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Application and optimization of headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography - flame-ionization detector (GC-FID) to determine products of the petroleum industry in aqueous samples
PublikacjaA simple and solvent-free analytical method has been optimized for the determination of hydrocarbons (C6 - C20) from products of the petroleum industry in aqueous samples. Extraction and analysis was carried out using headspace solid-phase microextraction (HS-SPME) and gas chromatography coupled with flame-ionization detector (GC-FID). A ZB-5 capillary column (30 m × 0.25 mm inner diameter, 0.25 µm film thickness) was used for...
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Molecular mechanism of retention in reversed-phase high-performance liquid chromatography and classification of modern stationary phases by using quantitative structure–retention relationships
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Simultaneous determination of hydrophobicity and dissociation constant for a large set of compounds by gradient reverse phase high performance liquid chromatography–mass spectrometry technique
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Determination of phenylbutazone, sulfamethazine, carbendazim and linuron using a novel pine bark biosorbent for solid-phase extraction (SPE) with high-performance liquid chromatography (HPLC)
PublikacjaThe paper presents a novel pine bark based biosorbent for solid-phase extraction (SPE). The morphology and composition of the pine bark were characterized using Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The biosorbent was used for the preparation of wastewater for the determination of phenylbutazone, sulfamethazine, carbendazim, and linuron by high performance liquid chromatography with...
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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)
PublikacjaPreparatywna 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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Optimal conditions of ramentaceone and plumbagin separation and isolation from carnivorous plants extracts using normal phase-high performance liquid chromatography (NP-HPLC)
PublikacjaPraca 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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Determination of eight artificial sweeteners and common Stevia rebaudiana glycosides in non-alcoholic and alcoholic beverages by reversed-phase liquid chromatography coupled with tandem mass spectrometry.
PublikacjaThe method for the determination of acesulfame-K, saccharine, cyclamate, aspartame, sucralose, alitame, neohesperidin dihydrochalcone, neotame and five common steviol glycosides (rebaudioside A, rebaudioside C, steviol, steviolbioside and stevioside) in soft and alcoholic beverages was developed using high-performance liquid chromatography and tandem mass spectrometry with electrospray ionisation (HPLC-ESI-MS/MS). To the best of...
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Comparison of hydrophilic interaction and reversed phase liquid chromatography coupled with tandem mass spectrometry for the determination of eight artificial sweeteners and common steviol glycosides in popular beverages
PublikacjaHydrophilic interaction liquid chromatography (HILIC) coupled with tandem mass spectrometry (MS/MS) was used to separate artificial and natural sweeteners approved for use in European Union (EU). Among three tested HILIC columns (BlueOrchid PAL-HILIC, Ascentis Express Si and Acclaim™ Trinity™ P2) the last one was selected for the development of HILIC method due to the best results obtained with it. Early eluting and coeluting compounds...
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Dispersive solid-phase extraction using multi-walled carbon nanotubes combined with liquid chromatography–mass spectrometry for the analysis of β-blockers: Experimental and theoretical studies
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Optimization of a Fabric Phase Sorptive Extraction protocol for the isolation of six bisphenols from juice pouches to be analysed by high performance liquid chromatography coupled with diode array detector
PublikacjaFabric Phase Sorptive Extraction (FPSE) combined with high pressure liquid chromatography using to diode array detection (HPLC-DAD) was applied for the simultaneous determination of bisphenols (BPA, BPB, BPC, BPE, BPF, BPS) in juice pouches. The FPSE procedure was optimized with regards to the critical parameters that affect the performance of the method including the selection of the FPSE membrane type and size, adsorption time,...
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Characterization of GM3 Gangliosides in Human Milk throughout Lactation: Insights from the Analysis with the Use of Reversed-Phase Liquid Chromatography Coupled to Quadrupole Time-Of-Flight Mass Spectrometry
PublikacjaGangliosides are complex lipids found in human milk that play important structural and biological functions. In this study, we utilized reversed-phase liquid chromatography coupled to quadrupole time-of-flight mass spectrometry to evaluate the molecular distribution of GM3 in human milk samples collected at distinct lactation stages, ranging from colostrum to advanced lactation samples. Throughout lactation, GM3 d40:1 emerged as...
