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Search results for: LC-MS/MS
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Electrochemistry/mass spectrometry (EC/MS) for fast generation and identification of novel reactive metabolites of two unsymmetrical bisacridines with anticancer activity.
PublicationThe development of a new drug requires knowledge about its metabolic fate in a living organism, regarding the comprehensive assessment of both drug therapeutic activity and toxicity profiles. Electrochemistry (EC) coupled with mass spectrometry (MS) is an efficient tool for predicting the phase I metabolism of redox-sensitive drugs. In particular, EC/MS represents a clear advantage for the generation of reactive drug transformation...
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The use of HPLC-Q-TOF-MS for comprehensive screening of drugs and psychoactive substances in hair samples and several “legal highs” products
PublicationNon-targeted screening of drugs present in herbal products, known as “legal high” drugs and in hair as a biological matrix commonly used in toxicological investigations was accomplished with the use of high pressure liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-Q-TOF-MS). In total, 25 and 14 therapeutical drugs and psychoactive substances/metabolites were detected in investigated hair samples...
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Miniaturized, green salting-out liquid–liquid microextraction coupled with GC–MS used to evaluate biogenic amines in wine samples
PublicationMonitoring of the biogenic amines (BAs) content in food products, including wine, is important due to the health and safety of consumers and from the quality control point of view. In a given study, simultaneous derivatization and salting-out liquid–liquid microextraction (SALLME) coupled with GC–MS for BAs determination from wine samples was developed. For the optimization the Box-Behnken design was applied, where three independent...
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The potential role of fatty acids in prostate cancer determined by GC–MS analysis of formalin-fixed paraffin-embedded tissue samples
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Dynamics of hepatitis B virus quasispecies heterogeneity in association with nucleos(t)ide analogue treatment determined by MALDI-TOF MS
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Simultaneous determination of individual isothiocyanates in plant samples by HPLC-DAD-MS following SPE and derivatization with N-acetyl-l-cysteine
PublicationThe procedure for the isothiocyanates (ITCs) determination that involves derivatization with N-acetyl-l-cysteine (NAC) and separation by HPLC was developed. Prior to derivatization, plant ITCs were isolated and purified using solid-phase extraction (SPE). The optimum conditions of derivatization are: 500 μL of isopropanolic eluate obtained by SPE combined with 500 μL of derivatizing reagent (0.2 M NAC and 0.2 M NaHCO3 in water)...
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Method for the simultaneous determination of monoaromatic and polycyclic aromatic hydrocarbons in industrial effluents using dispersive liquid-liquid microextraction with GC-MS
PublicationWe present a new method for simultaneous determination of 22 monoaromatic and polycyclic aromatic hydrocarbons in postoxidative effluents from the production of petroleum bitumen using dispersive liquid-liquid microextraction coupled to gas chromatography and mass spectrometry. The eight extraction parameters including the type and volume of extraction and disperser solvent, pH, salting out effect, extraction and centrifugation...
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Simultaneous determination of ibuprofen and its metabolites in complex equine urine matrices by GC-EI-MS in excretion study in view of doping control
PublicationA novel assay for the simultaneous determination of ibuprofen (IBU) and its four probable metabolites, 1-hydroxyibuprofen (1-OH IBU), 2-hydroxyibuprofen (2-OH IBU), 3-hydroxyibuprofen (3-OH IBU) and carboxyibuprofen (CBX IBU) in equine urine samples with the application of Gas Chromatography-Electron Ionization-Mass Spectrometry (GC-EI-MS) has been developed and elaborated. The new approach for sample preparation including minimizing...
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Study of effect of phosphate and uranium ions on the thermal properties of surfactant-modified natural red clay using TG–FTIR–MS techniques
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Identyfikacja lotnych składników ścieków z instalacji oksydacji asfaltów z wykorzystaniem chromatografii gazowej sprzężonej ze spektrometrią mas (GC-MS)
PublicationW pracy przedstawiono wyniki badań nad identyfikacją lotnych związków organicznych występujących w ściekach z instalacji oksydacji asfaltów. Ścieki poddano deemulgacji, w celu usunięcia fazy organicznej, a następnie ekstrakcji dichlorometanem, w celu wyizolowania pozostałych w ściekach związków organicznych. Zidentyfikowano 30 związków organicznych oraz szereg n-alkanów, które pozostały w ściekach pomimo zastosowanej deemulgacji....
