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Search results for: chromatographic analysis
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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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Current trends in analytical strategies for the determination of polybrominated diphenyl ethers (PBDEs) in samples with different matrix compositions – Part 2: New approaches to PBDEs determination
PublicationHerein, we review the latest technical solutions for polybrominated diphenyl ethers (PBDEs) determination in samples with different matrix compositions, largely focusing on gas chromatography but also presenting some liquid chromatography–based solutions. Moreover, we discuss the use of diverse sample injection techniques while considering the advantages and disadvantages of each injection system in the context of PBDEs analysis....
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New Polymeric Materials for Solid Phase Extraction
PublicationSolid phase extraction (SPE) is a popular sample preparation technique, which can be applied directly in gas–solid phase and liquid–solid phase, or indirectly to solid samples by using, e.g., thermodesorption with subsequent chromatographic analysis. Although SPE can be described as a physical extraction process involving a liquid phase and a solid phase, the increased use of packed sorbent formats seems to have led to a bias toward...
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Pharmaceutical and forensic drug applications of chiral supercritical fluid chromatography
PublicationTHE SUPERCRITICAL FLUID IS AN EXCELLENT CHOICE AS THE CHROMATOGRAPHIC MOBILE PHASE BECAUSE IT ALLOWS RAPID SEPARATION WITH HIGH EFFICIENCY AND APPLICATIONS INVOLVING ENANTIORESOLUTION ARE COMMON. SUPERCRITICAL FLUID CHROMATOGRAPHY (SFC) IS INCREASINGLY USED FOR ANALYTICAL, SEMI-PREPARATIVE AND PREPARATIVE PURIFICATION OF CHIRAL COMPOUNDS, INCLUDING PRODUCTION OF ENANTIOMERS THAT ARE MAINLY ENCOUNTERED DURING DRUG DEVELOPMENT. SFC...
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Molecularly imprinted polymers based on deep eutectic solvents as a greenest materials for selective extraction of emerging contaminants from complex samples
PublicationSome of the reagents applied in the synthesis of molecularly imprinted polymers (MIPs) may impact on health and the environment. Thus, a new generation of promising green chemicals are nowadays introduced and investigated, including deep eutectic solvents (DESs). DESs seems to be a reasonable choice as they are characterized as non-toxic, low cost, easy to prepare and biodegradable chemicals. This review presents the information...
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Lab-in-syringe as a practical technique for automatic microextraction: Evaluation by Blue Applicability Grade Index
PublicationLab-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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Advances in mass spectrometry for iron speciation in plants
PublicationIron is an important nutrient essential for plants and critical for human health. The state-of-the art of methods for iron speciation in cereal grains and plant fluids is critically reviewed. Particular attention is given to the latest developments in the coupling of HPLC with the parallel ICP MS and electrospray ionization (ESI) MS/MS detection, usually QTOF MS or Q-Orbitrap MS, for the identification and quantification of iron...
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The role of centrifugal partition chromatography in the removal of β-asarone from Acorus calamus essential oil
PublicationΒ-asarone is a phenylpropane derivative present in the rhizomes of Acorus calamus, that was proved to exhibit toxic effects in humans. Because of its presence the whole plant that is commonly used in traditional medicine for its sedative, anti-inflammatory, neuroprotective and other properties has limited application nowadays. In the study, qualitative and quantitative analysis of a collection of nine essential oil (EO) samples...
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Determination of flavanols by liquid chromatography with fluorescence detection. Application to the characterization of cranberry-based pharmaceuticals through profiling and fingerprinting approaches
PublicationIn this work, a new method based on reversed-phase high-performance liquid chromatography (HPLC) with fluorescence detection (FLD) was established for the determination of catechins and related oligomeric proanthocyanidins (PACs) in cranberry-based pharmaceuticals. Compounds were recovered by liquid extraction using methanol/water/hydrochloric acid (60:39:1, v:v:v) as the extraction solvent. The chromatographic separation was carried...
