Pub Date : 2019-02-28DOI: 10.33581/2520-257X-2019-1-45-50
Olga S. Scherbakova, Yuri V. Grigoriev, A. Zuraev, Inna Grigorieva, O. Ivashkevich
Optimization of the method for the synthesis of methylated poly-5-vinyltetrazole was carried out and it was shown that the process of its preparation, both with the homopolymer acrylonitrile and the commercially available copolymer with methyl acrylate and 2-acrylamido-2-methylpropane sulfonic acid, as starting materials, can be carried out in a single-step apparatus without intermediate release of poly-5-vinyltetrazole. At the same time, the resulting product is identical in composition, structure, and properties to that obtained using a two-stage process. Ability to refuse intermediate release of poly-5-vinyltetrazole allows to reduce the amount of dimethylformamide required for the preparation of methylated poly-5-vinyltetrazole twice, exclude the use of HCl solution from the process, and significantly reduce the time and energy costs of the process.
{"title":"Optimization of the method for synthesis of methylated poly-5-vinyltetrazole","authors":"Olga S. Scherbakova, Yuri V. Grigoriev, A. Zuraev, Inna Grigorieva, O. Ivashkevich","doi":"10.33581/2520-257X-2019-1-45-50","DOIUrl":"https://doi.org/10.33581/2520-257X-2019-1-45-50","url":null,"abstract":"Optimization of the method for the synthesis of methylated poly-5-vinyltetrazole was carried out and it was shown that the process of its preparation, both with the homopolymer acrylonitrile and the commercially available copolymer with methyl acrylate and 2-acrylamido-2-methylpropane sulfonic acid, as starting materials, can be carried out in a single-step apparatus without intermediate release of poly-5-vinyltetrazole. At the same time, the resulting product is identical in composition, structure, and properties to that obtained using a two-stage process. Ability to refuse intermediate release of poly-5-vinyltetrazole allows to reduce the amount of dimethylformamide required for the preparation of methylated poly-5-vinyltetrazole twice, exclude the use of HCl solution from the process, and significantly reduce the time and energy costs of the process.","PeriodicalId":17303,"journal":{"name":"Journal of the Belarusian State University. Chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87801804","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 : 2019-02-28DOI: 10.33581/2520-257X-2019-1-86-94
G. Shevchenko, V. Zhuravkov, N. P. Osipovich, G. V. Shishko
The possibility of Na2EDTA applying as a reducing and stabilizing reagent in aqueous medium to obtain gold hydrosols from hydrogen tetrachloroaurate was studied. It was found that, depending on the pH of the reaction medium, both nanosized precipitates (~60 nm) and gold hydrosols, consisting of spherical nanoparticles of uniform size (12–15 nm), can be obtained. Stable gold sols are formed at pH ≥ 10.5. Sol formation process rate depends on the temperature and concentration of Na2EDTA and increases with their increase. An electrochemical study of processes of HAuCl4 reduction and Na2EDTA oxidation showed that the possibility of gold hydrosols formation in an alkaline medium is due to the kinetic inhibition of the reduction process of gold hydroxo complexes formed during this process.
{"title":"Synthesis of gold hydrosols in the presence of Na2EDTA","authors":"G. Shevchenko, V. Zhuravkov, N. P. Osipovich, G. V. Shishko","doi":"10.33581/2520-257X-2019-1-86-94","DOIUrl":"https://doi.org/10.33581/2520-257X-2019-1-86-94","url":null,"abstract":"The possibility of Na2EDTA applying as a reducing and stabilizing reagent in aqueous medium to obtain gold hydrosols from hydrogen tetrachloroaurate was studied. It was found that, depending on the pH of the reaction medium, both nanosized precipitates (~60 nm) and gold hydrosols, consisting of spherical nanoparticles of uniform size (12–15 nm), can be obtained. Stable gold sols are formed at pH ≥ 10.5. Sol formation process rate depends on the temperature and concentration of Na2EDTA and increases with their increase. An electrochemical study of processes of HAuCl4 reduction and Na2EDTA oxidation showed that the possibility of gold hydrosols formation in an alkaline medium is due to the kinetic inhibition of the reduction process of gold hydroxo complexes formed during this process.","PeriodicalId":17303,"journal":{"name":"Journal of the Belarusian State University. Chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88313869","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 : 2019-02-21DOI: 10.33581/2520-257X-2019-1-51-58
Y. Matveichuk
UV spectrophotometric and chromatographic study of the distribution and hydration of trifluoroacetophenone (TFAF) and some its derivatives ( p-trifluoroacetyl benzoic acid heptyl ester (TFABAHE), p-methyltrifluoroacetophenone ( p-MTFAF), 2,4-dimethyltrifluoroacetophenone (DMTFAF), 2,4,6-trimethyltrifluoroacetophenone (TMTFAF)) in the hexane-water system, which models the polyvinyl chloride membrane of ion-selective electrodes was investigated. TFAF has a high solubility in water (distribution coefficient D is equal to 415) as compared with p-MTFAF, DMTFAF, TMTFAF and TFABAHE (D within 1360 –2700). Hydration occurs most strongly to TFABAHE and is especially strong in alkaline medium. It is established that p-MTFAF and TFABAHE form a crystalline hydrates.