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Application of multivariate mathematical-statistical methods to compare reversed-phase thin-layer and liquid chromatographic behaviour of tetrazolium salts in Quantitative Structure-Retention Relationships (QSRR) studies
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Preparation and evaluation of 1,3-alternate 25,27-dibenzyloxy-26,28-bis-[3-propyloxy]-calix[4]arene - bonded silica stationary phase for high performance liquid chromatography
PublikacjaOtrzymano nową fazę stacjonarną na bazie dibenzyloksy pochodnej kaliks[4]arenu w konformacji 1,3-naprzemianległej, chemicznie związaną z żelem krzemionkowym. Przeprowadzano badania selektywności i sprawności tej fazy w rozdzielaniu izomerów konstytucyjnych benzenu i pochodnych fenoli. Zaprezentowano wyniki badania wpływu pH fazy ruchomej oraz stężenia metanolu na zdolność rozdzielczą nowej fazy stacjonarnej.
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Studies on solid phase microextraction-gas chromatographic determination of volatile chloroorganic pollutants in soil. badanie lotnych związków chloroorganicznych w glebie przy użyciu techniki mikroekstrakcji do fazy stacjonarnej i chromatografii gazowej.
PublikacjaLotne związki chloroorganiczne (VOXs) mogą być obecne w powietrzu, wodzie i glebie. Związki te mają właściwości kancerogenne, dlatego też ich ilość w środowisku powinna być monitorowana. W pracy przedstawiono badania nad możliwością zastosowania techniki izolacji i wzbogacania jaką jest mikroekstrakcja do fazy stacjonarnej, jej przydatność w analizie lotnych węglowodorów chloroorganicznych w różnych typach gleb z wykorzystaniem...
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Application of gas flow headspace liquid phase micro extraction coupled with gas chromatography-mass spectrometry for determination of 4-methylimidazole in food samples employing experimental design optimization
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Preparation and evaluation of 1,3-alternate 25,27-bis-(pentafluorobenzyloxy)-26,28-bis-(3-propyloxy)-calix[4]arene-bonded silics gel high performance liquid chromatography stationary phase
PublikacjaA 1,3-alternate 25,27-bis-(pentafluorobenzyloxy)-26,28-bis-(3-propyloxy)-calix[4]arene-bonded silica gel stationary phase (CalixBzF10) was synthesized, structurally characterized, and used as a selector in liquid chromatography. The selectivity study of this phase was done by using fluorine-containing compounds (fluorobenzenes, fluoro-pyrimidine bases), as well as non-fluorinated analytes (non-steroidal anti-inflammatory drugs,...
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High-performance liquid chromatography of di- and trisubstituted aromatic positional isomers on 1,3-alternate 25,27-dipropoxy-26,28-bis-[3-propyloxy]-calix[4]arene-bonded silica gel stationary phase.
PublikacjaOtrzymano nową fazę stacjonarną na bazie dipropyloksy pochodnej kaliks[4]arenu w konformacji 1,3-naprzemianległej chemicznie związaną z żelem krzemionkowym. Przeprowadzono badanie selektywności i sprawności tej fazy w rozdzielaniu izomerów konstytucyjnych benzenu. Zaprezentowano wyniki badania wpływu warunków chromatograficznych (pH fazy ruchomej, temperatura, stężenie modyfikatora organicznego) na zdolność rodzielczą tej nowej...
