discussed. The methods provide chirality recognition even in the absence of pure enantiomers. Besides, a brief discussion on resolution by crystallization and enzymatic methods is included. The most interesting aspects include establishment of structure and molecular asymmetry of diastereomeric derivatives using LC-MS, proton nuclear magnetic resonance spectrometry, and by drawing conformations in three dimensional views by using certain software. A brief discussion has also been provided on the recovery of native enantiomers by TLC.

18

Development of a simple HPLC procedure for the determination of prochloraz residues in mushrooms

Csutoras Csaba, Misz Andras, Nagy-Koteles Csaba, Bakos-Barczi Nora, Racz Laszlo

Acta Chromatographica

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2022

|

Vol. 34, no. 3

373--375

EN

A simple HPLC-UV procedure is described in our paper which is suitable for the rapid and cost-efficient determination of prochloraz in mushrooms. Prochloraz is the only fungicide in EU which use is allowed in mushroom production. The aim of our work was the development of a simple method that is suitable for the control of this pesticide in everyday analyses during mushroom production. The procedure involves a simple sample preparation method based on solid-liquid extraction (modified QuEChERS extraction method EN 15662) followed by an HPLC-UV determination (recovery: 97–99%; limit of detection LOD: 0.01 mg/kg; limit of quantification LOQ: 0.05 mg/kg).

19

Nowe kierunki badań i wyzwania w analizie leków heparynowych

Sadowski Radosław, Krysztofiak Dominika, Gadzała-Kopciuch Renata, Buszewski Bogusław

Wiadomości Chemiczne

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2021

|

[Z] 75, 7-8

935--942

EN

The complexity of the structure of heparin anticoagulants requires appropriate sample preparation to be able to perform the analysis correctly. This stage of the analytical procedure is the most time-consuming and has a key impact on the obtained information. Therefore, it is important to improve the current and search for new solutions for the preparation of samples of anticoagulants as well as the separation and identification of components of such drugs. This paper discusses heparin drugs and new research directions and challenges related to the analytics of heparin anticoagulants.

20

Opracowanie metody oznaczania tetrabromobisfenolu A (TBBPA) z wykorzystaniem chromatografii gazowej sprzężonej ze spektrometrią mas (GC-MS) oraz chromatografii cieczowej z detektorem diodowym (LC-DAD)

Szyposzyńska Monika, Spławska Aleksandra, Mirosz Danuta, Stela Maksymilian

Przemysł Chemiczny

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2021

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T. 100, nr 12

1203--1206

PL

Przedstawiono metodę oznaczania TBBPA za pomocą chromatografii gazowej sprzężonej ze spektrometrią mas oraz chromatografii cieczowej sprzężonej z detektorem diodowym. Analizy za pomocą GC-MS przeprowadzono w kolumnie HP-5MS. Zaobserwowano satysfakcjonującą liniowość w zakresie stężeń 10-250 μg/mL. Granica wykrywalności wynosiła 10 μg/mL. Analizę z wykorzystaniem LC-DAD przeprowadzono, stosując jako fazę ruchomą mieszaninę metanol-woda (80:20% obj.), przy długości fali 206 nm i prędkości przepływu fazy ruchomej 1 mL/min. Granice wykrywalności i oznaczalności wynosiły odpowiednio: 0,12 μg/mL i 3,7 μg/mL.

EN

TBBPA assay was performed by GC-MS after derivatization with CF₃C[=NSi(CH₃)₃]OSi(CH₃)₃. GC-MS anal. were performed on HP-5MS column. The method showed a satisfactory linearity in the concn. range of 10-250 μg/mL. LC anal. was performed by measuring the absorbance at 206 nm and using water-MeOH mixt. (80:20 v/v) as mobile phase with a flow rate of 1 mL/min. The detection limits were 10 and 0.12 μg/mL for the GC-MS and LC methods, resp.