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Forced degradation studies of ivabradine and in silico toxicology predictions for its new designated impurities
PublicationAll activities should aim to eliminate genotoxic impurities and/or protect the API againstdegradation. There is a necessity to monitor impurities from all classification groups,hence ivabradine forced degradation studies were performed. Ivabradine was provedto be quite durable active substance, but still new and with insufficient stability data.Increased temperature, acid, base, oxidation reagents and...
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Glucosinolates from lepidium peruvianum as potential antiamnestic drugs
PublicationLepidium peruvianum (maca) (Brassicaceae) is a naturally occurring plant mainly in the high Andes of Peru. In recent years, it has been intensively researched in terms of its influence on various diseases and towards health improvement. Alzheimer’s disease is an incurable disease that most often affects adults over the age of 60. As since 2003 the US Food and Drug Administration (FDA) did not approve any new drug for Alzheimer’s...
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5-Thiocyanato-2′-deoxyuridine as a possible radiosensitizer: electron-induced formation of uracil-C5-thiyl radical and its dimerization
PublicationIn this work, we have synthesized 5-thiocyanato-2′-deoxyuridine (SCNdU) along with the C6-deuterated nucleobase 5-thiocyanatouracil (6-D-SCNU) and studied their reactions with radiation-produced electrons. ESR spectra in γ-irradiated nitrogen-saturated frozen homogeneous solutions (7.5 M LiCl in H2O or D2O) of these compounds show that electron-induced S–CN bond cleavage occurs to form a thiyl radical (dU-5-S˙ or 6-D-U-5-S˙) and...
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Novel Resveratrol-Based Substrates for Human Hepatic, Renal, and Intestinal UDP-Glucuronosyltransferases
PublicationTrans-Resveratrol (tRes) has been shown to have powerful antioxidant, anti-inflammatory, anti-carcinogenic, and anti-aging properties; however, its use as a therapeutic agent is limited by its rapid metabolism into its conjugated forms by UDP-Glucuronosyltransferases (UGTs). The aim of the current study was to test the hypothesis that the limited bioavailability of tRes can be improved by modifying its structure to create analogs...
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Structure and Stability Characterization of Natural Lake Pigments Made from Plant Extracts and Their Potential Application in Polymer Composites for Packaging Materials
PublicationNatural dyes were extracted from various plant sources and converted into lake pigments based on aluminum and tin. Three different plants (weld, Persian berries, and Brazilwood) were chosen as representative sources of natural dyes. High-performance liquid chromatography (HPLC) and triple-quadrupole mass spectrometry (QqQ MS) were used to identify dyestuffs in the raw extracts. The natural dyes and lake pigments were further characterized...
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Importance of Bile Composition for Diagnosis of Biliary Obstructions
PublicationDetermination of the cause of a biliary obstruction is often inconclusive from serum analysis alone without further clinical tests. To this end, serum markers as well as the composition of bile of 74 patients with biliary obstructions were determined to improve the diagnoses. The samples were collected from the patients during an endoscopic retrograde cholangiopancreatography (ERCP). The concentration of eight bile salts, specifically...
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Badania wpływu demulgacji i doboru optymalnego demulgatora na skład fazy gazowej i ciekłej ścieków pooksydacyjnych
PublicationOczyszczanie ścieków pooksydacyjnych, pochodzących z oksydacji pozostałości z destylacji próżniowej ropy naftowej i produkcji tzw. asfaltów utlenianych, szczególnie drogowych, a także przemysłowych, stanowi duży problem technologiczny i środowiskowy. Wynika to z obecności w ściekach różnych grup związków organicznych, w tym m.in. organicznych związków siarki, tlenu i azotu. Pewna ich część jest zaabsorbowana w wodzie i częściowo...
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Optimal conditions of ramentaceone and plumbagin separation and isolation from carnivorous plants extracts using reverse phase-high performance liquid chromatography (RP-HPLC)
PublicationPreparatywna chromatografia cieczowa jest szczególnie przydatną techniką do rozdzielania i izolacji użytecznych ilości substancji z różnych skomplikowanych mieszanin. Praca prezentuje optymalne warunki rozdzielania i izolacji ramentaceonu i plumbaginy uwzględniając maksymalną selektywność rozdzielania naftochinonów od substancji balastowych z chloroformowych ekstraktów roślinnych D. aliciae i D. capensis z zastosowaniem techniki...
