Papers by Pavel Nesterenko
SSRN, 2024
The retention regularities on a column packed with microspherical zeolite 13X particles were stud... more The retention regularities on a column packed with microspherical zeolite 13X particles were studied for different classes of compounds (alkanes, aromatic substances, oxygen-, nitrogen-, chlorine-, and sulfur-containing compounds) under conditions of normalphase high-performance liquid chromatography (NP HPLC) using methanol and acetonitrile as mobile phases. In general, the retention (logk') of studied substances having kinetic diameter less than zeolite pore size is proportional to their polarity. The retention of organic substances was compared for 13X and mesoporous silica columns. A special attention was paid to the retention of n-and iso-alcohols homologues, for which a clear molecular size effect was observed. It was found that retention factors (k') of solutes on 13X depend strongly on flow rate of the mobile phases indicating the presence of kinetic selectivity effect for the micrporous adsorbent. For the first time the baseline separation was obtained for the low homologues of n-alkanols. Also, the possibility of the separation of methanol and deuteromethanol is demonstrated with acetonitrile as the eluent.
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Journal of Chromatography Open, 2024
A new derivatization reagent, phthalylglycyl chloride (PG-Cl), for the analysis of urinary amino ... more A new derivatization reagent, phthalylglycyl chloride (PG-Cl), for the analysis of urinary amino acids was demonstrated using reversed-phase ultra-high performance liquid chromatography coupled to electrospray ionization-quadrupole-time-of-flight mass spectrometer. The study compares the limits of detection and quantification for different sample preparation techniques with the commonly used and effective method of derivatization using dansyl chloride. The stability of the derivatives was investigated, and the study includes an example of urinary amino acid analysis using PG-Cl derivatization. The optimal values for pH, temperature, and concentration of the derivatization reagent were established. Limits of quantification in the range of 0.5-500 µg/ mL were obtained for different amino acids. The possibility of phthalylglycyl chloride usage for non-target screening applications and targeted analysis of amino acids in urine was discussed. An advantages and issues of PG-Cl in comparison with commonly used acyl-chlorides (FMOC-Cl and DNS-Cl) provided and discussed.
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SSRN Electronic Journal, 2022
The silicon carbide and poly(butadiene-acrylonitrile) rubber (NBR) composite material was used fo... more The silicon carbide and poly(butadiene-acrylonitrile) rubber (NBR) composite material was used for the first time as adsorbent for gas-phase preconcentration of volatile hydrocarbons. The possibility of the preconcentration of n-alkanes and polyaromatic hydrocarbons from the air by using passive sampling on cartridges packed with this sorbent following by thermal desorptiongas chromatographic determination was demonstrated. The sorption rate of model substances from the air at room temperature and atmospheric pressure was studied. The optimum material for the storage and transportation of the collected samples was selected. The desorption efficiency of model compounds from the adsorbent was investigated. The result of thermo gravimetric analysis of the composite to provide the choice of temperature for the regeneration was given. Soil air at the oil field was analyzed using the developed method. The possibility of multiple use of the composite sorbent for analysis was demonstrated.
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Sorbtsionnye i khromatograficheskie protsessy., 2023
Inorganic zeolites or microporous crystalline aluminosilicates have high porosity, developed spec... more Inorganic zeolites or microporous crystalline aluminosilicates have high porosity, developed specific surface area, uniform pore size and ion exchange properties, which determines their molecular sieve and ad- sorption properties. The use of zeolites as catalysts, dryers of solvents and gases, and selective sorbents for the separation of low molecular weight compounds is widely known. Zeolites are widely used as fillers for chro- matographic columns in gas adsorption chromatography.Little is known about the use of zeolites in high-performance liquid chromatography (HPLC) and the mecha- nism of sorbate retention on these sorbents. Depending on the properties of sorbates, retention is determined by a combination of ion exchange, adsorption, molecular sieve effect, as well as kinetic selectivity. Due to solvation of the sorbent surface in HPLC, the thermodynamic parameters of the interaction of sorbates with zeolite change, the effective pore size decreases, and the diffusion of separated compounds into the pores of the sorbent becomes more difficult.Nevertheless, zeolites are promising adsorbents, since specific size (dpore) and the pore geometry of zeolites, as well as the possibility of selecting zeolites with a certain polarity, determines the high selectivity of the sepa- ration of low molecular weight compounds. Wide-pore zeolites with dpore (0.6-0.8 nm) with 8, 10, 12, and 14- membered ring channels are of greatest interest for HPLC.This review provides brief information about the classification, composition, structure of zeolites and their effect on their adsorption properties, as well as systematizes data on the use of zeolites in HPLC.
