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Search results for: SOLID-PHASE SYNTHESIS
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Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry
PublicationSolid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about...
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Deep eutectic solvents in analytical sample preconcentration Part B: Solid-phase (micro)extraction
PublicationOne 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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A headspace solid-phase microextraction method development and itsapplication in the determination of volatiles in honeys by gas chromatography
PublicationThe first part of the paper presents the detailed optimisation of all steps of the determination procedureof volatiles from Polish honeys by headspace solid-phase microextraction (HS-SPME) as the sample preparationmethod and gas chromatography/mass spectrometry (GC-MS) as the method of final determination.The methodology of semi-quantative analysis allowed the isolation and identification of volatile fractioncompounds from popular...
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Application of magnetic nanoparticles for magnetic solid-phase extraction in preparing biological, environmental and food samples
PublicationThe need to obtain meaningful results as the basis for determining the content of trace amounts of analytes has become the driving force behind the development of modern analytical techniques, including sample-preparation techniques, such as solid-phase extraction (SPE). Recently, great interest was aroused in the use of magnetic nanoparticles (MNPs) in SPE. These materials exhibit high selectivity, and, in small amounts, can provide...
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Understainding solid-phase microextraction: key factors influencing the extraction process and trends in improving the technique
PublicationAnalytical chemists are faced with the daunting challenges of accurately monitoring the state of the environment and the processes taking place in it and of determining an enormous range of analytes often present in trace and ultratrace amounts in sample matrixes with complex or variable compositions. Further challenges are presented by the need to introduce new methodologies into current analytical practice and equipment to comply...
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The dispersive micro-solid phase extraction method for MS-based lipidomics of human breast milk*
PublicationA 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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Solid phase microextraction combined with chromatography - a powerful tool for determination of warfare agents and related compounds
PublicationOpisano zastosowanie mikroekstrakcji do fazy stacjonarnej do izolacji wzbogacania środków bojowych i produktów ich degradacji w powietrzu, wodzie i glebie oraz próbkach bilogicznych. Na etapie oznaczeń końcowych stosuje się najczęściej chromatografię gazową. Anality można pobierać przez bezpośrednie zanurzenie włókna w próbce ciekłej i gazowej oraz w fazie nadpowierzchniowej. Stosując SPME-GC można osiągnąć niskie granice oznaczalności...
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New type of repeated Si–C-podand catalysts for solid–liquid phase transfer reactions
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Experimental investigations of hydraulic jump created by a two-phase impin-ging jet on a solid surface
PublicationPrzedstawiono rezultaty badań eksperymentalnych powstawania uskoku hydraulicznego tworzonego przez dwufazową strugę uderzającą.
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Determination of pesticides in water using new solid phase extraction technique - speedisk and speedisk column.
PublicationW publikacji opisano zastosowanie nowych narzędzi do ekstrakcji do fazy stałej: szybkie dyski i szybkie kolumienki (speedisk i speedisk column). Zaprezentowano ich zastosowanie do ekstrakcji pestycydów z próbek wody, przy zastosowaniu różnych rozpuszczalników.
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Evaluation of headspace solid-phase microextraction for the analysis of volatile carbonyl compounds in spirits and alcoholic beverages
PublicationOpracowano metodę oznaczania C1-C6 związków karbonylowych w układzie GC-ECD w roztworach alkoholowych poprzez derywatyzację pentafluorobenzylohydroksy-aminą i mikroekstrakcję w fazie stacjonarnej z fazy nadpowierzchniowej. Zoptymalizowano warunki eksperymantalne: zawartość alkoholu, czas ekspozycji, temperaturę i sposób mieszania próbki. W metodzie tej najpierw przeprowadza się rozcieńczenie spirytusu lub napojów alkoholowych do...
