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Achiral–chiral LC/LC–FLD coupling for determination of carvedilol in plasma samples for bioequivalence purposes

(Elsevier , 2007)
Medvedovici, Andrei
;
Albu, Florin
;
Georgita, Cristina
;
Sora, Daniela Iuliana
;
Galaon, Toma
;
Udrescu, Stefan
;
David, Victor
Bioequivalence data for two pharmaceutical formulations (solid oral dosage forms) containing carvedilol is presented for both racemic and enantiomers of the active substance. This was achieved by on-line coupling of two liquid chromatographic separations followed by fluorescence detection. The first LC dimension was used for a fast separation of racemic carvedilol from propranolol (IS) and the endogenous matrix, by means of a reversed phase mechanism. The peak of racemic carvedilol was on-line transferred to the second enantioselective LC dimension, based on a reversed phase separation on cellulose tris(3,5-dimethyl-phenylcarbamate) stationary phase. Both stages were monitored over a single run by means of a fluorescence detector operated at an excitation wavelength of 285 nm and an emission wavelength of 355 nm. Automated shortcutting of the racemic carvedilol peak to the chiral column and simultaneous detection over the two LC dimensions have been obtained by using an experimental set-up based on two six-port rotative switching valves. Linearity was demonstrated on the interval 2–150 ng/mL for racemic carvedilol and on 1–75 ng/mL intervals for enantiomers. LLOQ fits between 0.7 and 1.4 ng/mL. Recoveries of the target compounds are 87±4 and 81±4% for the IS. Precision ranged from 0.6 to 2.5% and the mean accuracy obtained on quality control samples (measured as % bias) over the whole study falls between −0.8 and 6.3%.
5
Assay of free captopril in human plasma as monobromobimane derivative, using RPLC/ (+)ESI/MS/MS: validation aspects and bioequivalence evaluation

(John Wiley & Sons, Ltd , 2009)
Medvedovici, Andrei
;
Albu, Florin
;
Sora, Daniela Iuliana
;
Udrescu, Stefan
;
Galaon, Toma
;
David, Victor
A sensitive method for determination of free captopril as monobromobimane derivative in plasma samples is discussed. The internal standard (IS) was 5-methoxy-1H-benzimidazole-2-thiol. Derivatization with monobromobimane immediately after blood collection and plasma preparation prevents oxidation of captopril to the corresponding disulfide compound and enhances the ionization yield. Consequently, derivatization enhances sample stability and detection sensitivity. Addition of the internal standard was made immediately after plasma preparation. The internal standard was also derivatized by monobromobimane, as it contains a thiol functional group. Preparation of plasma samples containing captopril and IS derivatives was based upon protein precipitation through addition of acetonitrile, in a volumetric ratio 1:2. The reversed-phase liquid chromatographic separation was achieved on a rapid resolution cartridge Zorbax SB-C18, monitored through positive electrospray ionization and tandem MS detection using the multiple-reaction monitoring mode. Transitions were 408–362 amu for the captopril derivative and 371–260 amu for the internal standard derivative. The kinetics of captopril oxidation to the corresponding disulfide compound in plasma matrix was also studied using the proposed method. A linear log–log calibration was obtained over the concentration interval 2.5–750 ng/mL. A low limit of quantitation in the 2.5 ng/mL range was obtained. The analytical method was fully validated and successfully applied in a three-way, three-period, single-dose (50 mg), block-randomized bioequivalence study for two pharmaceutical formulations (captopril LPH 25 and 50 mg) against the comparator Capoten 50 mg.
The coating of n[SiO1.5-(CH2)3(NH2)] ultrathin layers on the surface of Fe3O4 nanoparticles and the analysis of their coating dynamics