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Non-volatile molecular composition and discrimination of single grape white of chardonnay, riesling, sauvignon blanc and silvaner using untargeted GC–MS analysis
PublicationThis study developed and applied a GC–MS method aiming at molecular fingerprinting of 120 commercial single grape white wines (Chardonnay, Riesling, Sauvignon Blanc and Silvaner) for possible authentication according to grape variety. The method allowed detection of 372 peaks and tentative identification of 146 metabolites including alcohols, organic acids, esters, amino acids and sugars. The grape variety effect explained 8.3%...
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The use of RP-HPLC–Q-TOF–MS as a powerful tool for wastewater composition profiling and selection of water pollution marker specific to wastewater contamination
PublicationLimited drinking water resources and water pollution are one of the main worldwide problems. To reduce the consumption of fresh water resources, the use of treated wastewater has been proposed. The farmlands have been irrigated with wastewater for centuries, but the composition of used sewage has changed over the years. Recent research has revealed the presence of hundreds of new organic contaminants in many environmental waters,...
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Application of dynamic headspace and gas chromatography coupled to mass spectrometry (DHS-GC-MS) for the determination of oxygenated volatile organic compounds in refinery effluents
PublicationThe paper presents a new procedure for the determination of oxygenated volatile organic compounds (O-VOCs) in postoxidative effluents from the production of petroleum asphalt using dynamic headspace coupled to gas chromatography-mass spectrometry in the selected ion monitoring (SIM) mode (DHSGC-MS). Among the GC capillary columns tested, a polar SLB-IL111 column with the ionic liquid stationary phase was found to be superior due...
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Bezpośrednia analiza próbek z wykorzystaniem techniki spektrometrii mas. Cz. II. Technika PTR – MS – ciekawe rozwiązanie metodyczne w zakresie spektrometrii mas
PublicationTechnika spektrometrii mas stanowi niezwykle istotne narzędzie badawcze, umożliwiające uzyskanie wielu cennych informacji, dotyczących składu chemicznego wielu próbek rzeczywistych pochodzenia biologicznego, farmaceutycznego i spożywczego. Spektrometr mas zazwyczaj pełni role detektora w przypadku stosowania połączenia z urządzeniami chromatograficznymi (GC, LC). Dzięki zastosowaniu pewnych modyfikacji aparaturowych i metodycznych,...
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Determination of pharmaceutical residues in drinking water in Poland using a new SPE-GC-MS(SIM) method based on Speedisk extraction disks and DIMETRIS derivatization
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Direct-Ultrasonic Assisted Microextraction Coupled with RTL-GC-FID/GC-MS as a Future Standard Procedure for Monitoring 26 potentially Allergenic Fragrances in Water Samples
PublicationThis research topic grew up as a result of awareness of constant anthropogenic and natural input to the environment constituents of personal care products (PCPs) residues. This group of emerging pollutants encompasses a wide range of chemicals, including potentially allergenic fragrance compounds. The aim of the present study was to investigate presence of 26 fragrance allergens in water samples. Simple and rapid methodology based...
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Multi-residue method for the determination of 16 recently used pesticides from various chemical groups in aqueous samples by using DI - SPME coupled with GC-MS
PublicationA simple and solvent-free multi-residue method has been optimized to determine 16 currently used pesticides from different chemical groups in aqueous samples. The extraction of analytes was carried out with direct immersion solid-phase microextraction (DI-SPME) and for the identification and quantitative determination gas chromatography coupled with mass spectrometry (GC-MS) was applied. Two commonly used adsorbent coatings have...
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Phenolic composition and antioxidant properties of polish blue-berried honeysuckle genotypes by HPLC-DAD-MS, HPLC postcolumn derivatization with ABTS or FC, and TLC with DPPH visualization
PublicationIn this study, different Polish cultivars of blue-berried honeysuckles (Lonicera caerulea L.), wild and bog bilberry, were analyzed for bioactive compounds. The chemical properties verified included composition of anthocyanins and other polyphenols, antioxidant activity, and profiles of antioxidants by HPLC postcolumn derivatization or TLC. The antioxidant activities of different blue-berried honeysuckle cultivars were similar...