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Improvement of derivatized amino acid detection sensitivity in micellar electrokinetic capillary chromatography by means of acid-induced pH-mediated stacking technique
PublicationDerivatization is a frequently used sample prepara-tion procedure applicable to the enhancement of analyte de-tection sensitivity. Amino acids mostly require derivatization prior to electrophoretic or chromatographic analysis, especial-ly if spectrophotometric detection is used. This study presents an on-line preconcentration technique for derivatized amino acids. The sensitivity of the method was improved by the utilization of...
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Light-Modulated Sunscreen Mechanism in the Retina of the Human Eye
PublicationThe functioning of the human eye in the extreme range of light intensity requires a combination of the high sensitivity of photoreceptors with their photostability. Here, we identify a regulatory mechanism based on dynamic modulation of light absorption by xanthophylls in the retina, realized by reorientation of pigment molecules induced by trans–cis photoisomerization. We explore this photochemically switchable system using chromatographic...
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Analytical and legislative challenges of sewage sludge processing and management
PublicationThis article presents the most popular methods of sewage sludge management and analytical techniques which could be a powerful tool in designing new sewage sludge management methods. Chemical analysis is also described as a vital point at the subsequent stages of technological processes control and sewage sludge quality assessment. It is also an instrument essential to maintaining control of processed sewage sludge introduced to...
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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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Determination of trace levels of eleven bisphenol A analogues in human blood serum by high performance liquid chromatography–tandem mass spectrometry
PublicationChemicals showing structural or functional similarity to bisphenol A (BPA), commonly called BPA analogues, have recently drawn scientific attention due to their common industrial and commercial application as a substitute for BPA. In the European Union, the use of BPA has been severely restricted by law due to its endocrine disrupting properties. Unfortunately, it seems that all BPA analogues show comparable biological activity,...
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House dust as a source of analytical information on concentration of polybrominated diphenyl ethers (PBDEs) - first approach
PublicationPolybrominated diphenyl ethers (PBDEs), which are best recognized as flame retardants, were in 2001, by virtue of Stockholm Convention, listed in a group of Persistent Organic Compounds (POPs). Increasing concentration levels of PBDEs, reported in human tissues (e.g., blood, serum, breast milk, etc.) haverecently caught worldwide concern due to their potential tendency to disrupt thyroid hormones, neurobehavioral deficits and endocrine...
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Development of a solventless stir bar sorptive extraction/thermal desorption large volume injection capillary gas chromatographic-mass spectrometric method for ultra-trace determination of pyrethroids pesticides in river and tap water samples
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Evaluation of polycaprolactone as a new sorbent coating for determination of polar organic compounds in water samples using membrane–SPME
PublicationCommercially available solid-phase microextraction fibers used for isolation of polar analytes are based on the adsorption phenomenon. In consequence, typical limitations bonded with analytes displacement and matrix effects are very frequent. In the present study, alternative solution is described. Polycaprolactone (PCL) was used for the first time as sorbent to isolate polar organic compounds from water samples using the membrane–solid-phase...
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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.
PublicationLotne 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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DETERMINATION OF SURFACTANTS IN ENVIRONMENTAL SAMPLES - PART I. CATIONIC COMPOUNDS = Oznaczanie Surfaktantów W Próbkach Środowiskowych. Część I. Związki Kationowe
PublicationCompounds from the group of cationic surfactants are widely applied in household, industrial, cleaning, disinfectant, cosmetic and pharmaceutical products as their specific properties (antimicrobial, emulsifying, anticorrosion, softening). After use, cationic surfactants are disposed to wastewater-treatment plants and finally with effluent water to surface waters due to their incomplete degradation. Moreover, they can freely circulate...
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Determination of Glycerol, Propylene Glycol, and Nicotine as the Main Components in Refill Liquids for Electronic Cigarettes
PublicationRefill liquids for electronic cigarettes are an important area of research due to the health safety and quality control of such products. A method was developed for the determination of glycerol, propylene glycol, and nicotine in refill liquids using liquid chromatography, coupled with tandem mass spectrometry (LC-MS/MS) in multiple reaction monitoring (MRM) mode with electrospray ionisation (ESI). Sample preparation was based...