(INOE : [Bucharest] , 2008)
Zamora Iordache, Petrisor
;
Somoghi, Vasile
;
Petrea, Nicoleta
;
Mitru, Georgeta
;
Petre, Razvan
;
Dionezie, Bojin
;
Ordeanu, Viorel
;
Kim, Lidia
;
Mutihac, Lucia
This paper presents the unitary and controlled synthesis of nanostructures of the type Fe3O4-n[SiO1.5-(CH2)3(NH2)]-Snθ [Fe3O4 = magnetic core; n[SiO1.5-(CH2)3(NH2)] = coating layer; -NH2 = layer made up of groups which play an important part in biochemical interface; Snθ = exterior layer of biochemical cross-linked molecules]. The purpose of obtaining these nanostructures is to fix Fe3O4-n[SiO1.5-(CH2)3(NH2)]-Snθ on microorganism surface through covalent chemical bounds in order to determine them in magnetic field, as a function of the mass and volume of the microorganisms attached to the nanostructures. The nanocomposite materials with physical and chemical features induced in a controlled way in the basic physical structure in order to handle in a controlled manner the host structures, constitute a research field of current interest. The nanostructures we have drawn up are also important in fields connected to chemistry, such as: selective/unselective chemical separation, molecular macrocomplexes labeling, chemical/biological detection media and others.
2 96
Determination of nimesulide and its active metabolite in plasma samples based on solvent deproteinization and HPLC-DAD analysis

(Editura Academiei Romane , 2007)
Sora, Iulia
;
Galaon, Toma
;
David, Victor
;
Medvedovici, Andrei
A selective, sensitive and accurate HPLC method for the assay of nimesulide and its major metabolite (4’-hydroxynimesulide) in human plasma samples is presented. The sample preparation procedure was based on a simple protein precipitation with acetonitrile. The reversed phase liquid chromatography was used as separation technique followed by UV detection of analytes at 300 nm. Separation was achieved on a Chromolith Performance RP 18e column using a mobile phase consisting of aqueous 0.2% triethylamine at pH 3.0 with H3PO4 and methanol (1:1, v/v). A small volume of plasma is required for the sample preparation procedure (200 μL), nitrazepam being used as internal standard. The limits of quantification for nimesulide and 4’-hydroxy-nimesulide are 64 ng/mL and 41 ng/mL, respectively. Relative standard deviations characterizing intra-day and inter-day precision were less than 5%. The validated method was applied during a bioavailability study for a pharmaceutical formulation containing nimesulide (uncoated tablet) available on the Romanian market. Both nimesulide and 4’-hydroxy-nimesulide were determined from the real human plasma samples obtained from 22 volunteers, included in this study, after the administration of a single oral dose.
2 106
Deviation from van’t Hoff dependence in RPLC induced by tautomeric interconversion observed for four compounds

(WILEY-VCH Verlag GmbH & Co , 2011)
Galaon, Toma
;
David, Victor
The most encountered situations in reversed-phase liquid chromatography for temperature dependence of retention are those obeying the linear equation known as the van’t Hoff plot. When studying compounds that are involved in structural modifications, it is likely that the temperature dependences of their retention factors do not follow this rule. It is the aim of this paper to report some particular cases when compounds involved in tautomeric interconversion have a different retention behavior with temperature: a deviation from the linearity of ln k on 1/T, or, in certain temperature ranges, temperature increase leading to a retention increase. Examples of compounds exhibiting deviation from the van’t Hoff temperature dependence are piroxicam, drotaverine, vincamine, and epivincamine. A simple thermodynamic model relying on tautomeric equilibria in mobile phase is proposed for these compounds, which gives a polynomial dependence between ln k and 1/T.
4
Effect of counterion on the mesomorphic behavior and optical properties of columnar pyridinium ionic liquid crystals derived from 4-hydroxypyridine

(Elsevier B.V. , 2015)
Pana, Amalia
;
Badea, Florentina Laura
;
Ilis, Monica
;
Staicu, Teodora
;
Micutz, Marin
;
Pasuk, Iuliana
;
Circu, Viorel
A series of 3,4,5-tridodecyloxybenzyl pyridinium salts derived from 4-hydroxypyridine has been designed and prepared. The liquid crystalline properties of these compounds were investigated by polarized optical microscopy, differential scanning calorimetry and powder X-ray diffraction while their thermal stability was studied by thermogravimetric analysis. The N-3,4,5-tridodecyloxybenzyl-4-pyridone intermediate shows a monotropic columnar hexagonal mesophase ranging from 56 C down to room temperature while the corresponding bromide dodecyl O-alkylated pyridinium salt shows one enantiotropic columnar mesophase and one additional monotropic columnar phase at lower temperatures. Replacing bromide ion (Br ) with other counterions (NO 3 ; BF 4 and PF 6 ) resulted in mesophase suppression. These luminescent pyridinium salts show weak emission in dichloromethane solutions at room temperature and a pronounced red-shifted emission in solid state. Photoluminescent properties of the pyridinium salts do not depend significantly on the nature of counterion employed.
10
Effects of large volume injection of aliphatic alcohols as sample diluents on the retention of low hydrophobic solutes in reversed-phase liquid chromatography