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Alginate-based sorbents in miniaturized solid phase extraction techniques - Step towards greenness sample preparation
PublicationIn response to growing concerns about environmental degradation, one of the main areas of research activity in recent years has been to make sample preparation methods more sustainable and eco-friendly. The increasing greenness of this step can be achieved by minimizing the usage of reagents, automating individual stages, saving energy and time, and using non-toxic, biodegradable substances. Therefore, the use of natural materials...
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Facile synthesis N-doped hollow carbon spheres from spherical solid silica
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Porous material-based sorbent coatings in Solid-phase microextraction technique: Recent trends and future perspectives
PublicationThe use of porous materials as sorbents in sample preparation techniques has gained recent scientific attention in the context of developing novel fibers for the Solid-phase microextraction (SPME) technique. SPME requires the appropriate selection of a robust sorbent for successful utilization under variable conditions. A deeper understanding of the nature of newly developed porous SPME coatings and the impact of their structures...
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Direct solid phase microextraction combined with gas chromatography – Mass spectrometry for the determination of biogenic amines in wine
PublicationA direct method based on immersion solid phase microextraction (DI-SPME) gas chromatography mass-spectrometry (GC-MS) was optimized and validated for the determination of 16 biogenic amines in Polish wines. In the analysis two internal standards were used: 1,7-diaminoheptane and bis-3-aminopropylamine. The method allows for simultaneous extraction and derivatization, providing a simple and fast mode of extraction and enrichment....
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Determination of volatile fatty acid ethyl esters in raw spiritsusing solid phase microextraction and gas chromatography
PublicationPrzedstawiono opracowanie i opymalizację metody analitycznej oznaczania estrów etylowych kwasów tłuszczowych w destylatach rolniczych różnej jakości lub wyprodukowanych z różnych surowców. W badaniach wykorzystywano technikę mikroekstrakcji do fazy stacjonarnej (HS-SPME) oraz kapilarnej chromatografii gazowej (CGC) z detektorem płomieniowo-jonizacyjnym (FID). Ekstrakcja związków lotnych prowadzona była według opracowanej procedury,...
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Headspace solid-phase microextraction and gas chromatography-olfactometry analysis of raw spirits of different organoleptic quality
PublicationCelem pracy było określenie, ktore związki wnoszą wkład w aromat destylatów rolniczych i wskazać te z nich które mogą powodować obniżenie ich właściwości organoleptycznych. W badaniach zastosowano ekstrakcję lotnych analitów z fazy nadpowierzchniowej techniką mikroekstrakcji do fazy nadpowierzchniowej w połączeniu z chromatografia gazową z detekcja olfaktometryczną . Znaleziono 40 zsubstancji, które mogą być markerami jakości organoleptycznej
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Gas chromatographic determination of volatile aliphatic and selected aromatic amines, without derivatization: solid phase microextraction
PublicationW pracy opisano wykorzystanie techniki chromatografii gazowej do oznaczania śladowych stężeń lotnych amin alifatycznych i wybranych amin aromatycznych w próbkach o różnym składzie matrycy. W tym przypadku aminy nie podlegają procesowi derywatyzacji przed etapem końcowym a na etapie pobierania próbek analitów jest wykorzystana technika mikroekstrakcji do fazy stacjonarnej (SPME).
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Polymeric metal‐containing ionic liquid sorbent coating for the determination of amines using headspace solid‐phase microextraction
PublicationThis study describes the design, synthesis, and application of polymeric ionic liquid sorbent coatings featuring nickel metal centers for the determination of volatile and semivolatile amines from water samples using headspace solidphase microextraction. The examined polymeric ionic liquid sorbent coatings were composed of two ionic liquid monomers (tetra(3-vinylimidazolium)nickel bis[(trifluoromethyl)sulfonyl]imide [Ni2+(VIM)4]...
