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Search results for: ANALIZA LC-DAD-MS
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Determination of non-steroidal anti-inflammatory drugs in natural waters using off-line and on-line SPE followed by LC coupled with DAD-MS
PublicationOpisano dwie metody pozwalające na jednoczesne oznaczanie zawartości niesterydowych leków przeciwzapalnych (difluisal, diklofenak, naproksen, tolmetin, fenoprofen, ibuprofen) w próbkach wodnych. Próbki przygotowywano do analizy z użyciem techniki ekstrakcji do fazy stałej (off-line i on-line). Natomiast oznaczeń końcowych dokonano z użyciem LC-DAD-MS. Sprawdzono kilka różnych kolumienek ekstrakcyjnych i wybrano RP-18 jako najlepsze...
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Application of LC-MS technique in environmental studies
PublicationW ciągu ostatnich 10-15 lat obserwuje się ciągły wzrost zainteresowania możliwościami, jakie stwarza technika LC-MS, w związku z czym dokonano przeglądu prac badawczych zrealizowanych na Wydziale Chemicznym PG związanych z użyciem tej techniki. Szczególną uwagę zyskały: kwasy fenoksyoctowe i chlorofenole, które są stosowane w rolnictwie i które mogą zanieczyszczać wody gruntowe; cjanotoksyny, które są emitowane podczas zakwitów...
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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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Determination of biogenic amines in beers by LC-MS/MS
PublicationAnalysis of biogenic amines in beers was carried out by HPLC-MS/MS after their derivatization with p-toluenesulfonyl chloride (tosyl chloride). The developed method has been applied for analysis of eighteen biogenic amines in twelve samples of different kind of beers (Lager, Strong Lager, Schwarzbier, Weizenbier, Pils, nonalcoholic Pils, Stout). The method is sensitive and the results precise for majority of the analytes.
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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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RESIDUE ANALYSIS OF ETU AND PTU BY LC/MS
PublicationDithiocarbamates (DTCs) are important organosulfur compounds, which act as inhibitors of metal dependant and sulphydryl enzymes and have a serious consequence on biological systems. They possess variety of applications in agriculture as fungicides, as well as, in the rubber industry as vulcanization accelerators and antioxidants. In this way, DTCs are the main group of fungicides used to control approximately 400 pathogens of more...
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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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Development and validation of an LC–MS/MS method for the determination of biogenic amines in wines and beers
PublicationBiogenic amines are group of organic, basic, nitrogenous compounds that naturally occur in plant, microorganism, and animal organisms. Biogenic amines are mainly produced through decarboxylation of amino acids. They are formed during manufacturing of some kind of food and beverages such as cheese, wine, or beer. Histamine, cadaverine, agmatine, tyramine, putrescine, and b-phenylethylamine are the most common biogenic amines found...
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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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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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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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The potential of LC–MS technique in direct analysis of perfume content
PublicationPerfumes are products that consist of a wide range of natural and synthetic compounds. Due to complex composition, the determination of their ingredients is a difficult task. Most of the perfume components are either volatile or semi-volatile; however, most of the attention has been paid to volatile ones, and thus, gas chromatography or electronic noses are generally used. Nevertheless, in this study, liquid chromatography coupled...
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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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An LC-MS/MS Method for a Comprehensive Determination of Metabolites of BTEX Anaerobic Degradation in Bacterial Cultures and Groundwater
PublicationBTEX (benzene, toluene, ethylbenzene, and the different xylene isomers), known for carcinogenic and neurotoxic effects, are common environmental contaminants. The first step for the development of the bioremediation technologies is the detection of intense microbial degradation in contaminated waters in the quest for the most active bacterial strains. This requires the multispecies analysis for BTEX metabolites which are considered...
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Analysis of bisphenols and their derivatives in infant and toddler ready-to-feed milk and powdered milk by LC MS/MS
PublicationReady-to-feed milk and powdered milk packed in different types of packaging lined with resin are chosen as the primary or complementary diet for infants and toddlers. An HPLC–MS/MS method was established and validated for the determination of nineteen bisphenols and their derivatives in such samples. The recoveries were from 31% to 120%, while the values of limit of detection and quantification were in the range of 0.24–0.40 and...
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Main strategies, analytical trends and challenges in LC-MS and ambient mass spectrometry-based metabolomics
PublicationA plethora of analytical LC-MS-based methods have been successfully applied to analyses of complex samples of various origin for metabolomics investigations. Over the last ten years, the substantial evolution of ambient mass spectrometry (AMS) techniques has highlighted their tremendous potential in metabolomic studies due to the minimal sample pretreatment requirement and the ability to analyse samples in their native state. This...