(Elsevier , 2014)
David, Victor
;
Galaon, Toma
;
Aboul-Enein, Hassan
Recent studies showed that injection of large volume of hydrophobic solvents used as sample diluents could be applied in reversed-phase liquid chromatography (RP-LC). This study reports a systematic research focused on the influence of a series of aliphatic alcohols (from methanol to 1-octanol) on the retention process in RP-LC, when large volumes of sample are injected on the column. Several model analytes with low hydrophobic character were studied by RP-LC process, for mobile phases containing methanol or acetonitrile as organic modifiers in different proportions with aqueous component. It was found that starting with 1-butanol, the aliphatic alcohols can be used as sample solvents and they can be injected in high volumes, but they may influence the retention factor and peak shape of the dissolved solutes. The dependence of the retention factor of the studied analytes on the injection volume of these alcohols is linear, with a decrease of its value as the sample volume is increased. The retention process in case of injecting up to 200 L of upper alcohols is dependent also on the content of the organic modifier (methanol or acetonitrile) in mobile phase.
1
Ethanol and methanol sensing characteristics of Nb-doped TiO2 porous thin films

(WILEY-VCH Verlag GmbH & Co , 2011)
Dediu, Violeta
;
Schoonman, Joop
;
Musat, Viorica
Undoped and Nb-doped TiO2 porous thin films have been obtained through a sol–gel method using analytical grades Ti(OiC3H7)4 and Nb(OC2H5)5 as precursors. The morphology, crystalline microstructure, and the sensing properties towards ethanol and methanol of the obtained thin films have been investigated. The effects of the dopant on the film morphology and on alcohol sensing properties are discussed. Both direct current (DC) and alternating current (AC) measurements were performed at different temperatures in methanol and ethanol ambients to better understand the mechanisms of the alcohol detection. In the presence of a small amount of Nb, the activation energy for electrical conduction decreased. Nb doping improves the selectivity for methanol in the temperature range of 300–400 8C. The Nyquist diagrams showed complex phenomena during alcohol detection.
2
Extraction and transport behaviour of aromatic amino acids by modified cyclodextrin

(Taylor & Francis , 2009)
Kim, Lidia
;
Stancu, Ana Delia
;
Diacu, Elena
;
Buschmann, Hans-Jürgen
;
Mutihac, Lucia
The extraction efficiency together with the active transport assisted by the pH gradient trough liquid membrane of some aromatic native and derivative amino acids by using heptakis (2,3,6-tri-O-acetyl)-B-cyclodextrin as extractant agent or carrier has been studied. The modified cyclodextrin extracted aromatic amino acids, native (L-tryptophane, L-phenylalanine and L-tyrosine) and their methylester derivatives from aqueous phase into the organic phase. Moreover, the modified cyclodextrin exibits the carrier abilities for amino acid methylesters trough liquid membrane. In the case of transport processes involving liquid membranes, the physicochemical properties of the solvents play an important role in membrane stability. The results demonstrated that the inclusion properties of the investigated host are correlated with the structural properties of amino acid, and they also suggest further possibilities for optimal separation of amino acids derivatives.
4
Extraction behaviour of amino acid esters by functionalised calix[4]arenes

(Springer Science+Business Media , 2009)
Hamdi, Abdelwaheb
;
Souane, Rachid
;
Kim, Lidia
;
Abidi, Rym
;
Mutihac, Lucia
;
Vicens, Jacques
Calixarenes 2–4, 6 and 7 in the cone conformation variously substituted by acid or amido functions, glycolic chains and hydroxyl groups were synthesised. They have been used in extraction of native amino acid and amino acid esters.
13
Fast RPLC-UV method on short sub-two microns particles packed column for the assay of tenoxicam in plasma samples