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Determination of carbonyl compounds in distilled alcoholic beverages using gas chromatography and head-space solid phase microextraction. Oznaczanie związków karbonylowych w napojach alkoholowych z użyciem chromatografii gazowej i mikroekstrakcji do fazy stacjonarnej z fazy nadpowierzchniowej
PublikacjaW pracy przedstawiono badania nad opracowaniem procedury oznaczania związków karbonylowych z użyciem mikroekstrakcji do fazy stacjonarnej w wersji analizy fazy nadpowierzchniowej (HS-SPME), chromatografii gazowej z detekcją wychwytu elektronów(GC-ECD) oraz derywatyzacji pentafluorobenzylohydroksyloaminą (PFBHA). Opisano wpływ parametrów: temperatury, mieszania, czasu ekspozycji włókna, dodatku soli, stężenia alkoholu. Opracowaną...
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Zastosowanie połączenia mikroekstrakcji do fazy stacjonarnej i chromatografii gazowej do oznaczania lotnych kwasów tłuszczowych w próbkach środowiskowych i pokrewnych=Application of combination of solid phase microextraction and gas chromatography for determination of volatile fatty acids in environmental and related samples
PublikacjaOznaczanie lotnych kwasów tłuszczowych (LKT) w próbkach środowiskowych wymaga najczęściej izolacji i wzbogacania analitów na etapie przygotowania próbek oraz zastosowania techniki o dużym potencjale separacyjnym i identyfikacyjnym na etapie oznaczeń końcowych. W pracy dokonano krytycznego przeglądu zastosowań wygodnej i często stosowanej techniki mikroekstrakcji do fazy stacjonarnej (SPME) w połączeniu z wysokosprawną techniką...
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On the Mechanism of Electrochemical Oscilations in Three-Phase System Containing Nitrobenzene with Picric Acid as Liquid Membrane.O mechaniźmie oscylacji róznicy potencjału elektorchemicznego w trójfazowych układach zawierających nitrobenzen z kwasem pikrynowym jako membraną ciekłą.
PublikacjaPodano składowe różnicy potencjału elektrochemicznego między fazami wodnymi oscylatora z nitrobenzynową membraną ciekłą. Na tej podstawie oraz zmian stężeń składników układu w trakcie procesu zaproponowano mechanizm powstawania oscylacji w którym najważniejszą rolę odgrywają procesy adsorpcji/desorpcji surfaktantu na granicach faz.
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Opracowanie optymalnych warunków rozdzielania i identyfikacji metabolitów ro lin z rodzaju droseraceae, z zastosowaniem wysokosprawnej kolumnowej chromatografii cieczowej= A research on the composition of eluent for separation of plant metabolites by column reversed phase liquid chromatography
PublikacjaOd kilku lat na świecie trwają badania składników roślin owadożernych wykazujących atrakcyjne właściwości biologicznie czynne, tj. działanie przeciwbakteryjne, przeciwgrzybowe, antyoksydacyjne, a być może, także, przeciwnowotworowe. Pozyskiwanie substancji biologicznieaktywnych z materiału naturalnego, na drodze hodowli in vitro a następnie ekstrakcji i rozdzielania jest bardziej korzystne pod względem ekonomicznym, niż ich wytwarzanie...
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Zastosowanie chromatografii cieczowej w odwróconym układzie faz (RP-LC) w rozdzielanie i oznaczaniu polifenoli i naftochinonów w materiałach roslinnychreversed = Phase liquid chromatography (RP-LC) for separation and quantitative determination of polyphenols and naphtoquinones in plant materials
PublikacjaW pracy przedstawiono przegląd metod rozdzielania i oznaczania naftochinonów i polifenoli pochodzących z materiału roślinnego, z wykorzystaniem technik chromatograficznych w układzie faz odwróconych - RP-TLC (Reversed-Phase Thin Layer Chromatography) oraz RP-HPLC (Reversed-Phase High Performance Liquid Chromatography). Przeanalizowano procedury przygotowania próbki, etap rozdzielania, a także kontroli czystości zbieranych frakcji....
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Developments in ultrasound-assisted microextraction techniques for isolation and preconcentration of organic analytes from aqueous samples
PublikacjaThe great potential of ultrasonic assistance in sample preparation, especially extraction, is being recognized. In this review, we discuss the applications of ultrasonic radiation in assisting microextraction. Topics covered include ultrasound-assisted emulsification microextraction, ultrasound-assisted-emulsification-dispersive liquid-liquid microextraction, and ultrasound-assisted hollow-fiber liquid-phase microextraction with...
