{"title":"Mesoporous Silica With Covalently Immobilized Anthracene As Adsorbent For SPE Recovery Of PAHs Pollutants From Highly Lipidic Solutions","authors":"Albina Mikhraliieva, R. Gonçalves, V. Zaitsev","doi":"10.26434/chemrxiv.13394228.v1","DOIUrl":"https://doi.org/10.26434/chemrxiv.13394228.v1","url":null,"abstract":"Two samples of functionalized mesoporous silica containing anchored anthrylmethylamine groups (SiO2-Ant) have been prepared by surface assembling (1) and one step silane immobilization (2). Both adsorbents can be attributed to bimodal balanced hydrophobic-hydrophilic adsorbents with loading of anthracene groups about 15-33 %. The adsorbents have been used for solid-phase extraction (SPE) of anthracene from organic solvents (acetonitrile, acetone and heptane) and model solutions of lipids (myristic acid and vegetable oil). The obtained results were compared with commercial C18 SPE cartridge. While C18 cartridge recovers anthracene from water-containing media (acetonitrile/water, 1/1), SiO2-Ant cartridges much more efficient in extraction of anthracene from non-polar solvent (heptane). Lipids macrocomponents such as myristic acid and vegetable oil do not decrease the dynamic adsorption capacity and recovery of the model polycyclic aromatic hydrocarbon (PAH) on SiO2-Ant. It was demonstrated that π-π stacking interaction with the analyte determine the selectivity of SiO2-Ant towards of anthracene. This makes SiO2-Ant attractive for selective preconcentration of PAHs from high lipid content objects, such as vegetable oils.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2020-12-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46147220","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
M. Blazheyevskiy, Y. Scrypynets, A. Yegorova, V. Antonovich
{"title":"The Oxidative Derivatization Method For The Spectrofluorimetric Determination Of Periciazine In Pharmaceutical Preparations","authors":"M. Blazheyevskiy, Y. Scrypynets, A. Yegorova, V. Antonovich","doi":"10.17721/moca.2020.21-26","DOIUrl":"https://doi.org/10.17721/moca.2020.21-26","url":null,"abstract":"The oxidative derivatization method for the indirect spectrofluorimetric determination of Periciazine has been presented. Potassium hydrogenperoxymonosulfate (Oxone ®) is proposed as a derivatizing agent for Periciazine, yielding the strongly fluorescent Periciazine sulfoxide. A highly sensitive, simple and rapid method for determination of the Periciazine by fluorescence of its oxidation product with Oxone ® solution in 0.02 M hydrochloric acid solution (λex = 364 nm; λem = 444 nm) has been developed. The calibration plot is linear in concentration range of 0.05 – 4.00 µg mL -1 . LOQ (10S) is 0.05 µg mL -1 . The possibility of quantitative determination of Periciazine in pharmaceutical preparations (Neuleptil ®, 10 mg capsules and Neuleptil ®, a 30 mL 4 % oral (solution) drops) has been shown RSD < 2.2 % (δ < RSD).","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67435405","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Hayat E.L.Ouafy, T. E. Ouafy, M. Oubenali, M. Mbarki, M. Echajia
{"title":"Evaluation Of Carbon Paste Electrode Modified With Heavy Metals For The Analysis Of Paracetamol By Voltammetry And Impedance Spectroscopy","authors":"Hayat E.L.Ouafy, T. E. Ouafy, M. Oubenali, M. Mbarki, M. Echajia","doi":"10.17721/moca.2020.93-99","DOIUrl":"https://doi.org/10.17721/moca.2020.93-99","url":null,"abstract":"The present document reports on the electrocatalytic activity of heavy metals (Copper(II), Nickel(II), Manganese(II) and Lead(II)) modified carbon paste electrodes (HM/CPE) for the paracetamol (Pr) oxidation where its results are compared with carbon paste electrode. The voltammetric behavior of Pr is explored where a sensitive anodic peak has appeared at about 0.27 V (vs. Ag/AgCl/3 M KCl) in 0.1 M Na2SO4 (pH 12). This peak results from the irreversible oxidation of Pr at HM/CPE surface. The catalytic effect was evaluated using cyclic and square wave voltammetry. Electrochemical impedance spectroscopy also confirms our experimental results as the HM/CPE shows the least charge transfer resistance. Also, HM/ CPE can be utilized successfully to ameliorate the electroanalysis of Pr at very weak concentration with excellent sensitivity. The calibration curves were linear from 6.0 · 10-5 to 8.0 · 10-4 mol L-1. The detection limits were found approaching 10-9 mol L-1. Then, the proposed method was applied to detect Pr in river water samples with satisfactory results.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67435479","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