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PTR-MS and GC-MS as complementary techniques for analysis of volatiles: A tutorial review
PublicationThis tutorial review is a critical commentary on the combined use of two instrumental analytical techniques, namely GC-MS and PTR-MS. The first mention of such an analytical approach likely appeared after the year 2000 and despite many advantages, it has not been applied very often. Therefore, the aim of this article is to elaborate on the concept of their combined use and to provide a curse tutorial for those considering taking...
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CE-MS and GC-MS as “Green” and Complementary Methods for the Analysis of Biogenic Amines in Wine
PublicationTwo novel complementary analytical methods, namely an extraction-free capillary electrophoresis coupled to mass spectrometry (CE-MS) and direct immersion-solid-phase microextraction combined with gas chromatography-mass spectrometry (DI-SPME-GC-MS), have been developed and successfully applied for the determination of biogenic amines (BAs) in wine and fruit wine. They have been rigorously compared to each other in terms of various...
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Optimal conditions of ramentaceone and plumbagin separation and isolation from carnivorous plants extracts using normal phase-high performance liquid chromatography (NP-HPLC)
PublicationPraca prezentuje optymalne warunki rozdzielania i izolacji plumbaginy i ramentacenu z matrycy analitycznej, którą stanowią chloroformowe ekstrakty z roślin D.aliciae i D.capensis z wykorzystaiem techniki NP-HPLC. Skład eluentu dla żelu krzemionkowego jako fazy stacjonarnej był optymalizowany. Zostały przedstawione optymalne warunki powiększania skali procesu izolacji badanych metabolitów z ekstrakrów roślinnych. Określono również...
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Recent Applications of 1D GC-MS and 2D GC-MS in Foodomics Studies
PublicationGas chromatography coupled with mass spectrometry and food chemistry have been tightly linked since the 1960s. This setup is also an integral part of the omics studies when it comes to low mass metabolites. Therefore, the marriage of GC-MS and foodomics is obvious. Two-dimensional gas chromatography coupled with mass spectrometry fits perfectly within the latest trends in foodomics, since it is tailored for holistic food analysis....
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Non-toxic fluorine-doped TiO2 nanocrystals from TiOF2 for facet-dependent naproxen degradation
PublicationIn the present study, the photocatalytic degradation of naproxen (NPX), which is a nonsteroidal anti-inflammatory drug (NSAID), frequently detected in drinking water, was investigated. The F-doped TiO2 with defined morphology was successfully obtained from TiOF2 and applied for photocatalytic degradation under UV-vis and visible light. All samples were characterised by X-ray diffraction, scanning electron microscopy, X-ray photoelectron...
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Flavones in cocoa defence against Phytophthora megakarya
PublicationCross-pollination of suitable genotypes and earlier selection of elite offspring using adequate plants-associated defence markers in plantlets leaves are decisive for development of T. cacao genotypes tolerant to black pods disease (BPD). T. cacao plantlets from manual cross-pollination of ♀SNK64 × ♂UPA143 were analyzed for their susceptibility to BPD using leaf disc test. Subsequently, leaves (healthy, wounded and wound+infected)...
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Exploring DAD and ADD Methods for Dealing with Urban Heat Island Effect
PublicationThe Urban Heat Island (UHI) effect in the context of climate change and temperature fluctuations is an increasing challenge for contemporary cities. Numerous activities focus on mitigation and adaptation to the UHI effect using both appropriately selected design strategies and technological solutions. However, not all of these technologies support the postulates of ecological and low-carbon cities. Their design, implementation,...
