Pub Date : 2021-01-01DOI: 10.17721/moca.2021.81-87
Hayat El Ouafy, T. E. Ouafy, M. Oubenali, A. Haimouti, A. Gamouh, M. Mbarki
In this work, the electro-catalytic oxidation of ibuprofen was studied using aluminum oxide supported on clay (Clay/Al2O3). The latter has been successfully prepared by impregnating aluminum particles in the clay by heat treatment. The electro-catalytic performances of Clay/Al2O3 for the oxidation of ibuprofen were studied using cyclic voltammetry (CV), chronoamperometry, and differential pulse voltammetry (DPV) in 0.1 mol L-1 of the phosphate buffer (pH = 7). It has been shown that the proposed catalyst exhibits remarkably an electro-catalytic effect performance vis-a-vis the oxidation of ibuprofen. In addition, the peak oxidation currents depend linearly on the ibuprofen concentration in the wide ranges from 1.0·10-3 mol L-1 to 1.0·10-6 mol L-1 with a detection limit of 1.95·10-8 mol L-1 and response time of 30 second. Possible interferences were evaluated in 1.0·10-5 mol L-1 ibuprofen. The proposed catalyst also indicated suitable repeatability and stability. Besides, the proposed CPE-Clay/Al2O3 has been successfully applied for ibuprofen analysis in human blood with good recoveries.
{"title":"Electrocatalytic Effect of Al2O3 Supported on Clay in Oxidizing of Ibuprofen at Graphite Electrode","authors":"Hayat El Ouafy, T. E. Ouafy, M. Oubenali, A. Haimouti, A. Gamouh, M. Mbarki","doi":"10.17721/moca.2021.81-87","DOIUrl":"https://doi.org/10.17721/moca.2021.81-87","url":null,"abstract":"In this work, the electro-catalytic oxidation of ibuprofen was studied using aluminum oxide supported on clay (Clay/Al2O3). The latter has been successfully prepared by impregnating aluminum particles in the clay by heat treatment. The electro-catalytic performances of Clay/Al2O3 for the oxidation of ibuprofen were studied using cyclic voltammetry (CV), chronoamperometry, and differential pulse voltammetry (DPV) in 0.1 mol L-1 of the phosphate buffer (pH = 7). It has been shown that the proposed catalyst exhibits remarkably an electro-catalytic effect performance vis-a-vis the oxidation of ibuprofen. In addition, the peak oxidation currents depend linearly on the ibuprofen concentration in the wide ranges from 1.0·10-3 mol L-1 to 1.0·10-6 mol L-1 with a detection limit of 1.95·10-8 mol L-1 and response time of 30 second. Possible interferences were evaluated in 1.0·10-5 mol L-1 ibuprofen. The proposed catalyst also indicated suitable repeatability and stability. Besides, the proposed CPE-Clay/Al2O3 has been successfully applied for ibuprofen analysis in human blood with good recoveries.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"1 1","pages":""},"PeriodicalIF":0.7,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67436161","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}
Pub Date : 2020-12-21DOI: 10.26434/chemrxiv.13394228.v1
Albina Mikhraliieva, R. Gonçalves, V. Zaitsev
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.
{"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":"1 1","pages":""},"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}
Pub Date : 2020-01-01DOI: 10.17721/moca.2020.21-26
M. Blazheyevskiy, Y. Scrypynets, A. Yegorova, V. Antonovich
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).
建立了氧化衍生化间接荧光光谱法测定哌嗪的方法。氢过氧单硫酸氢钾(Oxone®)被提出作为Periciazine的衍生化剂，生成强荧光Periciazine亚砜。用Oxone®溶液在0.02 M盐酸溶液中(λex = 364 nm;λem = 444 nm)。校正图在0.05 ~ 4.00µg mL -1浓度范围内呈线性关系。定量限(10S)为0.05µg mL -1。定量测定药物制剂(Neuleptil®，10 mg胶囊和Neuleptil®，30 mL 4%口服(溶液)滴剂)中哌嗪的可能性显示RSD < 2.2% (δ < RSD)。
{"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":"1 1","pages":""},"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}
Pub Date : 2020-01-01DOI: 10.17721/moca.2020.93-99
Hayat E.L.Ouafy, T. E. Ouafy, M. Oubenali, M. Mbarki, M. Echajia
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.