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Understanding the origin of high corrosion inhibition efficiency of bee products towards aluminium alloys in alkaline environments
PublicationVarious bee products were found to be efficient corrosion inhibitors of aluminium in different environments. In particular, bee pollen was found to be highly effective in alkaline electrolytes, yet its highly complex composition and possible synergistic interactions hinder determination of the compounds acting as active corrosion inhibitors. The main purpose of the following work is to investigate the effect of solvents used for...
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Green aspects, developments and perspectives of liquid phase microextraction techniques
PublicationDetermination of analytes at trace levels in complex samples (e.g. biological or contaminated water or soils) are often required for the environmental assessment and monitoring as well as for scientific research in the field of environmental pollution. A limited number of analytical techniques are sensitive enough for the direct determination of trace components in samples and, because of that, a preliminary step of the analyte...
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Environmental problems and health risks with disposable baby diapers: Monitoring of toxic compounds by application of analytical techniques and need of education
PublicationDue to the widespread use of disposable diapers in healthy babies as well as children prone to allergiesand premature babies with reduced immunity, disposable diapers should only be made of non-toxic andnatural ingredients. Unfortunately, disposable diaper manufacturers are reluctant to present their exactchemical composition, claiming that their trade secrets apply. However, several reports show thatdisposable diapers of well-known...
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Milena Marycz dr inż.
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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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Determination of polybrominated diphenyl ethers in house dust using standard addition method and gas chromatography with electron capture and mass spectrometric detection
PublicationMonitoring of the environmental fate of polybrominated diphenyl ethers (PBDEs) involves determination of their concentration in air, airborne particles and settled dust. This requires the implementation of appropriate analytical tools like measuring instruments, reference materials and analytical procedures. In this study an analytical procedure was developed for determining PBDEs in samples with a complex matrix composition. The...
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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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Application of the MSPD Technique for the HPLC Analysis of Rutin in Sambucus nigra L.: The Linear Correlation of the Matrix Solid-Phase Dispersion Process
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Application of a commercially available derivatization instrument and commonly used reagents to HPLC on-line determination of antioxidants
PublicationThis study demonstrates the potential of a commercially available derivatization instrument coupled with HPLC for separation and on-line determination of antioxidants detected with widely used screening reagents - DPPH (2,2-diphenyl-1-picrylhydrazyl), ABTS (2,2'-azino-bis(3-ethylbenzthiazoline-6-sulphonic acid) or FCR (Folin-Ciocalteu's phenol reagent ). As the result of optimization, key parameters of the analytical procedure,...
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Drug-Eluting Biopsy Needle as a Novel Strategy for Antimicrobial Prophylaxis in Transrectal Prostate Biopsy
PublicationOBJECTIVES: To preclinically evaluate drug-eluting biopsy needles (patent pending WO2016118026) as a new potential way of antimicrobial prophylaxis for transrectal prostate biopsy. METHODS: Twenty steel biopsy needles have been coated with polyvinyl alcohol, ciprofloxacin, and amikacin. Modified biopsy needles have been randomly divided into 3 groups (1:2:1 ratio). Needles from group I were immersed for 30 minutes in dedicated...
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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
PublicationHydrophilic 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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Transportable, Portable and Micro Gas Chromatographs
PublicationSignificant benefits can be obtained by miniaturization of conventional benchtop gas chromatographs. The attractive features arising from miniaturization include low-power requirements, low heat capacity of separation columns, low consumption of mobile phase, enhanced performance, higher portability, and easily coupling to detectors and secondary chromatographic systems. In separation sciences, including gas phase separations,...
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Common methods for the chiral determination of amphetamine and related compounds I. Gas, liquid and thin-layer chromatography
PublicationThis article reviews the most common, useful methods for the chiral determination of amphetamine (AM) and AM-deriveddesigner drugs in different of matrix, including blood, hair, urine, medicaments or standard solutions, taking into considerationarticles published in the past 15 years. We consider chromatographic methods (e.g., gas, liquid, high-performance liquid, and thinlayer). We describe several types of chiral derivatization...