(Elsevier , 2007)
Sora, Iulia
;
Galaon, Toma
;
Udrescu, Stefan
;
Negru, Jean
;
David, Victor
;
Medvedovici, Andrei
An extraction-less sample preparation technique followed by a RPLC-UV method on sub-two microns particles packed short column were used for the assay of tenoxicam in plasma samples. Protein precipitation was made by means of trichloroacetic acid addition. Supernatant was injected to the chromatographic column without any further pH adjustment. The mobile phase consisted in a mixture of acetonitrile and aqueous 0.1% phosphoric acid, at 2 mL/min flow rate and gradient elution. The Zorbax SB-C18® column (50mm length, 4.6mm internal diameter and 1.8 m particle size) was thermostated at 60 ◦C. The mobile phase gradient composition program allowed separation of tenoxicam and piroxicam (internal standard), column clean-up and re-equilibration within 4 min. UV detection was achieved at 368±10 nm. The method is characterized by a low limit of quantitation of 25 ng/mL for tenoxicam, with a linearity interval up to 5500 ng/mL. The use of a low volume detection cell and detector high frequency data acquisition rate produced high precision and accuracy through a whole bioequivalence study of tenoxicam in two commercially available tablet formulations, after a single oral administration dose. Full method validation is presented. The high throughput characteristic of the proposed method allowed full validation and bioanalytical study completion within a 96 h period.
3
High-throughput liquid-chromatography method with fluorescence detection for reciprocal determination of furosemide or norfloxacin in human plasma

(John Wiley & Sons, Ltd , 2007)
Galaon, Toma
;
Udrescu, Stefan
;
Sora, Iulia
;
David, Victor
;
Medvedovici, Andrei
A simple, high-throughput, highly selective and sensitive HPLC-FLD method for isolation and determination of furosemide and/or norfloxacin in human plasma samples following a simple organic solvent deproteinization step with acetonitrile as sample ‘clean-up’ procedure is reported. One of the two drug substances plays the internal standard role for the determination of the other. Separation of analyte and internal standard was achieved in less than 5.3 min (injection to injection) on a Chromolith Performance RP-18e column, using an aqueous component containing 0.015 mol/L sodium heptane-sulfonate and 0.2% triethylamine brought to pH = 2.5 with H3PO4. The composition of the mobile phase was: acetonitrile–methanol–aqueous component = 70:15:15 (v/v/v) and the flow-rate was set up to 3 mL/min. The chromatographic method applied to the determination of furosemide relies on fluorescent detection parameters of 235 nm for the excitation wavelength, and 402 nm for the emission wavelength. In case of norfloxacin, the excitation wavelength is set up to 268 nm and the emission wavelength is set up to 445 nm. The overall method leads to quantitation limits of about 27 ng/mL for furosemide, and 19.5 ng/mL for norfloxacin, using an injection volume of 250 μL. The method was applied to the bioequivalence study of two furosemide-containing formulations.
2
HPTLC identification of bioactive compounds and antioxidant activity of Pleurotus ostreatus and Lentinus edodes extracts

(University Politehnica of Bucharest, Romania , 2017)
Bubueanu, Corina
;
Grigore, Alice
;
Serban, Ecaterina Anca
;
Popa, Gabriela
;
Cornea, Petruta Calina
Because of the special flavour and of the therapeutic properties, Pleurotus ostreatus and Lentinus edodes are among the most cultivated and consumed mushrooms species. This work aimed to evaluate the antioxidant properties and free radical scavenger activities of Pleurotus ostreatus and Lentinus edodes methanol extracts by phosphomolybdenum and DPPH- assays respectively, total phenolic content (Folin – Ciocalteu) and identification of bioactive compounds by HPTLC (high-performance thin layer chromatography). The obtained fingerprints of extracts, in tree systems (for phenols, coumarins and triterpenoid saponins) have shown the presence of ferulic acid as main compounds in Pleurotus ostreatus extract and ergosterol (provitamin D2) in both of them. Total phenol content was 2.03 g/100g for Lentinus edodes extract and 1.24 g/100g for Pleurotus ostreatus extract. Radical scavenger activity and total antioxidant capacity, was higher for Lentinus edodes extract (90.14%, 203.05 mg AA) in comparison with the results obtained for Pleurotus ostreatus extract (85.32%, 168.34mg AA). The mushrooms examined in this work could represent important and accessible sources of natural antioxidants for food, food supplement and cosmetic industry.
5 109
Hydrophobicity parameter (log Kow) estimation for some phenolic compounds of pharmaceutical interest from retention studies with mobile phase composition in reversed‐phase liquid chromatography