{"title":"Investigation of hydration and distribution of trifluoroacetophenone and its derivatives in hexane – aqua system","authors":"Y. Matveichuk","doi":"10.33581/2520-257X-2019-1-51-58","DOIUrl":"https://doi.org/10.33581/2520-257X-2019-1-51-58","url":null,"abstract":"UV spectrophotometric and chromatographic study of the distribution and hydration of trifluoroacetophenone (TFAF) and some its derivatives ( p-trifluoroacetyl benzoic acid heptyl ester (TFABAHE), p-methyltrifluoroacetophenone ( p-MTFAF), 2,4-dimethyltrifluoroacetophenone (DMTFAF), 2,4,6-trimethyltrifluoroacetophenone (TMTFAF)) in the hexane-water system, which models the polyvinyl chloride membrane of ion-selective electrodes was investigated. TFAF has a high solubility in water (distribution coefficient D is equal to 415) as compared with p-MTFAF, DMTFAF, TMTFAF and TFABAHE (D within 1360 –2700). Hydration occurs most strongly to TFABAHE and is especially strong in alkaline medium. It is established that p-MTFAF and TFABAHE form a crystalline hydrates.","PeriodicalId":17303,"journal":{"name":"Journal of the Belarusian State University. Chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87164297","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 : 2019-02-21DOI: 10.33581/2520-257x-2019-1-3-13
A. A. Sladkova, I. Edimecheva, A. Sosnovskaya, O. Shadyro
А new way of the free radical ROS- and HOCl-induced destruction of serine, threonine, and their peptide derivatives due to the nitrogen-centered radicals formation and their subsequent decomposition with the side chain elimination has been established. It has been shown that substances with reducing properties are inhibitors of this process, while oxygen does not affect the probability of its occurrence. The data obtained are relevant for the development of novel approaches to the search for effective free radical processes regulators.
{"title":"Free radical destruction of hydroxyl-containing amino acids","authors":"A. A. Sladkova, I. Edimecheva, A. Sosnovskaya, O. Shadyro","doi":"10.33581/2520-257x-2019-1-3-13","DOIUrl":"https://doi.org/10.33581/2520-257x-2019-1-3-13","url":null,"abstract":"А new way of the free radical ROS- and HOCl-induced destruction of serine, threonine, and their peptide derivatives due to the nitrogen-centered radicals formation and their subsequent decomposition with the side chain elimination has been established. It has been shown that substances with reducing properties are inhibitors of this process, while oxygen does not affect the probability of its occurrence. The data obtained are relevant for the development of novel approaches to the search for effective free radical processes regulators.","PeriodicalId":17303,"journal":{"name":"Journal of the Belarusian State University. Chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76619959","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 : 2019-02-21DOI: 10.33581/2520-257x-2019-1-32-37
L. Sadovskaya, T. V. Sviridova, M. V. Morozova, D. Sviridov
The possibility of synthesis of highly photoactive nanosized titania employing ion exchange to exert control over polycondensation of titanium acid in aqueous medium has been demonstrated. The resultant spherical TiO2 nanoparticles exhibits extra high light-induced oxidation activity remaining for some time even after termination of UV illumination. The nanodispersed titania readily penetrate into the surface pores and can be used for deposition of photocatalytic coatings by impregnation technique.