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Determination of the chemical structure of potencial organic impurities occuring in the drug substance opopramol
PublicationThe tricyclic antipsychotic and antidepressant drug opipramol was examined with regard to the chemical structure of its organic impurities. Impurities were isolated from the technical product by chromatographic methods and their chemical structures were estabilished by HMNR, MS and FTIR.
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Jacek Namieśnik prof. dr hab. inż.
PeopleScientific discipline: chemistryRector in 2016-2019 He was born on 10 December, 1949 in Mogilno. He graduated in 1972 at the Faculty of Chemistry at Gdańsk University of Technology, obtaining a master's degree in chemical engineering. In 1972 he started working at Gdańsk University of Technology, where in 1978 he defended his doctoral thesis and in 1985 he completed his habilitation. He was appointed an associate professor in 1991...
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State of the art and prospects of methods for determination of lipophilicity of chemical compounds
PublicationLipophilicity of the compounds is useful to (i) explain their distribution in biological systems, which is different in plant and in animal organisms, (ii) predict the possible pathways of pollutant transport in the environment, and (iii) support drug discovery process and select optimal composition in terms of bioactivity and bioavailability. The lipophilic properties can be determined by two main approaches, experimental, which...
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Distinction of citrus fruits based on their volatile composition using the electronic nose
PublicationThe aim of the study was to analyze the volatile fraction of the citrus fruit using an electronic nose device integrated with ultrafast gas chromatography. The subjects were Citrus aurantifolia, Fortunella margarita Swingle and Citrus × floridana. The chromatographic data obtained were analyzed by means of chemometric methods: PCA and SQC. On the basis of the charts obtained, it is possible to distinguish the fruits tested on the...
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Liquid chromatography techniques for separation of flavonoids from Droseraceae
PublicationFlavonoids which are presented in insectivorous plants of the Droseraceae family have wide range of advantageous properties i.e. an antioxidant, anti-inflammatory and antimicrobial activities, antitumor activity was reported as well.The purpose of the research was to develop the most favourable conditions for liquid chromatographic separation and identification of myricetin and quercetin in extracts of insectivorous plants. In...
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Comparison of classical and modern approach of determination of highly polar compounds by High Performance Liquid Chromatography coupled with Tandem Mass Spectrometry
PublicationAbstract: Sugars and sugar alcohols are known as highly polar compounds. Four analytes were taken into consideration for comparison of classical and modern approach of separation of highly polar substances. Mannitol was chosen as an example of simple sugar alcohol, sucrose and lactulose as examples of disaccharides and structural isomers, raffinose as an example of complex trisaccharide. Raffinose was also used as internal standard...
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IZOLACJA I IDENTYFIKACJA NATURALNYCH SUBSTANCJI BARWIĄCYCH OBECNYCH W PRÓBKACH FARB ARTYSTYCZNYCH I TKANINACH POCHODZENIA HISTORYCZNEGO
PublicationNatural organic dyes are group of substances that belong to various types of chemical compounds. The most commonly used in paintings and dyeing textiles were naturally occurring dyestuffs from group of anthraquinones, flavones and indigoid dyes. Identification of coloring substances present in historical artistic paints provides relevant information for a wide range of specialists dealing with works of art and in the field of conservation science....
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Simple method for preparation of Dialkyl (2,3-dihydro-1,3-thiazol-2-yl)-phosphonates
PublicationAbstract A simple synthesis of dialkyl (2,3-dihydro-1,3-thiazol-2-yl)-phosphonates from thiazoliumsalts and trialkyl phosphites is described. The series of dialkyl (2,3-dihydro-1,3-thiazol-2-yl)-phosphonates with various substituents in positions 3, 4, and 5 of the thiazole ring wereprepared. However, only phosphonates with an aryl on the nitrogen atom were stable enoughfor chromatographic purification, although all the new phosphonates...