V. Vasylechko, V. Fedorenko, O. Gromyko, G. Gryshchouk, Y. Kalychak, S. Tistechok, I. Us, A. Tupys
{"title":"Sorption Preconcentration Of Silver For Atomic Absorption Analysis And Antibacterial Properties Of The Acid-Modified Clinoptilolite – Ag Composite","authors":"V. Vasylechko, V. Fedorenko, O. Gromyko, G. Gryshchouk, Y. Kalychak, S. Tistechok, I. Us, A. Tupys","doi":"10.17721/moca.2020.73-82","DOIUrl":"https://doi.org/10.17721/moca.2020.73-82","url":null,"abstract":"Sorptive properties of the acid-modified Transcarpathian clinoptilolite towards Ag(I) were studied under dynamic conditions. It was found that the most effective acid-modifier is 1 M HNO3 solution. The sorption capacity value of H-clinoptilolite under the optimal conditions is 6.15 mg of Ag per 1 g of zeolite. The solid-phase extraction procedure with acid-modified clinoptilolite was used to pre-concentrate trace amounts of silver ions in aqueous solutions and then finally to determine them by the atomic absorption method. Due to the acceptable recoveries (≥ 98 %) and RSD values (2.3-4.7 %) for tap and lake water, the developed method can be successfully applied for the determination of trace amounts of silver ions in the presence of major components of water. It was established that the initial form of clinoptilolite has a better antibacterial effect against E. coli than the H-form. However, antagonistic activity against S. aureus was lower than against E. coli in both forms. The combination of different forms of clinoptilolite with Ag(I) increases their antibacterial activity.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67435744","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
P. Rydchuk, O. Tymoshuk, L. Oleksiv, T. Chaban, V. Matiychuk
{"title":"Voltammetric Determination Of Pt(IV) Using 5-Hydroxyimino-4- Imino-1,3-Thiazolidine-2-One","authors":"P. Rydchuk, O. Tymoshuk, L. Oleksiv, T. Chaban, V. Matiychuk","doi":"10.17721/moca.2019.130-139","DOIUrl":"https://doi.org/10.17721/moca.2019.130-139","url":null,"abstract":"5-Hydroxyimino-4-imino-1,3-thiazolidine-2-one has been suggested as a new organic reagent for the voltammetric determination of platinum. The optimal conditions of Pt(IV) voltammetric determination using 5-hydroxyimino-4- imino-1,3-thiazolidine-2-one on the peak of catalytic hydrogen currents have been determined: the background electrolyte is 0.3 M NaCl, pH of the solution is 2.0, 50-fold concentration excess of organic reagent. The sensitive method of Pt(IV) voltammetric determination was developed (LOD = 4.1·10-9 М). The range of determinable contents covers two concentration orders. The selectivity of the developed methods have been studied towards concomitant metals ions. The accuracy of the developed method has been tested on model solutions using “added-found” method. The method has been approved during the analysis of a real sample, viz. the catalyst for oxidation of exhaust gases of the car “Chevrolet”.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2019-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67434243","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Monitoring And Distribution Of Organochlorine Pesticides, Polychlorinated Biphenyls And Polycyclic Aromatic Hydrocarbons In Surface River Water And Suspended Particulate Matter","authors":"M. Milyukin, M. Gorban, M. M. Skrynnyk","doi":"10.17721/moca.2019.117-129","DOIUrl":"https://doi.org/10.17721/moca.2019.117-129","url":null,"abstract":"The monitoring results of organochlorine pesticides (OCPs), polychlorinated biphenyls (PCBs) and polycyclic