{"title":"Synthesis of nanodispersed titanium dioxide via pH-controlled polymerization of titanium acid","authors":"L. Sadovskaya, T. V. Sviridova, M. V. Morozova, D. Sviridov","doi":"10.33581/2520-257x-2019-1-32-37","DOIUrl":"https://doi.org/10.33581/2520-257x-2019-1-32-37","url":null,"abstract":"The possibility of synthesis of highly photoactive nanosized titania employing ion exchange to exert control over polycondensation of titanium acid in aqueous medium has been demonstrated. The resultant spherical TiO2 nanoparticles exhibits extra high light-induced oxidation activity remaining for some time even after termination of UV illumination. The nanodispersed titania readily penetrate into the surface pores and can be used for deposition of photocatalytic coatings by impregnation technique.","PeriodicalId":17303,"journal":{"name":"Journal of the Belarusian State University. Chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88378519","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 : 2019-02-21DOI: 10.33581/2520-257x-2019-1-14-21
E. Petrova, Ya. A. Shavshukova, D. Kotsikau, K. Yanushkevich, K. Laznev, V. Pankov
Thermal treatment of ferrite magnetic nanoparticles in NaCl matrix gives an opportunity to increase their specific magnetization with preservation of nanoscale size. Composite materials based on mixed ferrites Co0.65Zn0.35Fe2O4 and Mg 0.5Zn0.5Fe2O4 were synthesized by spray-drying of aqueous suspensions in presence of NaCl and annealed at 300 –900 °C. The microstructure and phase composition of nanoparticles before and after annealing were studied by scanning and transmission electron microscopy (SEM and TEM), X-ray diffraction analysis and IR spectroscopy. The magnetic properties of nanoparticles were estimated using a ponderomotive method of measuring the specific magneti zation at room temperature in a magnetic field with an induction of 0.86 T. The increase of the annealing temperature up to 900 °C was established to lead to the increase in the specific magnetization of ferrites – from 32.79 to 91.3 emu/g (Co0.65Zn0.35Fe2O4) and from 2.76 to 22.31 emu/g (Mg 0.5 Zn 0.5Fe2O4) due to recrystallization processes and increase of crystallinity degree of the ferrites. Due to the NaCl insulating layer, the particle size increases just slightly (from ~ 10 nm before annealing to ~ 60 nm after annealing at 900 °C). This method is effective for substantial increase in specific magnetization of ferrite nanoparticles with preservation of their nanoscale size.
{"title":"Thermolysis of sprayed suspensions for obtaining highly spinel ferrite nanoparticles","authors":"E. Petrova, Ya. A. Shavshukova, D. Kotsikau, K. Yanushkevich, K. Laznev, V. Pankov","doi":"10.33581/2520-257x-2019-1-14-21","DOIUrl":"https://doi.org/10.33581/2520-257x-2019-1-14-21","url":null,"abstract":"Thermal treatment of ferrite magnetic nanoparticles in NaCl matrix gives an opportunity to increase their specific magnetization with preservation of nanoscale size. Composite materials based on mixed ferrites Co0.65Zn0.35Fe2O4 and Mg 0.5Zn0.5Fe2O4 were synthesized by spray-drying of aqueous suspensions in presence of NaCl and annealed at 300 –900 °C. The microstructure and phase composition of nanoparticles before and after annealing were studied by scanning and transmission electron microscopy (SEM and TEM), X-ray diffraction analysis and IR spectroscopy. The magnetic properties of nanoparticles were estimated using a ponderomotive method of measuring the specific magneti zation at room temperature in a magnetic field with an induction of 0.86 T. The increase of the annealing temperature up to 900 °C was established to lead to the increase in the specific magnetization of ferrites – from 32.79 to 91.3 emu/g (Co0.65Zn0.35Fe2O4) and from 2.76 to 22.31 emu/g (Mg 0.5 Zn 0.5Fe2O4) due to recrystallization processes and increase of crystallinity degree of the ferrites. Due to the NaCl insulating layer, the particle size increases just slightly (from ~ 10 nm before annealing to ~ 60 nm after annealing at 900 °C). This method is effective for substantial increase in specific magnetization of ferrite nanoparticles with preservation of their nanoscale size.","PeriodicalId":17303,"journal":{"name":"Journal of the Belarusian State University. Chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74561683","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 : 2019-02-21DOI: 10.33581/2520-257x-2019-1-22-31
Ruslan A. Anushko, Alesia V. Zyhmant, T. Savitskaya, Nadzeia G. Tsyhankova, D. Hrynshpan
The effect of aluminum coagulants composition and pH regulator dosing method on colloidal characteristics of aluminum hydroxide dispersions (diameter, particle size distribution, density and sedimentation rate of aggregates) was investigated by using of laser diffraction method. Highly basic polyaluminum chloride «Brilliant-50» was established to form aggregates of larger size and lower density than aluminum sulfate. Size and density of the aluminum sulfate aggregates were found to be a function of the pH dosing method (multi- or single-stage dosing). This effect became more evident when powdered coagulant was used as compared to its solution. According to computational study results hydration of aluminum polynuclear hydroxocomplexes increased with their molecular mass increasing, and consequently density of coagulation aggregates formed by them was suggested to decrease.