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Understanding the early-stage release of volatile organic compounds from rapeseed oil during deep-frying of tubers by targeted and omics-inspired approaches using PTR-MS and gas chromatography
PublicationDuring deep-frying, a plethora of volatile products is emitted with the fumes. These compounds could act as oil quality indicators and change the indoor air composition leading to health risks for occupants. The presented experiments focus on deep-frying of different tubers in rapeseed oil at different frying temperatures. Here, two scenarios for real-time monitoring of volatile organic compounds (VOCs) using proton transfer reaction...
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Can matrix solid phase dispersion (MSPD) be more simplified? Application of solventless MSPD sample preparation method for GC–MS and GC–FID analysis of plant essential oil components
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Wykorzystanie technik GC×GC-TOF-MS i olfaktometrii terenowej do oceny uciążliwości zapachowej powietrza atmosferycznego na obszarach przyległych do terenu składowiska odpadów komunalnych
PublicationUciążliwość zapachowa jest poważnym problemem środowiskowym i jednym z powodów skarg ludności dotyczących złej jakości powietrza atmosferycznego. Źródłem emisji nieprzyjemnych zapachów do środowiska (odorów) są obiekty gospodarki komunalnej, w tym składowiska odpadów komunalnych. Ze względu na negatywny wpływ emisji substancji zapachowych na zdrowie i życie człowieka, konieczne jest stosowanie odpowiednich narzędzi analitycznych...
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Characteristics of Cucumis metuliferus, Actinidia deliciosa and Musa paradisica fragrance profiles using a comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometric detection (GC×GC-TOF MS)
PublicationComprehensive two-dimensional gas chromatography with time-of-flight mass spectrometric detection (GC×GC-TOF-MS) is a modern analytical technique used in many fields. This technique enables an effective separation of volatile chemical compounds [1]. In recent years, the topic of healthy food and healthy living has become very popular. For this reason, more and more scientific publications related to the analysis of food products...
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Application of Headspace Solid-phase Microextraction with Poly(1-vinyl-3- Hexylimidazolium Chloride) Polymeric Ionic Liquid Coating using GC - MS to Determine Volatile Fatty Acids in Dairy Wastewater
PublicationVolatile fatty acids were determined in this study using headspace solid-phase microextraction (HS-SPME) with a poly(1-vinyl-3-hexylimidazolium chloride) polymeric ionic liquid coated fiber followed by gas chromatography - mass spectrometry. Experimental parameters such as extraction time and temperature, sample volume as well as desorption time and temperature were optimized. Detection limits of the method were in the range of...
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Badania emisji lotnych związków organicznych z asfaltów drogowych z wykorzystaniem techniki dynamicznej analizy fazy nadpowierzchniowej i chromatografii gazowej sprzężonej ze spektrometrią mas (DHS - GC - MS)
PublicationAsfalty drogowe pochodzenia naftowego są wytwarzane z pozostałości z destylacji próżniowej ropy naftowej. Ze względu na częciowy kraking termiczny mający miejsce na etapie destylacji próżniowej oraz jej utleniania (oksydacji) prowadzącego do powstania finalnegoproduktu, w gotowej masie bitumicznej występują lotne związki organiczne. Podczas dalszego wykorzystania asfaltu, na etapie jego ekspedycji oraz budowy dróg, z gorącej masy...
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Optymalizacja projektu montażu obiektu MS-4/B realizowanego w ramach zadania „Budowa drogi ekspresowej S7 na odc. Miłomłyn-Olsztynek, Pododcinek Ostróda Północ - Ostróda Południe, w ciągu drogi S7 wraz z budową obwodnicy Ostródy w ciągu DK 16 (Pododcinek "B")” wraz z uzgodnieniami z nadzorem autorskim i nadzorem naukowym
PublicationCelem opracowania jest przeprowadzenie optymalizacji projektu montażu obiektu MS-4/B realizowanego w ramach zadania „Budowa drogi ekspresowej S7 na odc. Miłomłyn-Olsztynek, Pododcinek Ostróda Północ - Ostróda Południe, w ciągu drogi S7 wraz z budową obwodnicy Ostródy w ciągu DK 16 (Pododcinek "B")” oraz uzgodnienie wprowadzonych zmian z Nadzorem Autorskim (NA).