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Application of additional factors supporting the microextraction process
PublikacjaDue to the fact that green analytical chemistry is of high importance, the past two decades have witnessed a rapid growth in the sample preparation area with special emphasis on simplification, miniaturization and automation of extraction procedures. In addition, to accelerate the extraction processes and to improve the separation of analytes, several enhanced parameters are applied. These factors include, ultrasounds, microwaves,...
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Ionic liquids in the microextraction techniques: the influence of ILs structure and properties
PublikacjaIonic liquids (ILs) are composed entirely of ions thus they possess unique properties, including negligible volatility, a liquid state in a broad range of temperatures and ability to change them depending on the chosen type of anion and cation, which make ILs unique and useful for many applications in sample preparation techniques. A deeper understanding of the nature of ILs and the impact of their structure on their parameters...
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Sorbents modified by deep eutectic solvents in microextraction techniques
PublikacjaIn recent years, considerable attention has been directed towards the employment of green solvents, specifically deep eutectic solvents (DES), in liquid phase microextraction techniques. However, comprehensive and organized knowledge regarding the modification of sorbent surface structures with DES remains limited. Therefore, this paper reviews the application of DES in modifying and improving the properties of sorbents for microextraction...
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Analytical applications and physicochemical properties of ionic liquid-based hybrid materials: A review
PublikacjaIonic liquids with their unique properties found so far numerous analytical applications. Among them ionic liquids immobilized on the surface or within the pores of a solid support were successfully utilized in extraction techniques dedicated to preconcentration of the analytes from food, environmental and biological samples. In this review we focus on comprehensive summarizing of available literature data on the examples of ionic...
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Hydrophobic deep eutectic solvents in microextraction techniques–A review
PublikacjaOver the past decade, deep eutectic solvents (DES) have been widely studied and applied in sample preparation techniques. Until recently, most of the synthesized DES were hydrophilic, which prevented their use in the extraction of aqueous samples. However, after 2015 studies on the synthesis and application of hydrophobic deep eutectic solvents (HDES) has rapidly expanded. Due to unique properties of HDES i.e. density, viscosity,...
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Deep eutectic solvents in analytical sample preconcentration Part B: Solid-phase (micro)extraction
PublikacjaOne of the key challenges of modern analytical chemistry is the monitoring of trace amounts of contaminants using sensitive and selective instrumental techniques. Due to the variety and complexity of some samples, it is often necessary to properly prepare a sample and to perform a preconcentration of trace amounts of analytes. In line with the principles of Green Analytical Chemistry (GAC), it is important for an analytical procedure...
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Polymeric porous membranes as solid support and protective material in microextraction processes: A review
PublikacjaPolymeric porous membranes have proven to be a versatile and efficient material for microextraction processes. In analytical practice, they are used both as a solid support and as a protective medium for improved sample preparation in various analytical applications. Polymeric porous membranes offer unique advantages in microextraction due to their large surface area and controllable pore size, eliminating interfering effects from...
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Lab-in-syringe as a practical technique for automatic microextraction: Evaluation by Blue Applicability Grade Index
PublikacjaLab-in-syringe (LIS) is a powerful automatic technique that is derived from sequential injection analysis. In LIS, a computer-controlled syringe pump is employed, and its syringe barrel serves as a mixing, reaction, and/or extraction chamber. Until now, the LIS concept has been efficiently employed for the automation of solid-phase microextraction and liquid-phase microextraction protocols as a front-end to a plethora of chromatographic...
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Application of modern sample-preparation techniques to the determination of chloropropanols in food samples
PublikacjaChloropropanols are heat-induced food toxicants that recently caused concern among industrial and scientific experts. World and European organizations related to food safety asked researchers to investigate mitigation strategies regarding these contaminants. The essential objective of this project was development of fast analytical methods enabling reliable determination and quantification of 3-monochloropropane-1,2-diol, 2-monochloropropane-1,3-diol...