(Taylor & Francis Group, LLC , 2008)
Galaon, Toma
;
Medvedovici, Andrei
;
David, Victor
Chromatographic retention of some phenolic compounds (impurities of related pharmaceutical active substances) was studied for different organic modifier contents in mobile phase. Their capacity factors k' versus organic modifier content (acetonitrile, or methanol) in mobile phase were measured and the corresponding dependences were studied by linear and polynomial regressions and then they were extrapolated to a mobile phase with no content in organic modifier in order to estimate their octanol/water partition coefficient (log Kow). The values of log Kow from retention data were compared to known shake-flask experimental values and theoretical values predicted by fragment methodology. Linear dependences for methanol and second-degree polynomial dependences for acetonitrile between organic modifier volume percentage and log k' provided good estimation of log Kow. The chromatographic method can be considered as a method of choice for estimating hydrophobicity parameter for different solutes. The linear dependence between extrapolated values of log k' for 0% organic modifier and log Kow estimated by means of fragment methodology for the model compounds can be used to predict chromatographic retention of other similar compounds.
7
Hypoglycosylated E-cadherin promotes the assembly of tight junctions through the recruitment of PP2A to adherens junctions

(Elsevier , 2010)
Nita-Lazar, Mihai
;
Rebustini, Ivan
;
Walker, Janice
;
Kukuruzinska, Maria A.
Epithelial cell–cell adhesion is controlled by multiprotein complexes that include E-cadherin-mediated adherens junctions (AJs) and ZO-1-containing tight junctions (TJs). Previously, we reported that reduction of E-cadherin N-glycosylation in normal and cancer cells promoted stabilization of AJs through changes in the composition and cytoskeletal association of E-cadherin scaffolds. Here, we show that enhanced interaction of hypoglycosylated E-cadherin-containing AJs with protein phosphatase 2A (PP2A) represents a mechanism for promoting TJ assembly. In MDCK cells, attenuation of cellular N-glycosylation with siRNA to DPAGT1, the first gene in the N-glycosylation pathway, reduced N-glycosylation of surface E-cadherin and resulted in increased recruitment of stabilizing proteins γ-catenin, α-catenin, vinculin and PP2A to AJs. Greater association of PP2A with AJs correlated with diminished binding of PP2A to ZO-1 and claudin-1 and with increased pools of serine-phosphorylated ZO-1 and claudin-1. More ZO-1 was found in complexes with occludin and claudin-1, and this corresponded to enhanced transepithelial resistance (TER), indicating physiological assembly of TJs. Similar maturation of AJs and TJs was detected after transfection of MDCK cells with the hypoglycosylated E-cadherin variant, V13. Our data indicate that E-cadherin N-glycans coordinate the maturity of AJs with the assembly of TJs by affecting the association of PP2A with these junctional complexes.
1
The influence of mobile phase flow-rate in RP-LC on thermodynamic parameters studied for polar compounds

(Taylor & Francis Group, LLC , 2011)
Galaon, Toma
;
Mihailciuc, Constantin
;
Medvedovici, Andrei
;
David, Victor
Thermodynamic parameters, such as standard enthalpy (DH0) and entropic contributions (DS0/R+volume phase ratio) of the partition between mobile and stationary phases, for several polar model compounds of pharmaceutical interest, were estimated in RP-LC for different flow-rates and using an octadecyl-silicagel stationary phase. The temperature range used to plot van’t Hoff curves was 25–50 C, which is the usual range for separation in RP-LC. Below 20 C, van’t Hoff plots become non-linear for all studied compounds, due to the changes of the balance between hydrophobic and solvophobic forces that influence the retention process. Other significant deviations were observed for one compound that is involved in inter-changeable tautomeric equilibria (as discussed for piroxicam). Regression parameters of the linear dependences obtained between retention (natural logarithm of retention factor, ln k’) and reciprocal absolute temperature (1=T) together with the estimated phase ratio were used to calculate the thermodynamic parameters of the model compounds. A slight variation was observed when flow-rate was changed within the interval from 0.6 to 2.0 mL=min. The enthalpy value decreased with increasing flow-rate up to a minimum at 1.4mL=min; at higher flow-rates these values increased slightly or remained constant.
1
The influence of mobile phase pH on the retention and selectivity of related basic compounds in reversed-phase liquid chromatography