aromatic hydrocarbons (PAHs) in Ukranian and world surface river waters were summarized. Total concentrations of OCPs, PCBs and PAHs in surface waters of Ukrainian rivers (Dnieper and Dniester) were 1.4–17.1; 2.8–57.2; 7.5–378.6 ng/dm3 , respectively. These pollution levels are medium on a global scale. Higher concentrations were recorded in the surface water of China, India and other Asian countries. Distribution of these organic ecotoxicants between water and suspended particulate matter (dispersionphase distribution) was analyzed and it was shown that in the majority of river waters ≥50% of them are associated with suspended particles. By the case of River Dnieper antibate correlations between watersoluble parts of individual OCPs, PCBs and PAHs and coefficient of their hydrophobicity were recorded. These correlations were presented graphically. In addition, relevant correlation coefficients and criterions of probability were calculated. The clearest correlation was established for PCBs.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2019-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67434146","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
E. A. Reshetnyak, N. Nemets, O. Chernyshova, A. Panteleimonov, V. M. Ostrovskaya
{"title":"Visual Binary Testing Of Hydrogen Sulfide Dissolved In Return Underground Local-Water Of Oil And Gas Condensate Fields","authors":"E. A. Reshetnyak, N. Nemets, O. Chernyshova, A. Panteleimonov, V. M. Ostrovskaya","doi":"10.17721/moca.2019.146-152","DOIUrl":"https://doi.org/10.17721/moca.2019.146-152","url":null,"abstract":"In order to screen samples of return underground local-water of oil and gas condensate fields for the presence of dissolved hydrogen sulfide, it was proposed to use single comparison sample for visual binary testing of H2S. Two indicator reactions occurring in solutions were selected — the formation of a stabilized suspension of MnS and CdS. Suspensions prepared in the presence of borate buffer (pH 9.18) and gelatin (stabilizer) are stable during the twenty four hours; a difference in the turbidity of suspensions can be observed near the normalized concentration of hydrogen sulfide (сlim = 15 mg L-1). When establishing the concentration of H2S in the comparison samples, a statistical approach was applied; the estimated values of the threshold concentration of H2S (ccomp.) are less than the normalized level on the value which providing the risk of a false-negative test result not more than 5% - 11.6 mg L-1 for MnS and 13.4 mg L-1 for CdS. Preference was given to a test system based on a stabilized suspension of CdS, because for this reaction, a narrower interval of unreliability and the value of ccomp. is nearer to the value of the сlim. The correctness of the visual binary testing of H2S in the samples of the analyzed water was confirmed by spectrophotometric method with p-phenylenediamine.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2019-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67434775","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
O. Bayer, O. Kaminska, L. Shevchenko, V. Mykhalska, О.М. Stupak, O. V. Bondarets, Yu.V. Dobrozhan
{"title":"Development And Evaluation Of The Suitability Of The Method For Determining The Content Of Egg Coccidiostatics Using Ultra Performance Liquid Chromatography - Tandem Mass Spectrometry (UPLC-MS/MS)","authors":"O. Bayer, O. Kaminska, L. Shevchenko, V. Mykhalska, О.М. Stupak, O. V. Bondarets, Yu.V. Dobrozhan","doi":"10.17721/MOCA.2019.43-51","DOIUrl":"https://doi.org/10.17721/MOCA.2019.43-51","url":null,"abstract":"The conducted studies assessed the suitability of the method of ultra performance liquid chromatography - tandem mass spectrometry (UPLC-MS/MS) and established the MS/MS detection parameters and determined its validation characteristics for the analysis of residual content of coccidiostatics in food eggs. It has been proved that this method is accurate, practical and universal, which is confirmed by the data of ССα for amprolium – 2.14 μg/kg, diclazuril – 2.37 μg/kg, monensin – 2.34 μg/kg, narazin – 2.28 μg/kg, semduramicin – 2.23 μg/kg, toltrazuril 2.5 – μg/kg, salinomycin – 3.32 μg/kg, halofuginone – 6.18 μg/kg, maduramycin – 13.06 μg/kg, decoquinate – 2.37 μg/kg, robenidine – 26.06 μg/kg, nicarbazine – 316.7 μg/kg, percentage of return is 92.4 – 111 %. The results obtained for assessing the suitability, accuracy and reproducibility of the results meet the requirements of the European Directives.The developed method allows to detect residual amounts of about 12 coccidiostatics that are used in poultry for the prevention of coccidiosis.