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Preparation and HPLC evaluation of a new 1,3-alternate 25,27-bis-[p-chlorobenzyloksy]26,28-bis-[3-propyloxy]-calix[4]arene silica bonded stationary phase
PublicationPrzeprowadzono syntezę nowej fazy stacjonarnej HPLC na bazie pochodnej 25,27-bis-[p-chlorobenzyloksy]26,28-bis-[3-propyloksy]-kaliks[4]arenu zablokowanego w konformacji 1,3-naprzemianległej. Zbadano selektywność i sprawność fazy w stosunku do aromatycznych izomerów pozycyjnych, alkilobenzenów, WWA, sulfonamidów i niesterydowych leków przeciwbólowych.
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Application of GC-MS/MS technique for the determination of benzodiazepines in blood samples
PublicationAbstract Benzodiazepines (BZD) are widely used as pharmaceuticals in medicine. However, due to psychostimulatory effect of BZD, in the last decade, they are more and more often used as drugs of abuse. These compounds produce similar effects to classical illicit drugs and are sold as “legal” alternatives to them as new psychoactive substances (NPS). Currently new BZD, named designer benzodiazepines (DBZD), are synthesized each year...
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O badaniach i analizach mostów tymczasowych typu Bailey - MS 22-80
PublicationPrzedstawiono sposoby modelowania oraz wyniki badań in situ konstrukcji mostów tymczasowych typu Bailey - MS 22-80. Sformuowano wnioski dotyczące rzeczywistego zachowania się tego rodzaju konstrukcji oraz zasad modelowania w celu jednoznacznego określenia pracy i wytężenia ustroju.
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Usefulness of separation techniques for identification and determination of Oxygenated Volatile Organic Compounds used in process analytics of water and wastewater
PublicationW pracy przedstawiono przegląd i porównanie metodyk identyfikacji i oznaczania Lotnych Związków Tlenoorganicznych (LZT). Porównano metodyki klasyczne umożliwiające oznaczanie wybranej grupy związków chemicznych należących do LZT lub dokonywanie oznaczeń sumarycznej zawartości z metodykiami wykorzystującymi techniki rozdzielania. Lotne związki tlenoorganicze, do których zaliczane są aldehydy, alkohole, ketony, estry, etery oraz...
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Development and validation of a GC–MS/MS method for the determination of 11 amphetamines and 34 synthetic cathinones in whole blood
PublicationPurpose Psychoactive compounds that contain a phenylethylamine structure (such as amphetamine-type stimulants and synthetic cathinones) are one of the major classes of stimulants on the recreational drug market. Approximately 670 new psychoactive substances (NPS) are monitored only in Europe; however, new psychoactive compounds are being developed for illicit trade each year. In this context, the development of new analytical procedures...
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MS Project 2013 i MS Project Server 2013. Efektywne zarządzanie projektem i portfelem projektów
PublicationMS Project 2013 i MS Project Server 2013. Efektywne zarządzanie projektem i portfelem projektów to książka, która kompleksowo opisuje możliwości programu oraz oferowane przez niego narzędzia, uzupełniając wiedzę czytelnika o informacje związane z metodyką prowadzenia przedsięwzięć. Układ podręcznika odzwierciedla specyfikę pracy kierowników projektów, krok po kroku przedstawiając zadania, które mają oni do wykonania, a także najbardziej...
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Levels of 13 multi-class pesticide residues in Polish honeys determined by LC-ESI-MS/MS
PublicationLevels of 13 pesticides in 40 honey samples form Poland are reported. A rapid and sensitive method was developed for the LC-ESI-MS/MS determination of multi-class pesticide residues in honey samples. Liquid-liquid extraction (LLE) on a diatomaceous earth support (requiring the use of small amounts of organic solvent), followed by chromatographic separation on a C18 column and gradient elution were employed. The method quantifies...
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LC-MS/MS dtermination of isoprostanes in plasma samples collected from mice exposed to doxorubicin or tert-butyl hydroperoxide
PublicationIsoprostanes are stable products of arachidonic acid peroxidation and are regarded as the most reliable markers of oxidative stress in vivo. Here we describe the LC-MS/MS procedure enabling simultaneous determination of four regioisomers (8-iso prostaglandin F2α, 8-iso-15(R)-prostaglandin F2α, 11β-prostaglandin F2α, 15(R)-prostaglandin F2α) in plasma samples collected from mice. The four plasma isoprostanes are determined by LC–ESI-MS/MS...