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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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Urine metabolic fingerprinting using LC–MS and GC–MS reveals metabolite changes in prostate cancer: A pilot study
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A Robust Method for Sample Preparation of Gastrointestinal Stromal Tumour for LC/MS Untargeted Metabolomics
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Analysis of urinary nucleosides as potential cancer markers determined using LC–MS technique
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Determining pesticide contamination in honey by LC-ESI-MS/MS - Comparison of pesticide recoveries of two liquid-liquid extraction based approaches
PublicationHoney, a valuable food product, may be contaminated by xenobiotics during its production and/or harvest. The determination of trace levels of contaminants in a complex matrix like honey still presents a challenge to analytical chemists. The aim of this work was to assess and compare the extraction efficiencies of 30 pesticide residues (acaricides, insecticides, herbicides, fungicides), belonging to over 15 different chemical classes....
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Extraction and Analysis of Bisphenols and Their Derivatives in Infant and Toddler Ready-to-feed Meals by Ultrasound-assisted Membrane Extraction Followed by LC MS/MS
PublicationThis research developed an ultrasound-assisted membrane extraction coupled with liquid chromatography-tandem mass spectrometry method for the determination of nineteen bisphenols and their derivatives in infant and toddler ready-to-feed meals. The calibration curves for all analytes were linear in the tested range, and the limit of detection and limit of quantitation were in the range 0.27 to 0.79 ng/g and 0.80 to 2.4 ng/g, respectively....
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Direct injection liquid chromatography-mass spectrometry (DI-LC-MS) analysis for rapid lipidomic profiling of extracellular vesicles
PublicationExtracellular vesicles (EVs) are small, spherical particles produced by eukaryotic and prokaryotic cells, surrounded by a bilayer membrane and carrying various bioactive molecules, such as proteins, surface receptors, membrane and soluble proteins, lipids, and nucleic acids. EVs are of substantial interest because of their important roles in cell communication, epigenetic regulation and possible application in disease diagnosis...
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Determining the true content of quercetin and its derivatives in plants employing SSDM and LC–MS analysis
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Zastosowanie techniki LC-MS/MS oraz biotestów w analityce próbek środowiskowych w celu oznaczenia ich potencjału endokrynnego i zawartości wybranych związków endokrynnych
PublicationWyniki wielu badań prowadzonych w przeciągu ostatnich lat mogą stanowić podstawę do stwierdzenia, że zanieczyszczenia emitowane do środowiska ze źródeł antropogennych mogą stanowić kolejny rodzaj zagrożenia, z którego nie zdawano sobie sprawy wcześniej. Zanieczyszczeniami takimi są substancje z grupy EDC definiowane jako jakikolwiek czynnik, który wpływa na syntezę, wydalanie, transport, wiązanie, działanie lub wydalanie hormonów...
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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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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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Plant-based meat substitute analysis using microextraction with deep eutectic solvent followed by LC-MS/MS to determine acrylamide, 5-hydroxymethylfurfural and furaneol
PublicationFor the analysis of plant-based meat substitutes and the determination of Maillard reaction products such as acrylamide, 5-hydroxymethylfurfural and furaneol, a novel and effective procedure based on hydrophobic natural deep eutectic solvent and liquid chromatography coupled with tandem mass spectrometry was developed for the first time. The 49 compositions of the deep eutectic solvents were designed and screened to select the...
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A method for a comprehensive lipidomic analysis of flaxseed (Linum usitatissimum) with the use of LC–Q-TOF-MS and dispersive micro-solid-phase (μDSPE) extraction
PublicationFlaxseed (FS) is one of the richest sources of α-linolenic acid oil and lignans, and it is suggested that the consumption of flaxseed may contribute to the prevention of certain chronic diseases such as many types of cancer, diabetes, cardiovascular diseases and cerebrovascular stroke. Here, we demonstrate a new method for comprehensive FS lipidome profiling with the use of LC–Q-TOF-MS and dispersive micro-solid-phase extraction....
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Metabolic Evaluation of Urine from Patients Diagnosed with High Grade (HG) Bladder Cancer by SPME-LC-MS Method
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A comprehensive lipidomic analysis of oilseeds using LC-Q-TOF-MS and dispersive micro-solid phase (D-μ-SPE) extraction techniques
PublicationGrowing public health awareness increased the demand for natural products with positive health benefits. Vegetable oils containing omega-3 fatty acids (FA) such as alpha-linolenic acid (ALA) has been proposed as a possible source of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA). In this work, a comprehensive lipidome analysis and comparison of seven oilseeds, including flaxseed, chia, hemp, black cumin, white sesame,...