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Determination of isoprostanes in exhaled breath condensate samples by liquid chromatography coupled with tandem mass spectrometry
PublicationOxidative stress (OS) is a state of imbalance between continuously generating reactive oxygen species (ROS) during normal cell metabolism and mechanism of detoxifying oxygen radicals through a network of antioxidative enzymes. Isoprostanes are prostaglandin -like substances that are produced in vivo primarily by free radical-induced peroxidation of arachidonic acid. The measurement of isoprostanes in biological fluids and/or tissue...
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Determination of hormones in water samples using liquid chromatography coupled with tandem mass spectrometry
PublicationOver the past few years, many synthetic (ethinylestradiol) and natural (estradiol,estriol, estrone) compounds present in the environment have been affecting the hormonalbalance of humans and animals. Steroid hormones are very often used for medical purposesand have high estrogenic activity what makes them endocrine disrupters. Most hormonalcompounds are released into the water as a result of their incomplete removal in wastewatertreatment...
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Comparison of Two Methods for the Determination of Selected Pesticides in Honey and Honeybee Samples
PublicationDeveloped and validated analytical methods for the determination of a wide spectrum of pesticide residues in honey and honeybee samples after the modification of QuEChERS extraction in combination with gas chromatography–tandem quadrupole mass spectrometry (GC-MS/MS) and liquid chromatography–tandem quadrupole mass spectrometry (LC-MS/MS) were discussed and compared. The developed methods were evaluated regarding the utilized equipment...
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Rapid ion-exchange matrix removal for a decrease of detection limits in the analysis of salt-rich reservoir waters for fluorobenzoic acids by liquid chromatography coupled with tandem mass spectrometry
PublicationA matrix removal procedure with ion-exchange resin prior to analysis for 18 fluorinated benzoic acids (FBAs) tracers in saline (>25% salt) reservoir water was optimized. The elimination of >98% of salt and the simultaneous matrix sample cleanup allowed the direct analysis using the supernatant by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). This resulted in a gain in detection limits for most of the tracers...
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Analysis of chiral pharmaceutical residues in influent and effluent samples at racemic and enantiomeric level using liquid chromatography-tandem mass spectrometry
PublicationIn this work, two different chromatographic methods for seasonal monitoring of pharmaceutical residue in wastewater samples were developed. In the case of enantiomeric separation of selected compounds, LC-MS technique combining with vancomycin based chiral stationary phase was used. The performance of chiral analysis enabled to monitor the pharmaceutical contamination at the enantiomeric level. The d-SPE procedure was developed...
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Troubleshooting of the determination of bisphenol A at ultra-trace levels by liquid chromatography and tandem mass spectrometry
PublicationDetermination of trace amounts of bisphenol A (BPA) may cause problems mainly related to the presence of BPA in solvents (even in LC-MS grade), laboratory vessels, and plastic equipment used for sample preparation. Variable and sometimes significant amounts of BPA present in the background cause problems in obtaining good repeatability of measurements at the ultra-trace levels. Such observations (i.e., poor repeatability of results)...
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Abuse or contamination? Ratio determination of clenbuterol enantiomers to distinguish between doping use and meat contamination
PublicationClenbuterol has been detected in urine of several athletes during routine doping control in the past years. Athletes claimed that the clenbuterol was ingested by eating contaminated meat. Providing analytical prove for this claim is difficult. clenbuterol consists of two enantiomers, R(-) and S(+)-clenbuterol. Currently available human and veterinary preparations were found to consist of a racemic mixture of both enantiomers. When...
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Sensitive simultaneous determination of 19 fluorobenzoic acids in saline waters by solid-phase extraction and liquid chromatography–tandem mass spectrometry
PublicationA solid-phase extraction (SPE) procedure using C18 stationary phase was optimized for the preconcentration of 19 fluorinated derivatives of benzoic acid (FBA): mono-, di-, tri-, and tetrafluorosubstituted in the ring, trifluoromethylbenzoic acid and 3,5-bistrifluoromethyl benzoic acid from undiluted salt-rich (>20%) reservoir waters. Quantitative (>90%) retention/elution of 16 out of 19 analyte compounds was achieved allowing a...
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Rapid Characterization of the Human Breast Milk Lipidome Using a Solid-Phase Microextraction and Liquid Chromatography-Mass Spectrometry-Based Approach.