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Wykorzystanie HPLC do izolacji i badań czystości antybiotyków peptydowych
PublicationPrzedstawiono metodologię izolacji i badania czystości antybiotyków peptydowych z wykorzystaniem wysokosprawnej chromatografii cieczowej (HPLC)
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Determination of benzodiazepines and Z-hypnotic drugs in whole blood samples by GC–MS/MS: Method development, validation and application
PublicationBenzodiazepines (BZDs) and Z-drugs are widely used as anxiolytics, sedative hypnotics, anticonvulsants and muscle relaxants. “Designer benzodiazepines” (DBZDs) are a new psychoactive substance class consisting of benzodiazepine derivatives that are not allowed for medical use and are known for being used recreationally. From a toxicologist standpoint, the huge number of such substances implicate a necessity for developing fast...
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Separation of fatty acids, their methyl esters and triacylglycerols by non-aqueous electrochromatography and HPLC.
PublicationElektrochromatografię kapilarną (CEC) oraz HPLC w odwróconym układzie faz zastosowano do rozdzielenia wolnych kwasów tłuszczowych, ich estrów metylowych oraz triacylogliceroli TAG. Zaproponowano własną konstrukcję zestawu laboratoryjnego do CEC oraz sposób preparowania mikrokolumn o średnicy 100 mm i długości złoża (Hypersil ODS 3 mm) 200 mm. Z porównania względnych czasów retencji TAG rozdzielanych technikami CEC i HPLC przy użyciu...
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A comparison of the spectrophotometric Winkler method and HPLC technique in the determination of 5-Hydroxymethylfurfural in natural honey
PublicationPorównano technikę HPLC i klasyczną metodę spektrofotometryczną Winklera pod względem odzysku, precyzji, wykrywalności i oznaczalności 5-hydroksymetylofurfuralu (HMF) w miodach naturalnych. Zawartości HMF obiema metodami oznaczono w 15 różnych miodach naturalnych. Sześć miodów pochodziło z trójmiejskich punktów handlowych, 9 miodów pozyskano bezpośrednio od pszczelarzy z sześciu pasiek. Testem t-Studenta oszacowano istotność różnic...
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Determination of impurities in pharmaceutical products using LC-MS
PublicationPharmaceutical products can be contaminated by residues of solvents, reagents (used for the synthesis) or degradation products. Impurities in drug may pose a risk to human health and life, therefore analysis and identification of impurities in pharmaceutical products is veryimportant and inevitable.High performance liquid chromatography coupled with mass spectrometry (MS) is very useful technique for identification impurities in...
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Comparison of GC–MS and MEKC methods for caffeine determination in preworkout supplements
PublicationIn this study, GC–MS- and MEKC-based methods for determination of caffeine (CAF) in preworkout supplements were developed and validated. The proposed protocols utilized minimal sample preparation (simple dilution and syringe filtration). The developed methods achieved satisfactory validation parameters, i.e. good linearity (R2 0.9988 and R2 0.9985 for GC–MS- and MEKC-based method, respectively), satisfactory intraand interaccuracy...
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Metodyka korekty programu elucji w kolumnowej chromatografii cieczowej - HPLC/UPC
PublicationUżytkownika aparatu HPLC / UPC oczekuje zgodności przebiegu programu elucji na wlocie do kolumny z zaprogramowana jego postacią. W praktyce - szczególnie z zastosowaniem modułów zasilania kolumny eluentem o programowanym składzie, wyposażonych w tzw. zawory proporcjonujące - mają miejsce odchylenia przebiegu programu elucji od wymaganej postaci. Ich amplituda mierzona w funkcji czasu, zależy od wartości opóźnienia transportowego...
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Determination of free tyrosine in equestrian supplements by LC–MS/MS and comparison of its quantity with total free amino acids content in view of doping control
PublicationThe reports on the probable beneficial impact of tyrosine (TYR) supplementation on performance enhancement have contributed to the growth of interest in TYR in equestrian sports field and related industries, such as the manufacture of dietary and nutritional supplements. In this study, the first attempt to the assessment of horses exposure to TYR during nutritional supplementation was demonstrated by quantification of unbound TYR...