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Rapid and simple multi-analyte LC–MS/MS method for the determination of benzodiazepines and Z-hypnotic drugs in blood samples: Development, validation and application based on three years of toxicological analyses
PublicationBenzodiazepines (BZDs) and Z-drugs have been particularly important treatments for sleeping and anxiety disorders for many years. However, recently, a number of new benzodiazepines (named designer benzodiazepines, DBZDs) were synthesised, but some of them have never been used in the clinic; they reached the black drug market as new psychoactive substances and are used for recreational purposes. The abuse of these substances has...
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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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Concentration of Potentially Bioactive Compounds in Italian Extra Virgin Olive Oils from Various Sources by Using LC-MS and Multivariate Data Analysis
PublicationHigh quality extra virgin olive oils represent an optimal source of nutraceuticals. The European Union (EU) is the world’s leading olive oil producer, with the Mediterranean region as the main contributor. This makes the EU the greatest exporter and consumer of olive oil in the world. However, small olive oil producers also contribute to olive oil production. Beneficial effects on human health of extra virgin olive oil are well...
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Selectivity Tuning by Natural Deep Eutectic Solvents (NADESs) for Extraction of Bioactive Compounds from Cytinus hypocistis—Studies of Antioxidative, Enzyme-Inhibitive Properties and LC-MS Profiles
PublicationIn the present study, the extracts of Cytinus hypocistis (L.) L using both traditional solvents (hexane, ethyl acetate, dichloromethane, ethanol, ethanol/water, and water) and natural deep eutectic solvents (NADESs) were investigated in terms of their total polyphenolic contents and antioxidant and enzyme-inhibitive properties. The extracts were found to possess total phenolic and total flavonoid contents in the ranges of 26.47–186.13...
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Activity assay of O-Acetyl-L-homoserine sulfhydrylase (CaMet15p).
Open Research DataThe study aimed to obtain conditions optimal for the activity of O-acetyl-L-homoserine sulfhydrylase (CaMet15p) and a method suitable for its measurement. The selection of appropriate reaction conditions included the identification of the reaction buffer and its pH, substrate and enzyme concentrations. The activity of CaMet15p was measured by the detection...
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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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Barbara Kusznierewicz dr hab. inż.
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Cyanobacterial toxins in fresh and brackish waters of Pomorskie Province (Northern Poland)
PublicationPraca dotyczy oznaczania toksyn należących do grupy hepatotoksycznych peptydów cyklicznych oraz neurotoksycznych alkaloidów. Są one odpowiedzialne za uszkodzenia ryb i ptaków, które powstają w wyniku zakwitu glonów. Badano zakwity w wodach słodkich Pomorza. Oznaczano hepatoksyny, mikrocysty oraz nodularynę. Opracowano w tym celu warunki analityczne przy zastosowaniu techniki HPLC-DAD. Do identyfikacji anatoksyny-A użyto techniki...
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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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Metody chromatograficzne
e-Learning CoursesCelem nadrzędnym jest zapoznanie studentów z rozmaitymi technikami umożliwiającymi rozdzielanie mieszanin substancji. Techniki separacyjne, a szczególnie techniki chromatograficzne są dzisiaj najczęściej stosowanymitechnikami laboratoryjnymi, żadne współczesne laboratorium chemiczne czy biochemiczne nie może się bez nich obejść. Studenci będą zapoznawali się z technikami takimi, jak: współczesna chromatografia cieczowa, kapilarna...
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Studies on fluorene stability in different liquid media. Badania stabilności fluorenu w środowiskach ciekłych.
PublicationPrzedstawiono degradację fluorenu w różnych rozpuszczalnikach (acetonitryl,metanol, woda, DMSO, heksan, cykloheksan). Proces monitorowano przy zastosowaniu techniki HPLC-DAD-MS. Zbadano wpływ światła, bakterii i temperatury.Zidentyfikowano produkty degradacji jakimi okazał się kwas salicylowy oraz g-fluorenon.
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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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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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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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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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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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The influence of plant protection by effective microorganisms on the content of bioactive phytochemicals in apples
PublicationThe phytochemicals of two apple cultivars (Yellow Transparent and Early Geneva) protected in two ways, conventionally with chemical pesticides or by effective microorganisms (EM), were compared. Two types of components were determined: lipids synthesised constitutively and generated via inducible pathways polyphenols along with antioxidant activity and profiles. The antioxidant activities assessed with ABTS, DPPH and Folin–Ciocalteu...