PublicationHuman breast milk (HBM) is a biofluid consisting of various biomolecules such as proteins, lipids, carbohydrates, minerals and bioactive substances. Due to its unique and complex composition, HBM provides not only nutritional components required for the growth of the infant, but also additional protection against infections. Global insight into the composition of HBM is crucial to understanding the health benefits infants receive...
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Determination of Butyltin Species in Sea Water Samples Using Solid Phase Extraction Followed by Liquid Chromatography - Tandem Mass Spectrometry
PublicationReverse phase liquid chromatography (RP-HPLC)-electrospray ionization-tandem mass spectrometry (ESI-MS-MS) was evaluated for the analysis of TBT using solid phase extraction as sample preparation method. TBT was extracted from acidified water samples (spiked with tripropyltin as internal standard) using reversed phase polymeric Strata-X cartridges. Analytes were eluted from cartridges using acetonitrile-water mixture and the volume...
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Profiling of polar ionogenic metabolites in Polish wines by capillary electrophoresis-mass spectrometry
PublicationThe composition of wine is determined by a complex interaction between environmental factors, genetic factors (i.e., grape varieties), and winemaking practices (including technology and storage). Metabolomics using NMR spec-troscopy, GC-MS, and/or LC-MS has shown to be a useful approach for assessing the origin, authenticity, and quality of various wines. Nonetheless, the use of additional analytical techniques with complementary...
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Phototransformation of three selected pharmaceuticals, naproxen, 17α-Ethinylestradiol and tetracycline in water: Identification of photoproducts and transformation pathways
PublicationTransformation products (TPs) may be formed during various processes, however, it was proved that one of the main mechanisms responsible for degradation of pharmaceuticals in natural waters is photolysis. Three compounds were selected, tetracycline (TC), 17-α-ethinylestradiol (EE2) and naproxen (NAP), for degradation experiments which were performed using a xenon lamp emitting light with a spectrum closely approximating that of...
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Comparison of classical and modern approach of determination of highly polar compounds by High Performance Liquid Chromatography coupled with Tandem Mass Spectrometry
PublicationAbstract: Sugars and sugar alcohols are known as highly polar compounds. Four analytes were taken into consideration for comparison of classical and modern approach of separation of highly polar substances. Mannitol was chosen as an example of simple sugar alcohol, sucrose and lactulose as examples of disaccharides and structural isomers, raffinose as an example of complex trisaccharide. Raffinose was also used as internal standard...
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Determination of Glycerol, Propylene Glycol, and Nicotine as the Main Components in Refill Liquids for Electronic Cigarettes
PublicationRefill liquids for electronic cigarettes are an important area of research due to the health safety and quality control of such products. A method was developed for the determination of glycerol, propylene glycol, and nicotine in refill liquids using liquid chromatography, coupled with tandem mass spectrometry (LC-MS/MS) in multiple reaction monitoring (MRM) mode with electrospray ionisation (ESI). Sample preparation was based...
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Consequences of New Approach of Chemical Stability Tests of Active Pharmaceutical Ingredients (APIs)
PublicationThere is a great need of broaden look on stability tests of active pharmaceuticalingredients (APIs) in comparison with current requirements contained in pharmacopeia.By usage of many modern analytical methods the conception of monitoring the changesof APIs during initial stage of their exposure to harmful factors has been developed. Newknowledge must be acquired in terms of identification of each degradation...
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A new dilution-enrichment sample preparation strategy for expanded metabolome monitoring of human breast milk that overcomes the simultaneous presence of low- and high-abundance lipid species
PublicationThe complex nature of human breast milk (HBM) makes samples difficult to analyze, requiring several extraction techniques and analytical platforms to obtain high metabolome coverage. In this work, we combined liquid-liquid extraction (LLE) and solid-phase extraction (SPE) techniques to prepare HBM samples to overcome the challenge of low- and high-abundance lipid species, enabling the semiquantitative analysis of total HBM lipids...
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Pesticide residues levels in honey from apiaries located of Northern Poland
PublicationConcentration levels of 30 pesticide residues were measured in honey samples collected from apiaries in northern part of Poland (Pomerania) using method based on the QuEChERS extraction followed by liquid chromatography-tandem mass spectrometry with electron spray ionization (LC-ESI-MS/MS). In 29% of the samples were found positive for at least some of the target compounds. Concentration of bifenthrin, fenpyroximate, methidathion,...