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Russian Journal of Physical Chemistry A, 1997
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Russian Journal of Physical Chemistry A, 1991
The diphilic sorbent based оп Silasorb is рrераrеd by аdsоrрtiоn and subsequent treatment with g... more The diphilic sorbent based оп Silasorb is рrераrеd by аdsоrрtiоn and subsequent treatment with glutaraldehyde and human sеrum albumin (HSA). Тhе chromatographic рrорегtiеs of the sorbent аrе studied. Its usefulness in analysis of medicinal preparations in biological fluids with direct sample injection onto the separating column is demonstrated
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Analytical Methods, 2013
ABSTRACT
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Analytical Methods, 2010
ABSTRACT A new chelation ion chromatographic system for the determination of transition metals wa... more ABSTRACT A new chelation ion chromatographic system for the determination of transition metals was developed. The isocratic separation of Fe2+, Fe3+ and Cu2+ simultaneously with Mn2+, Pb2+, Cd2+, Co2+, Zn2+ and Ni2+ was obtained on an iminodiacetic acid (IDA) functionalized silica column 150 × 4.0 mm i.d. with an optimized eluent composed of 2.5 mmol L−1 dipicolinic acid, 10 mmol L−1 HCl and 60% v/v of methanol at flow rate of 0.5 mL min−1. Post-column reaction with 4-(2-pyridylazo)resorcinol (PAR) was used for sensitive spectrophotometric detection at 510 nm of the separated metals at low ppb level. The applicability of the developed method to the analysis of fuelethanol was demonstrated.
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Analytical Chemistry, 2012
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Analytical and Bioanalytical Chemistry, 2010
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Analytical and Bioanalytical Chemistry, 2013
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Analytica Chimica Acta, 2013
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Analytica Chimica Acta, 2012
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Analytica Chimica Acta, 2012
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Analytica Chimica Acta, 2005
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Analytica Chimica Acta, 1994
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Analytica Chimica Acta, 2009
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Analytica Chimica Acta, 2006
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ACS Applied Materials & Interfaces, 2013
A novel hierarchical nanotemplated carbon monolithic rod (NTCM) was prepared using a novel facile... more A novel hierarchical nanotemplated carbon monolithic rod (NTCM) was prepared using a novel facile nanotemplating approach. The NTCM was obtained using C60-fullerene modified silica gels as hard templates, which were embedded in a phenolic resin containing a metal catalyst for localized graphitization, followed by bulk carbonization, and template and catalyst removal. TEM, SEM, and BET measurements revealed that NTCM possessed an integrated open hierarchical porous structure, with a trimodal pore distribution. This porous material also possessed a high mesopore volume and narrow mesopore size distribution. During the course of carbonization, the C60 conjugated to aminated silica was partly decomposed, leading to the formation of micropores. The Raman signature of NTCM was very similar to that of multiwalled carbon nanotubes as exemplified by three major peaks as commonly observed for other carbon materials, i.e., the sp3 and sp2 carbon phases coexisted in the sample. Surface area measurements were obtained using both nitrogen adsorption/desorption isotherms (BET) and with a methylene blue binding assay, with BET results showing the NTCM material possessed an average specific surface area of 435 m2 g(-1), compared to an area of 372 m2 g(-1) obtained using the methylene blue assay. Electrochemical studies using NTCM modified glassy carbon or boron doped diamond (BDD) electrodes displayed quasi-reversible oxidation/reduction with ferricyanide. In addition, the BDD electrode modified with NTCM was able to detect hydrogen peroxide with a detection limit of below 300 nM, whereas the pristine BDD electrode was not responsive to this target compound.
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Separations, 2023
The new scheme of the rapid preconcentration of volatile organic substances followed by the therm... more The new scheme of the rapid preconcentration of volatile organic substances followed by the thermodesorption and gas chromatographic determination by using a flame ionization detector is proposed for the analysis of air. The scheme implies a change in the geometry of the adsorbent layer in a column during the transition from adsorption to thermal desorption steps. The extraction of analytes is carried out in a wide tube, allowing quantitative adsorption at higher flow rates of the analyzed air passed through the magnetic sorbent held in a thin layer retained by a permanent magnet without any supporting frits. Novel magnetic adsorbents composed of magnetite or a zirconia/magnetite
core and pyrocarbon shell are developed for this application. At the end of the adsorption step, the magnet moved out of the system, and the adsorbent transferred under the gravity force into a narrow tube, which provides the more efficient heating of the adsorbent and minimal blurring of the analyte zones during the subsequent thermal desorption. The proposed scheme allows a significant reduction (approximately 10 times) of the time required for the preconcentration of analytes, which is illustrated by the GC determination of alcohols (butanol-1, pentanol-1), phenol, and o-cresol in the air.
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Papers by Pavel Nesterenko
core and pyrocarbon shell are developed for this application. At the end of the adsorption step, the magnet moved out of the system, and the adsorbent transferred under the gravity force into a narrow tube, which provides the more efficient heating of the adsorbent and minimal blurring of the analyte zones during the subsequent thermal desorption. The proposed scheme allows a significant reduction (approximately 10 times) of the time required for the preconcentration of analytes, which is illustrated by the GC determination of alcohols (butanol-1, pentanol-1), phenol, and o-cresol in the air.
core and pyrocarbon shell are developed for this application. At the end of the adsorption step, the magnet moved out of the system, and the adsorbent transferred under the gravity force into a narrow tube, which provides the more efficient heating of the adsorbent and minimal blurring of the analyte zones during the subsequent thermal desorption. The proposed scheme allows a significant reduction (approximately 10 times) of the time required for the preconcentration of analytes, which is illustrated by the GC determination of alcohols (butanol-1, pentanol-1), phenol, and o-cresol in the air.