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The dispersive micro-solid phase extraction method for MS-based lipidomics of human breast milk*
PublikacjaA simple and rapid microextraction method ensuring high lipidome coverage was developed for liquid chromatography mass spectrometry (LC-MS)-based lipidomics of human breast milk. The dispersive microsolid phase extraction (D-µ-SPE) technique, coupled with the design of experiment (DoE) method, enabled the study of the influence of several conditions (desorption solvent, stationary phase ratio, and sorption and desorption time)...
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Solventless and solvent-minimized sample preparation techniques for determining currently used pesticides in water samples: A review
PublikacjaThe intensification of agriculture means that increasing amounts of toxic organic and inorganic compounds are entering the environment. The pesticides generally applied nowadays are regarded as some of the most dangerous contaminants of the environment. Their presence in the environment, especially in water, is hazardous because they cause human beings to become more susceptible to disease. For these reasons, it is essential to...
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New achievements in the field of extraction of trace analytes from samples characterized by complex composition of the matrix
PublikacjaWithout any doubt, the monitoring of compounds present in samples at trace or ultra-trace level usually requires a preliminary step of isolation and/or enrichment of analytes due to the fact that majority of analytical techniques are not sensitive enough for direct determination of trace compounds. On the other hand, sample preparation is considered as crucial part of whole analytical procedures, in particular in samples characterized...
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Multicriteria decision analysis in ranking of analytical procedures for aldrin determination in water
PublikacjaThe study presents the possibility of multi-criteria decision analysis (MCDA) application when choosing analytical procedures with low environmental impact. A type of MCDA, Preference Ranking Organization Method for Enrichment Evaluations (PROMETHEE), was chosen as versatile tool that meets all the analytical chemists – decision makers requirements. Twenty five analytical procedures for aldrin determination in water samples (as...
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Dariusz Mikielewicz prof. dr hab. inż.
OsobyDariusz Mikielewicz – urodził się 6 lutego 1967 roku w Gdańsku, w 1985r. zdał pomyślnie egzaminy wstępne na Wydział Budowy Maszyn Politechniki Gdańskiej, który ukończył z wynikiem bardzo dobrym w 1990 roku na specjalności Maszyny i Urządzenia Energetyczne. Zainteresowania pracą naukową skłoniły go do podjęcia badań na University of Manchester na wydziale mechanicznym i energetyki jądrowej (Mechanical and Nuclear Engineering Department)...
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Analytical procedures for quality control of pharmaceuticals in terms of residual solvents content: Challenges and recent developments
PublikacjaResidual solvents play an important role in the synthesis of drugs and in product formulations. In addition, they pose a serious problem, that is toxicity, as many of them exhibit toxic or environmentally hazardous properties. Therefore, constant monitoring of quality control is needed. In this study, we present an overview of regulatory and general methods described by various pharmacopoeias. Then, the most commonly used methodologies...
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Nowe rozwiązania metodyczne i techniczne w zakresie techniki mikroekstrakcji do fazy stracjonarnej
PublikacjaSample preparation has been recognized as a critical step of the analytical process, being even considered as the bottleneck of the overall process. Enrichment of target compounds, transfer of the analytes into a solvent compatible with the analytical instrumentation, minimization of potential interferences, and efficient sample clean-up, are among the main aims of sample preparation techniques. In this regard, liquid-liquid extraction...
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Evaluation of Green Sample Preparation Techniques for Organic Compounds
PublikacjaNowadays, Green Analytical Chemistry (GAC) idea is of high importance, with impact on the rapid growth in the sample preparation area with special emphasis on sample preparation simplification, miniaturization and automation. Due to the fact that GAC is of high importance today, this study is focused on the evaluation of green sample preparation techniques for organic compounds. It is well known that sample preparation is considered...