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Synthesis, structural characterization and reactivity of new trisubstituted N1-acylamidrazones: solid state and solution studies
PublicationA series of new linear trisubstituted N1-acylamidrazones have been investigated using a variety of analytical techniques and theoretical calculations to check the influence of the type of N1-acyl substituent on the resonance forms and conformational behavior in the solid state and in solution. The 1D- and 2D-NMR experiments, supported by computational studies, revealed that in solution all amidrazones exhibit conformational syn/anti...
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Studies on applicability of new solid-phase microextraction fibers for the selective extraction and determination of short - chain monocarboksylic acids
PublicationShort-chain monocarobxylic acids, sometimes referred to as volatile fatty acids (VFA), are a group of low molecular weight alkyl monocarboxylic acids that are widely distributed within the environment. These molecules contain any from 2 to 8 carbon atoms and originate from the anaerobic biodegradation of organic matter such as carbohydrates, proteins, and fats. These compounds are commonly found in the effluents from animal farming,...
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A solid phase extraction–ion chromatography with conductivity detection procedure for determining cationic surfactants in surface water samples
PublicationA new analytical procedure for the simultaneous determination of individual cationic surfactants (alkyl benzyl dimethyl ammonium chlorides) in surface water samples has been developed. We describe this methodology for the first time: it involves the application of solid phase extraction (SPE – for sample preparation) coupled with ion chromatography–conductivity detection (IC-CD – for the final determination). Mean recoveries of...
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The mechanical properties and conduction of solid polyurethane electrolytes depending on the methods of synthesis and LiClO4 content as addition
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Determination of antifreeze substances in the airport runoff waters by solid-phase microextraction and gas chromatography–mass spectrometry method
PublicationA new method has been developed for the determination of antifreeze agents such as ethylene glycol (EG), propylene glycol (PG), and diethylene glycol (DEG) in the samples of airport runoff water. The method is based on headspace solid–phase microextraction (HS–SPME) of target analytes, which is coupled with gas chromatography–mass spectrometry (GC–MS). Until now, there was a lack of appropriate methodology for collecting reliable...
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Synthesis, structure and application of a new class of Tr-podands derived in phase-transfer catalysis
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Tuning the extraction properties of ionogel-coated Solid-phase microextraction fibers based on the solvation properties of the ionic liquids
PublicationA silica-based network was used to immobilize ionic liquid-based ionogels and applied as a fiber coating forsolid-phase microextraction (SPME). The ionogels were prepared by a sol–gel process, using two ionic liquids,triethylsulfonium bis(trifluoromethylsulfonyl)imide ([Set3][TFSI]) and 1-butyl-1-methylpiperidinium bis(tri-fluoromethylsulfonyl)imide ([C4C1Pip][TFSI]), as well as their equimolar mixture. Methyltrimethoxysilane wasused...
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Headspace Solid-Phase Microextraction Coupled with Gas Chromatography–Mass Spectrometry for the Determination of Volatile Organic Compounds in Urine
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Silicon polypodands: powerful metal cation complexing agents and solid–liquid phase-transfer catalysts of new generation
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Solid phase extraction clean up of soil and sediment extracts for the determination of various types of pollutants in a single run.
PublicationOpisano nową procedurę oczyszczania ekstraktów rozpuszczalnikowych (uzyskanych w trakcie obróbki próbek gleby i osadów dennych) z wykorzystaniem techniki ekstrakcji do fazy stałej. Oryginalność podejścia polega na znalezieniu takiej kombinacji sorbentów, że uzyskuje się ekstrakt przygotowany do analizy chromatograficznej na zawartość różnych typów zanieczyszczeń (polichlorowane bifenyle, wielopierścieniowe węglowodory aromatyczne,...
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Development of headspace solid-phase microextraction-gas chromatography method for the determination of solvent residues in edible oils and pharmaceuticals
PublicationW pracy przedstawiono wyniki opracowania procedury oznaczania pozostałości rozpuszczalników organicznych w olejach jadalnych z wykorzystaniem techniki HS-SPME na etapie izolacji i wzbogacania analitów. Przedstawiono proces optymalizacji etapu izolacji i rozdzielenia związków. Dla każdego z analitów wyznaczono parametry walidacyjne charakteryzujące procedurę tj. granice wykrywalności, granicę oznaczalności, liniowość, zakres pomiarowy,...