本文报道了重金属(铜(II)、镍(II)、锰(II)和铅(II))修饰的碳糊电极(HM/CPE)对扑热息痛(Pr)氧化的电催化活性，并将其结果与碳糊电极进行了比较。在0.1 M Na2SO4 (pH 12)中，Pr的伏安行为在0.27 V (vs. Ag/AgCl/3 M KCl)处出现了一个敏感的阳极峰。这个峰是由HM/CPE表面Pr的不可逆氧化引起的。用循环伏安法和方波伏安法评价了催化效果。电化学阻抗谱也证实了我们的实验结果，HM/CPE表现出最小的电荷转移电阻。此外，HM/ CPE还能以优异的灵敏度改善极弱浓度下的Pr电分析。标定曲线在6.0·10-5 ~ 8.0·10-4 mol L-1范围内呈线性关系。检出限接近10-9 mol L-1。将该方法应用于河流水样中Pr的检测，结果令人满意。
{"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":"1 1","pages":""},"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}
Pub Date : 2020-01-01DOI: 10.17721/moca.2020.73-82
V. Vasylechko, V. Fedorenko, O. Gromyko, G. Gryshchouk, Y. Kalychak, S. Tistechok, I. Us, A. Tupys
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.
在动态条件下研究了酸改性的喀尔巴阡斜沸石对Ag(I)的吸附性能。结果表明，1 M HNO3溶液是最有效的酸调节剂。在最佳条件下，h -斜沸石对银的吸附量为6.15 mg / 1g。采用酸改性斜沸石固相萃取法对水溶液中痕量银离子进行预富集，最后用原子吸收法测定。自来水和湖水的回收率≥98%，RSD值为2.3 ~ 4.7%，可用于自来水和湖水中主要成分中痕量银离子的测定。结果表明，斜发沸石初始形态对大肠杆菌的抑菌效果优于h型。然而，对金黄色葡萄球菌的拮抗活性低于对大肠杆菌的拮抗活性。不同形态的斜沸石与Ag(I)的结合提高了其抗菌活性。
{"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":"1 1","pages":""},"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}
Pub Date : 2019-01-01DOI: 10.17721/moca.2019.130-139
P. Rydchuk, O. Tymoshuk, L. Oleksiv, T. Chaban, V. Matiychuk
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”.
5-羟基亚胺-4-亚胺-1,3-噻唑烷-2-酮被认为是一种新的有机伏安法测定铂的试剂。确定了催化氢电流峰上5-羟基亚胺-4-亚胺-1,3-噻唑烷-2- 1伏安法测定Pt(IV)的最佳条件:背景电解质为0.3 M NaCl，溶液pH为2.0，有机试剂过量浓度为50倍。建立了灵敏的铂(IV)伏安法测定方法(LOD = 4.1·10-9 М)。可测定含量范围包括两个浓度顺序。研究了所开发方法对伴生金属离子的选择性。用“加-求”法在模型解上验证了该方法的准确性。该方法在实际样品分析中得到了认可，即“雪佛兰”汽车废气氧化催化剂。
{"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":"1 1","pages":""},"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}
Pub Date : 2019-01-01DOI: 10.17721/moca.2019.117-129
M. Milyukin, M. Gorban, M. M. Skrynnyk
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.
{"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":"1 1","pages":""},"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}
Pub Date : 2019-01-01DOI: 10.17721/moca.2019.146-152
E. A. Reshetnyak, N. Nemets, O. Chernyshova, A. Panteleimonov, V. M. Ostrovskaya
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.
为了筛选油气凝析田地下回水样品中是否存在溶解硫化氢，提出了采用单比对样品对H2S进行视觉二元检测的方法。选择溶液中发生的两种指示反应-形成稳定的MnS和CdS悬浮液。在硼酸缓冲液(pH 9.18)和明胶(稳定剂)存在下制备的悬浮液在24小时内是稳定的;在硫化氢归一化浓度(с m m = 15 mg L-1)附近，可以观察到悬浮液浊度的差异。在确定比较样品中H2S的浓度时，采用统计学方法;H2S (ccomp.)阈值的估计值小于该值的标准化水平，该值提供假阴性测试结果的风险不超过5% - MnS为11.6 mg L-1, cd为13.4 mg L-1。优先考虑基于稳定的cd悬浮液的测试系统，因为对于这种反应，不可靠的区间和ccomp值较窄。是更接近于价值的。用对苯二胺分光光度法对分析水样品中H2S进行目测二元检测的正确性进行了验证。
{"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":"1 1","pages":""},"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}
Pub Date : 2019-01-01DOI: 10.17721/MOCA.2019.43-51
O. Bayer, O. Kaminska, L. Shevchenko, V. Mykhalska, О.М. Stupak, O. V. Bondarets, Yu.V. Dobrozhan
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.
{"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":"1 1","pages":""},"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}
Pub Date : 2019-01-01DOI: 10.17721/MOCA.2019.21-29
Y. Khomenko, L. Ishchenko, V. Ishchenko, S. Midyk, D. Y. Rybalchenko, V. Ushkalov, V. Spyrydonov
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).
{"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":"25 1","pages":""},"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}
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