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Application of ionic liquids in microextraction techniques: Current trends and future perspectives
PublikacjaIonic liquids (ILs) with their unique properties found so far numerous analytical applications. Among them ILs both in their liquid form and immobilized on the surface or within the pores of a solid support were successfully utilized in microextraction techniques. The scope of this review will cover a comprehensive summarizing of available literature data on selected properties of ILs playing a key role in analytical purposes,...
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Ionic liquids-based microextraction techniques
PublikacjaIn recent years, the development of highly efficient analytical techniques is of great importance, however, the direct analysis of complex sample matrix is still impossible in many cases. Therefore, the step of sample preparation is commonly involved in an analytical procedure. Over the years, it has been realized that the major source of inaccuracy and imprecision on general analysis results from the operations associated to sample...
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‘Green’ multi - residue methods for the determination of high importance currently used pesticides in environmental samples
PublikacjaThe purpose of the research has been to develop and apply ‘green’ analytical methodologies to control and monitor the level of currently used pesticides from different chemical groups in aqueous samples. For extraction of analytes solid - phase microextraction (SPME) and dispersive liquid - liquid microextraction (DLLME) have been applied and compared. For SPME, commonly used materials for coating fibers include: polydimethylsiloxane...
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Head-Space SPME for the Analysis of Organophosphorus Insecticides by Novel Silica IL-Based Fibers in Real Samples
PublikacjaThis work demonstrates the suitability of a newly developed ionic liquid (IL)-based silica SPME fiber for the determination of seven organophosphorus insecticides in cucumber and grapefruit samples by headspace solid-phase microextraction (HS-SPME) with a gas chromatography–flame ionization detector (FID). The sol-gel method released four different sorbent coatings, which were obtained based on a silica matrix containing ILs immobilized...
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DETERMINATION OF SURFACTANTS IN ENVIRONMENTAL SAMPLES. PART II. ANIONIC COMPOUNDS
PublikacjaSurfactants (SAA) with negative charge of polar group are named as anionic compounds. They are main constituent of most products containing synthetic surfactants. The linear alkylbenzene sulfonates (LAS), alkyl ethoxysulfates (AES) and alkyl sulfates (AS) are typically applied from this class of compounds. Those surfactants are ingredients of household detergents and cleaners, laundry detergents, cosmetic. Moreover they can be...
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PBDEs in environmental samples: Sampling and analysis
PublikacjaThe paper reviews the subject literature concerning analytical procedures routinely sed for monitoring polybrominated diphenyl ethers (PBDE) in environmental samples. It describes and summarizes subsequent stages of analytical procedure including sample collection and preparation, extraction, clean-up and final determination. Different approaches with their advantages and limitations are presented. Special attention is drawn to...
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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
PublikacjaThis 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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Solid Phase Micro-Extraction, a Versatile and Handy Tool in Environmental Trace Organic Analysis, Gets a New Class of Coatings, Polymeric Ionic Liquids
PublikacjaSolid phase microextraction (SPME) fundamentals, characteristics and application are described. The special stress is put on characteristics of sorbents used as SPME fiber coatings. Description of commercially available fibers and the present-day trends in development of new sorbents for SPME are given. Discussion is focused on possibility of application of ionic liquids (IL) and polymeric ionic liquids (PIL) as SPME fiber coatings....
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Multi-objective optimization of microextraction procedures
PublikacjaOptimization of extraction process requiresfinding acceptable conditions for many analytes and goodperformance in terms of process time or solvent consumption. These optimization criteria are oftencontradictory to each other, the performance of the system in given conditions is good for some criteriabut poor for others. Therefore, such problems require special assessment tools that allow to combinethese contradictory criteria into...
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Microextraction by packed sorbent: Uncommon detection techniques, sorbents, samples and analytes
PublikacjaAmong sample preparation approaches, the most desirable are procedures that ensure high efficiency and reproducibility, that are cheap, fast and simple, that minimize the number of operational steps and that require a small amount of sample and solvent and are thus environmentally friendly. Microextraction by packed sorbent (MEPS) is a miniaturized form of solid-phase extraction, the use of which has been continuously expanding...