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Pozostałości farmaceutyków w środowisku - problem daleki od rozwiązania
PublicationDo środowiska dostaje się coraz więcej związków pochodzenia farmaceutycznego. Zainteresowanie nimi tym bardziej wzrasta ze względu na ich niekorzystny wpływ nie tylko na środowisko, ale także na organizm ludzki. Mogą one powodować m.in. feminizację samców, wzrost odporności bakterii na antybiotyki oraz wzrost lekooporności ludzi. Dodatkowo farmaceutyki mogą przekształcać się w inne związki, których potencjał wywoływania efektów...
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Isolation of xanthone and benzophenone derivatives from Cyclopia genistoides (L.) Vent. (honeybush) and their pro-apoptotic activity on synoviocytes from patients with rheumatoid arthritis
PublicationA fast and efficient method for the isolation of the C-glucosidated xanthones mangiferin and isomangiferin from the South-African plant Cyclopia genistoides was developed for the first time. Two benzophenone derivatives: 3-C-β-glucosides of maclurin and iriflophenone, were isolated from C. genistoides extracts using semi-preparative. The structures of the compounds were determined by 1D and 2D NMR experiments and/or LC-DAD-ESI–MS.
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Comprehensive determination of flavouring additives and nicotine in e-cigarette refill solutions. Part II: Gas-chromatography–mass spectrometry analysis
PublicationFlavouring compounds are an essential part of e-liquid products for cigarettes. In general, they are regarded as safe for ingestion, but they may have unrecognized risks when they are inhaled. In some cases, manufactures do not currently abide by the Tobacco Products Directive (2014/40/EU) and do not declare the detailed contents of e-liquids on their labels. To help evaluate the health impact of flavouring substances, there is...
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Prediction of Overall In Vitro Microsomal Stability of Drug Candidates Based on Molecular Modeling and Support Vector Machines. Case Study of Novel Arylpiperazines Derivatives
PublicationOther than efficacy of interaction with the molecular target, metabolic stability is the primary factor responsible for the failure or success of a compound in the drug development pipeline. The ideal drug candidate should be stable enough to reach its therapeutic site of action. Despite many recent excellent achievements in the field of computational methods supporting drug metabolism studies, a well-recognized procedure to model...
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Determination of Pesticide Residues in Honeybees using Modified QUEChERS Sample Work-Up and Liquid Chromatography-Tandem Mass Spectrometry
PublicationIncreasing emissions of chemical compounds to the environment, especially of pesticides, is one of factors that may explain present honeybee colony losses. In this work, an analytical method employing liquid chromatography-tandem mass spectrometry (LC-MS/MS) was optimized for the simultaneous screening of 19 pesticides which have not been yet determined in honeybee samples from northern Poland (Pomerania). The sample preparation,...
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Bisphenols and their derivatives in baby diaper samples.
PublicationMany common products contain and leach hazardous chemicals, including endocrine-disrupting chemicals such as bisphenols that are harmful to human health. For toddlers, this dangerousness is higher because of their not fully developed detoxification system. Due to this, bisphenols content in products such as baby diapers, should be monitored. Baby diapers not only remain in close contact with the skin, but are also used from the...
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A study on the protection of methionine and the reduction of methionine sulfoxide in methionine-containing analogues of the growth-modeling factor Gly-His-Lys
PublicationThe protection of methionine and the reduction of methionine sulfoxide in methionine-containing analogues of Gly-His-Lys are described. The peptides were synthesized by a solid-phase method using the standard Fmoc procedure. Simultaneous deprotection of the peptide side chain and liberation from the resin were achieved using an appropriate TFA cocktail. The TFA cocktail was selected to minimize oxidation of the methionine residue....
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Degradation kinetics and mechanism of pentoxifylline by ultraviolet activated peroxydisulfate
PublicationDegradation of pentoxifylline (PTX) by sodium peroxydisulfate (SPDS) assisted by UV irradiation has been investigated in deionized water. The treatment was more favorable over direct photolysis or peroxydisulfate oxidation alone. The effects of various parameters, including different dosage of oxidant agent, PTX concentration, initial solution pH levels, and the presence of inorganic ions like chloride, nitrate and carbonate have...