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2019-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67435017","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Y. Khomenko, L. Ishchenko, V. Ishchenko, S. Midyk, D. Y. Rybalchenko, V. Ushkalov, V. Spyrydonov
{"title":"Development Of ELISA Kit For Detection Of Glyphosate-Resistant Genetically Modified Soybean","authors":"Y. Khomenko, L. Ishchenko, V. Ishchenko, S. Midyk, D. Y. Rybalchenko, V. Ushkalov, V. Spyrydonov","doi":"10.17721/MOCA.2019.21-29","DOIUrl":"https://doi.org/10.17721/MOCA.2019.21-29","url":null,"abstract":"The goal of research was development of competitive ELISA kit for detection of genetically modified plants resistant to glyphosate. As the source for gene isolation we have used leaves of GM soybean RoundUp Ready, line 40-3-2 (Monsanto). Using polymerase chain reaction the gene encoding the enzyme 5-enolpiruvilshykimat-3-phosphate synthase (CP4 EPSPS) was isolated, which provides resistance to the herbicide glyphosate. Isolated gene has been cloned into plasmid vector pET24(a), creating genetic construct pET-CP4EPSPS. E.coli (BL 21(DE3)) has been transformed by genetic construct and over expressed after induction by 0.5 mM IPTG. Recombinant enzyme CP4 EPSPS with molecular weight 45 kD was purified as inclusion bodies and used as antigen for 96-well polystyrene plates immobilization. Monoclonal antibodies CP4 EPSPS mAb3 (Artron BioResearch Inc., Canada) was used for synthesis of horseradish peroxidase conjugate and receiving diagnostic reagent. We have shown that in the competitive ELISA we can detect at least 0.1% of GM plants resistant to glyphosate, on the example of soybean (line RR 40-3-2), moreover we can also detect rapeseed (line GT73) and sugar beet (line H7-1).","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2019-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67435029","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Girish Tigari, J. G. Manjunatha, D. Ravishankar, G. Siddaraju
{"title":"Enhanced Electrochemical Determination Of Riboflavin In Biological And Pharmaceutical Samples At Poly (Arginine) Modified Carbon Paste Electrode","authors":"Girish Tigari, J. G. Manjunatha, D. Ravishankar, G. Siddaraju","doi":"10.17721/moca.2019.216-223","DOIUrl":"https://doi.org/10.17721/moca.2019.216-223","url":null,"abstract":"An electrogenerated Polyarginine modified carbon paste electrode (PAMCPE) was fabricated through a simple electropolymerization procedure. The devised electrode was characterized by cyclic voltammetry (CV) and Field Emission Scanning Electron Microscopy (FESEM). This electrode was utilized for electrocatalytic estimation of Riboflavin (RF) and its instantaneous resolution with ascorbic acid (AA) and folic acid (FA) in phosphate buffer solution (PBS) of pH 6.0 by differential pulse voltammetry (DPV). It was observed to be a very responsive electrode for the electrochemical detection and quantification of RF. It was revealed that PAMCPE generates higher current response towards RF contrast to the bare carbon paste electrode (BCPE). Under optimized condition, the RF oxidation current values were linearly reliant on the RF concentration increment with a limit of detection (LOD) of 9.3·10-8 M using DPV. The stable PAMCPE was effectively applied for estimation of RF in B-complex pill and complex human blood serum samples.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2019-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67435318","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}