(Editura Academiei Romane , 2012)
Galaon, Toma
;
David, Victor
Retention change with the pH of the mobile phase is shown for several basic compounds of pharmaceutical importance (drotaverine, ketotifen and chlorphenamine) and some of their related compounds. The partition model is used to explain the pH dependence of the retention for these compounds. Based on the experimental retention data, the dependence between the retention factor (k’) and pH of the mobile phase were plotted. Sigmoid shapes were obtained confirming thus the applied theoretical model. The pKa values were estimated for all the investigated compounds using the inflexion curve parameter. Comparison with theoretical pKa values obtained with specialized software leads to good correlation for some of the studied compounds.
3 150
Magnetite: From synthesis to applications

(Bentham Science Publishers , 2015)
Usoy, Gozde
;
Gunduz, Ufuk
;
Oprea, Ovidiu
;
Ficai, Denisa
;
Sonmez, Maria
;
Radulescu, Marius
;
Alexie, Mihaela
;
Ficai, Anton
In this review the synthesis, functionalization and some applications of magnetite nanoparticles (MNPs) were highlighted. It is our intention to highlight the correlations between the synthesis routes, related synthesis parameters, functionaliztion strategies and the properties expected for the materials containing MNPs. The uses of MNPs are strongly influenced by the properties of the materials. Therefore this review is trying to discuss the applications of the magnetite and magnetite based nanomaterials by taking into account all the factors that can influence the properties of the final materials and consequently their potential applications.
13
Mass spectrometric behavior of functionalized calix[4]arenes: the screening ability of host–guest complex formation with amino acid methyl esters

(Springer Science+Business Media , 2011)
Medvedovici, Andrei
;
Albu, Florin
;
Hamdi, Abdelwaheb
;
Souane, Rachid
;
Kim, Lidia
;
Mutihac, Lucia
;
Vicens, Jacques
The ESI–MS and MS/MS behavior of functionalized calix[4]arenes (1–5) has been studied in both positive and negative-ion mode. Liquid chromatography coupled to ESI–MS has been successfully used for separation of the byproducts issuing from the functionalization pathways, through the application of a simple reversed phase mechanism. The ability of (1–5) to host methyl esters of amino acids, tyrosine, tryptophan, phenylalanine, cysteine, valine, serine, leucine, isoleucine, and threonine has been evaluated by means of MS identification of the host– guest resulting in protonated molecular ions. The direct infusion within the ESI source of the solutions containing the two partners (i.e., calixarene and amino acid derivative) could act as a fast screening means for the evaluation of hosting capability. Only positive ionization may offer information about the host–guest complexes being formed. The influence of the excess of a partner in the infused solution strongly alters ionization yields, making quantitative approaches meaningless. Attempts to chromatographically isolate the host–guest complexes failed, probably due to the fact that interactions of the partners with the mobile and stationary phases are higher than the inclusion interactions. Structures consisting of combined fragments of the host–guest partners resulting from the collisional induced dissociation have not been observed.
2
Mercury determination in fish samples by flow injection using gold electrodes made from CD-R’s

(SYSCOM 18 SRL , 2011)
Cristea, Ionut
;
Radulescu, Maria Cristina
;
Ciomartan, Razvan
A new flow injection set up was developed for mercury determination by stripping chronopotentiometry. The FIA system was based on using solenoid valves controlled by a computer. A flow cell was manufactured with the gold working electrode made from a recordable compact disk (CD-R). The following operational parameters were studied and optimized: sample flow rate, time of mercury deposition by electrolysis on the electrode surface and current imposed for mercury dissolution off the working electrode. Mercury could be measured within 5 - 100 ng/mL domain at a deposition time of 180 s. Detection limit was 0.1 ng/mL at 600 s deposition time. RSD for a concentration of 40 ng/mL mercury was 1.04% (n=6) under optimal working conditions. . A concentration of 0.157±0.031μg mercury/g sample was found in a cod sample with this method. Recovery degree of a known amount of mercury introduced in the analyzed sample was 96.2%.
5 7

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