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ALTERNATIVE, DIRECT SYNTHESIS METHOD OF THE CERAMIC SOLID SOLUTIONS BASED ON BaTiO3 THROUGH A HIGH ENERGY BALL MILLING
PublicationPolycrystalline samples BaTiO3 and the solid solutions Ba0.9Sr0.1TiO3, Ba0.9Sr0.1Ti0.9Sn0.1O3, Ba0.9Sr0.1Ti0.8Sn0.2O3 were obtained by means of a mechanochemical treatment based on the high-energy ball milling technique and next a high temperature solid state reaction method. The influence of synthesis condition on microstructural, dielectric and ferroelectric properties of obtained solid solutions were investigated. The structure...
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Determination of volatile organic compounds in water samples using membrane-solid phase microextraction (M-SPME) (headspace version)
PublicationThe results of a study on the use of membrane-solid phase microextraction (M-SPME) for sampling volatile organic compounds (VOCs) from the headspace above the liquid medium are presented. The sampled VOCs were subsequently quantified by gas chromatography (GC). Two systems were compared in this study, i.e. a novel two-phase sorption system (M-SPME), and a commercial fibre. Headspace sampling using SPME was optimized with respect...
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Miniaturized Solid Phase Extraction techniques for different kind of pollutants analysis: State of the art and future perspectives – PART 1
PublicationSolid Phase Extraction (SPE) has been practiced in a modern form for more than half a century. It was constantly developing, driven by the analysts needs. These needs are coming from the importance to select an appropriate analytical method, which should have satisfactory accuracy, precision and sensitivity. In the case of sorbent-based microextraction techniques, the choice of miniaturized variants that meet these requirements...
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Application of response surface methodology to optimize solid-phase microextraction procedure for chromatographic determination of aroma-active monoterpenes in berries
PublicationMost of scientific papers concern the qualitative or semi-quantitative analysis of aroma-active terpenes in liquid food matrices. Therefore, the procedure based on solid-phase microextraction and comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry for determination of monoterpenes in fresh berries was developed. The optimal extraction conditions using divinylbenzene-carboxen-polydimethylsiloxane fiber...
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Ionogel sorbent coatings for determining organophosphorus and pyrethroid insecticides in water and fresh juice samples by headspace-solid phase microextraction
PublicationThe sol–gel method yielded three different ionogel sorbent coatings that were obtained based on a silica material containing ionic liquids (ILs) immobilized in its pores. Two ILs, triethylsulfonium bis(trifluoromethylsulfonyl) imide [Set3][TFSI] and 1-butyl-1-methylpiperidinium bis(trifluoromethylsulfonyl)imide [C4C1Pip][TFSI], as well as their equimolar mixture [Set3/C4C1Pip], were used to obtain ionogel fibers. The developed...
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New Green Determination of Cu, Fe, Mn, and Zn in Beetroot Juices along with Their Chemical Fractionation by Solid-Phase Extraction
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The quantification of bisphenols and their analogues in wastewaters and surface water by an improved solid-phase extraction gas chromatography/mass spectrometry method
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Preparation and evaluation of solid-phase microextraction fibres based on functionalized latex nanoparticle coatings for trace analysis of inorganic anions
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A simple graphene-based pipette tip solid-phase extraction of malondialdehyde from human plasma and its determination by spectrofluorometry
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New approach based on solid-phase extraction for the assessment of organic compound pollutions in so-called pharmaceutically pure water
PublicationOpisano mozliwość zastosowania nowej procedury analitycznej opartej na wykorzystaniu techniki ekstrakcji do fazy stałej (na etapie izolacji i wzbogacania analitów) do oznaczania śladowych ilości zanieczyszczeń organicznych w wodzie specjalnej czystości używanej do celów farmaceutycznych.Próbka badanej wody jest przepuszczana przez złoże sorbenta, które jest osuszane za pomocą strumienia oczyszczonego powietrza, przed etapem termicznej...