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Oznaczanie ilościowe w HPLC.
PublicationOmówiono metody oznaczania zawartości substancji z wykorzystanie wysokosprawnej chromatografii cieczowej tj. metodę wzorca zewnętrznego, metodę dodatku wzorca, metodę prostej normalizacji oraz metodę normalizacji z uwzględnieniem współczynników korekcyjnych.
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Fazy stacjonarne na bazie pochodnych kaliksarenów : nowy typ wypełnień do HPLC
PublicationPraca przeglądowa przedstawia dotychczasowe metody syntezy faz stacjonarnych na bazie pochodnych kaliksarenów chemicznie związanych z żelem krzemionkowym. podsumowano zastosowanie tych faz w rozdzielaniu szeregu klas związków organicznych i nieorganicznych metodą Wysokosprawnej Chromatografii Cieczowej HPLC.
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Development and validation of GC–MS/MS method useful in diagnosing intestinal dysbiosis
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pH Gradient Reversed-Phase HPLC
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Rapid Evaluation of Poultry Meat Shelf Life Using PTR-MS
PublicationThe use of proton transfer reaction mass spectrometry (PTR-MS) for freshness classification of chicken and turkey meat samples was investigated. A number of volatile organic compounds (VOCs) were selected based on the correlation (> 95%) of their concentration during storage at 4 °C over a period of 5 days with the results of the microbial analysis. In order to verify if the selected compounds are not sample-specific, a number...
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LC-MS and LC-NMR as Complementary Techniques for the Determination of Pharmaceuticals in Dosage Formulations
PublicationPharmaceuticals contain not only pharmacologically active compounds but also a range of excipients. The danger exists that impurities may also be present in such drugs, which may adversely affect their efficacy and even endanger patient health and life. Monitoring the composition of pharmaceutical products is therefore essential. The trace amounts of such impurities in pharmaceuticals are often identified and determined with liquid...
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The optimisation of analytical parameters for routine profiling of antioxidants in complex mixture by HPLC coupled post-column derivatisation
PublicationIntroduction: The wide application of natural and artificial antioxidants in food, cosmetic and pharmaceutical industry as well as the recognition of the importance of food antioxidants for supporting human health created demand for reliable and industrially applicable methods of determining antioxidative activity. This requirement can be fullfilled with the recently proposed HPLC-post-column derivatisation approach enabling the...
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Problems of PAH quantification by GC-MS method using isotope-labelled standards.
PublicationChromatografia gazowa w połączeniu ze spektromerią mas (GC-MS) jest obecnie rutynowo stosowaną metodą w analityce środowiskowej do oznaczania śladowych ilości zanieczyszczeń organicznych. Stosowanie detektora mas sprawia, że wygodnym wzorcem wewnętrznym są stabilne izotopowo analogi oznaczanych związków. Związki te są wykorzystywane do śledzenia i kompensacji strat analitów podczas wykonywania określonych operacji związanych z...
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Studies on selectivity of hydrocarbon group type separation of petroleum vacuum distillates and base oils by HPLC.
PublicationW pracy przedstawiono wyniki badań nad doborem selektywnego chromatograficznego układu HPLC, umożliwiającego rozdzielenie grupowe produktów naftowych otrzymanych z destylacji próżniowej ropy naftowej, w tym, mineralnych olejów bazowych. Stwierdzono, że konieczny układ chromatograficzny wymaga wykorzystania dwóch kolumn wypełnionych żelem krzemionkowym ze związanymi grupami nitrofenopropylowymi, połączonych szeregowo z dwiema...
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Preparation of Internal Standards for 2D-UPLC-MS/MS Quantification of Noncanonical DNA Bases
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Revealing dynamic changes of the volatile profile of food samples using PTR–MS
PublicationVolatile compounds carry valuable information regarding the properties of foodstuffs. Volatiles emitted from food can be used as, for example, indicators of quality, shelf-life, or authenticity. A better understanding of the multitude of transformations which occur during food processing could facilitate the optimisation of production, increase the desirability of food products, and also their wholesomeness. However, as some of...