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Developments in Green Chromatography
PublicationGreen analytical chemistry is a widely recognized concept that has led to the development of new analytical methods with reduced environmental impact and minimized analyst occupational exposure. Achievements include the development of microextraction, ultrasound-assisted extraction (UAE), and microwave-assisted extraction (MAE) techniques. Research towards greener separation processes focuses on the elimination of toxic solvents...
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Quality evaluation of agricultural distillates using different types of electronic noses
PublicationThe paper presents the results of investigation on quality evaluation of agricultural distillates using a prototype of electronic nose instrument and a commercial electronic nose of Fast/Flash GC type – HERACLES II. The prototype was equipped with TGS type semiconductor sensors. HERACLES II included two chromatographic columns with different polarity of stationary phase and two FID detectors. In case of the prototype volatile fraction...
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Retention modeling of some saccharides separated on an amino column.
PublicationUsing an amino column (Supelcosil LC-NH2) and different mixtures of acetonitrile-water, quantitative structure-retention relationship models are discussed. These models are based on computed molecular descriptors representing numerically structured features of some saccharides. The obtained results are underlining the lipophilicity/hydrophilicity balance, and how this is controlling the separation of the saccharides. The resulting...
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Novel amides of mycophenolic acid and some heterocyclic derivatives as immunosuppressive agents
PublicationThe group of new amide derivatives of mycophenolic acid (MPA) and selected heterocyclic amines was synthesised as potential immunosuppressive agents functioning as inosine-5'-monophosphate dehydrogenase (IMPDH) uncompetitive inhibitors. The synthesis employed uronium-type activating system (TBTU/HOBt/DIPEA) while or phosphonic acid anhydride method (T3P/Py) facilitating amides to be obtained in moderate to excellent yields without...
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“Dilute & Shoot” approach for rapid determination of trace amounts of nicotine in zero-level e-liquids by reversed phase liquid chromatography and hydrophilic interactions liquid chromatography coupled with tandem mass spectrometry-electrospray ionization
PublicationTwo analytical procedures are proposed where HILIC and RPLC techniques are coupled with tandem mass spectrometry detection for rapid determination of trace amounts of nicotine in zero-level liquids for electronic cigarettes. Samples are prepared on the basis of the approach “dilute & shoot” which makes this important step quick and not complicated. The chromatographic separation was carried out on a Zorbax XDB column (RPLC method)...
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The occurence and diagnosis of biomarkers of ethyl alcohol consumption
PublicationEthyl alcohol is a legal and a widely available psychoactive drug. However, its excessive consumption causes addiction. This leads to aggressive behaviors, family battery, difficulties in interpersonal relations, legal offences, suicides, car accidents and deterioration in labor productivity, what causes financial problems. Despite many social actions against alcohol consumption, this problem is still unresolved. Therefore, fast...
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Determination of SCFAs in water using GC-FID. Selection of the separation system
PublicationIn the present study, an analytical procedure was developed for the determination of short-chain fatty acids (SCFAs) in landfill leachate and municipal wastewater employing injection of aqueous samples to gas chromatograph with flame ionization detector (GC-FID). Chromatographic conditions such as a separation system, injection volume, oven temperature program were investigated and selected. With two columns, one with a polar (polyethylene...
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Ion Chromatography with Pulsed Amperometric Detection for Determining Cyanide in Urine and Meconium Samples
PublicationThe parents’ addictions and eating habits have a significant influence on the child’s growth. The first stool of a newborn baby provides a large amount of information about xenobiotics transmitted by the mother’s body. The analytical technique used in the study is ion chromatography with pulsed amperometric detection (IC-PAD). The biological samples, which were obtained from women staying in a maternity ward and their partners,...
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Novel stationary phases based on asphaltenes for gas chromatography
PublicationWe present the results of investigations on the possibility of the application of the asphaltene fraction isolated from the oxidized residue from vacuum distillation of crude oil as a stationary phase for gas chromatography. The results of the investigation revealed that the asphaltene stationary phases can find use for the separation of a wide range of volatile organic compounds. The experimental values of Rohrschneider/McReynolds...