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Estimation of platinum in environmental water samples with solid phase extraction technique using inductively coupled plasma mass spectrometry
PublicationZoptymalizowano metodykę oznaczania śladowych poziomów stężeń platyny (IV) w oparciu o technikę ekstrakcji do fazy stałej w połączeniu ze spektrometrią mas z plazmą wzbudzoną indukcyjnie. Na etapie wzbogacania platyny wykorzystano żel krzemionkowy modyfikowany grupami aminopropylowymi. Ilościowy odzysk platyny uzyskano poprzez wykorzystanie 1.0 mol L-1 roztworu tiomocznika jako eluenta. Odchylenie standardowe wyników (RSD) było...
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Evaluation of solid phase extraction for downstream separation of propane-1,3-diol and butan-1-ol from fermentation broth
PublicationGlycerol is mainly a by-product of fat splitting and biodiesel production. This study examined the use of chemically modified silica gels for downstream separation of propane-1,3-diol and butan-1-ol from fermentation broths obtained through the glycerol fermentation process. The developed method was found to be simple and efficient for the isolation and purification of butan-1-ol from the other components in the fermentation mixture....
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Determination of volatile aliphatic amines in air by solid phase microex traction coupled with gas chromatography with flame ionization detection.
PublicationOpisano nową metodę oznaczania lotnych amin alifatycznych w powietrzu. Metodyka oparta jest na zastosowaniu techniki mikroekstrakcji do fazy stacjonarnej na etapie pobierania próbek oraz zestawu GC-FID do rozdzielania i oznaczania poszczególnych analitów.Badaniom poddano nowe typy faz stacjonarnych.Zbadano wpływ wilgotności powietrza na proces pobierania próbek analitów z powietrza.
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Miniaturized solid phase extraction techniques for different kind of pollutants analysis: State of the art and future perspectives – PART 2
PublicationDetermination of pollutants present in environmental samples at a low concentration level very often requires the analytical protocol that includes analytes isolation and/or enrichment prior to the final quantification. Miniaturized SPE offers an interesting alternative to LLE. Nowadays, many types of sorbents are available and can be used as selective materials for extraction of varied analytes in different kinds of samples. The...
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Structure and electrical properties of ceramic proton conductors obtained with molten-salt and solid-state synthesis methods
PublicationPublikacja omawia wyniki badań niobanu lantanu domieszkowanego akceptorowo pod kątem właściwości elektrycznych i strukturalnych.
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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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Matrix solid-phase dispersion (MSPD) as simple and useful sample preparation technique for determination of polybrominated diphenyl ethers (PBDEs) in dust
PublicationIn the present study a novel analytical procedure for the determination of polybrominated diphenylethers in dust samples was developed.The main aim of the research was the selection of the optimum conditions of the matrix solid-phasedispersion before thefinal determination of polybrominated diphenyl ethers in dust samples. In order toassess the best usefulness of this technique, a favourable ratio of sample amount to the mass ofdispersing...
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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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Simultaneous Determination of Indolic Compounds in Plant Extracts by Solid-Phase Extraction and High-Performance Liquid Chromatography with UV and Fluorescence Detection
PublicationA high-performance liquid chromatographic method with UV and fluorescence detection (HPLC-DAD-FLD) was developed for simultaneous determination of indolic compounds in plant material. Indole-3-carbinol (I3C), indole-3-acetic acid (I3AA), indole-3-acetonitrile (I3ACN), and 3,3′-diindolylmethane (DIM) were used as representative compounds that cover a wide spectrum of indole structures occurring in nature. For concentration and purification...
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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...