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Recent advancements in LC‐MS based analysis of biotoxins: Present and future challenges
PublicationThere has been a rising concern regarding the harmful impact of biotoxins, source of origin, and the determination of the specific type of toxin. With numerous reports on their extensive spread, biotoxins pose a critical challenge to figure out their parent groups, metabolites, and concentration. In that aspect, liquid chromatography‐mass spectrometry (LC‐MS) based analysis paves the way for its accurate identification and quantification....
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A novel methodology for the enantiomeric resolution of methamphetamine, its precursors and intermediates by GC-MS
PublicationImpurity profiling and classification of abused drugs using chiral analytical techniques is of particular interest and importance because of the additional information obtained from this approach. When these methods are applied to the synthesis of illicitly used substances, they can supply valuable information about the conditions/chemicals used in the synthesis. In this study, simultaneous chiral separation of methylamphetamine,...
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Validation and modification of HPLC method for monitoring acetaminophen plasma concentrations in patients with chronic pancreatitis
PublicationBackground. Pancreatitis is the inflammation of the pancreas. The infl ammation may occur suddenly and resolve in a few days with the treatment in case of acute pancreatitis (AP). Chronic pancreatitis (CP) is a persistent inflammation of the pancreas that results in irreversible morphological changes and impairment of both exocrine and endocrine functions. Abdominal...
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LC–MS/MS analysis, antioxidant and anticholinergic properties of galanga (Alpinia officinarum Hance) rhizomes
PublicationGalanga (Alpinia officinarum Hance) is a pungent and aromatic rhizome, which is a member of the ginger family (Zingiberaceae). The rhizomes of this plant have been used as a traditional medicine in far east countries for relieving stomach ache, invigorating the circulatory system, treating colds, and reducing swelling. The aim of this study was to investigate antioxidant and anticholinergic properties of galanga. For this purpose,...
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OZNACZANIE POZOSTAŁOŚCI PESTYCYDÓW W ORGANIZMACH PSZCZELICH ORAZ W MIODZIE Z WYKORZYSTANIEM PROCEDURY OPARTEJ NA ZASTOSOWANIU CHROMATOGRAFÓW SPRZĘŻONYCH Z TANDEMOWYMI SPEKTROMETRAMI MAS (GC-MS/MS i LC-MS/MS)
PublicationPestycydy to bardzo liczna grupa różnorodnych związków chemicznych stosowa-nych w rolnictwie. Ze względu na swoją trwałość gromadzą się w różnych elementach środowiska i mogą występować w obszarze, na którym nigdy nie zostały użyte. Zachodzi także proces ich bioakumulacji w tkankach oraz narządach zwierząt i roślin. Stosowane w rolnictwie środki ochrony roślin (szczególnie w okresie wzmożonych zabiegów agro-technicznych wiosną...
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Assessment of Lipophilicity Indices Derived from Retention Behavior of Antioxidant Compounds in RP-HPLC
PublicationReverse phase high pressure liquid chromatography was employed in order to evaluate the lipophilicity of antioxidant compounds from different classes, such as phenolic acids, flavanones, flavanols, flavones, anthocyanins, stilbenes, xantonoids, and proanthocyanidins. The retention time of each compound was measured using five different HPLC columns: RP18 (LiChroCART, Purosphere RP-18e), C8 (Zorbax, Eclipse XDBC8), C16-Amide (Discovery...
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Mosty tymczasowe typu BAILEY - MS 22-80 w świetle badań in SITU
PublicationW pracy przedstawiono i omówiono zakres badań, wybrane modele obliczeniowe, wyniki analiz teoretycznych i badań odbiorowych (próbnych obciążeń o rozszerzonym zakresie), oraz spostrzeżenia dotyczące zachowania się konstrukcji na przykładzie kilku badanych obiektów mostów tymczasowych typu bailey - MS 22-80.
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Quantification of methadone and its metabolites: EDDP and EMDP determined in autopsy cases using LC‐MS/MS
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