{"title":"Colloidal characteristics of aluminum hyd roxide dispersions depending on coagulant composition and pH regulator dosing method","authors":"Ruslan A. Anushko, Alesia V. Zyhmant, T. Savitskaya, Nadzeia G. Tsyhankova, D. Hrynshpan","doi":"10.33581/2520-257x-2019-1-22-31","DOIUrl":"https://doi.org/10.33581/2520-257x-2019-1-22-31","url":null,"abstract":"The effect of aluminum coagulants composition and pH regulator dosing method on colloidal characteristics of aluminum hydroxide dispersions (diameter, particle size distribution, density and sedimentation rate of aggregates) was investigated by using of laser diffraction method. Highly basic polyaluminum chloride «Brilliant-50» was established to form aggregates of larger size and lower density than aluminum sulfate. Size and density of the aluminum sulfate aggregates were found to be a function of the pH dosing method (multi- or single-stage dosing). This effect became more evident when powdered coagulant was used as compared to its solution. According to computational study results hydration of aluminum polynuclear hydroxocomplexes increased with their molecular mass increasing, and consequently density of coagulation aggregates formed by them was suggested to decrease.","PeriodicalId":17303,"journal":{"name":"Journal of the Belarusian State University. Chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90922163","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 : 2019-02-21DOI: 10.33581/2520-257x-2019-1-38-44
T. Salamakha, E. Trusova, Y. Tratsiak
In this paper an original method for obtaining glass-ceramics based on barium iodide powder activated with Eu2+ is proposed, their structural and spectral-luminescent properties are investigated. X-ray diffraction analysis has evidenced that glass-ceramics containing BaI2 ∙ 2H2O and BaI2 are formed when 50 mas. % of the starting iodide powder is used in the synthesis process. The possibility of using glass-ceramics for preventing the contact of iodide powder with water vapor has been confirmed.
{"title":"Preparation and study of the luminescent glass-ceramics based on barium iodide activated with Eu2+","authors":"T. Salamakha, E. Trusova, Y. Tratsiak","doi":"10.33581/2520-257x-2019-1-38-44","DOIUrl":"https://doi.org/10.33581/2520-257x-2019-1-38-44","url":null,"abstract":"In this paper an original method for obtaining glass-ceramics based on barium iodide powder activated with Eu2+ is proposed, their structural and spectral-luminescent properties are investigated. X-ray diffraction analysis has evidenced that glass-ceramics containing BaI2 ∙ 2H2O and BaI2 are formed when 50 mas. % of the starting iodide powder is used in the synthesis process. The possibility of using glass-ceramics for preventing the contact of iodide powder with water vapor has been confirmed.","PeriodicalId":17303,"journal":{"name":"Journal of the Belarusian State University. Chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81462829","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 : 2019-02-21DOI: 10.33581/2520-257x-2019-1-66-77
Valeryia B. Filistovich, T. Savitskaya, Irina M. Kimlenka, D. Hrynshpan, S. E. Makarevich, V. Teplyakov, D. Syrtsova
A «green» method of obtaining gas separation composite membranes from cellulose solutions and its mixtures with chitosan in orthophosphoric acid is proposed for industrial use, and differs from the viscose method of producing cellophane and other known methods for producing cellulose gas separation membranes without gaseous emissions and wastewater. It is shown that new composite cellulose membranes on a viscose fabric substrate are characterized by high productivity and selectivity for O2/ N2 pairs, comparable to the values obtained for known membranes made of synthetic polymers, as well as increased mechanical strength. The developed composite membranes demonstrate an inverse selectivity for the CH4/CO2 pair, which is not typical for gas separation membranes described in the literature with cellulose-based selective layers.
{"title":"Novel membranes based on cellulose for gas separation and green method for their preparing","authors":"Valeryia B. Filistovich, T. Savitskaya, Irina M. Kimlenka, D. Hrynshpan, S. E. Makarevich, V. Teplyakov, D. Syrtsova","doi":"10.33581/2520-257x-2019-1-66-77","DOIUrl":"https://doi.org/10.33581/2520-257x-2019-1-66-77","url":null,"abstract":"A «green» method of obtaining gas separation composite membranes from cellulose solutions and its mixtures with chitosan in orthophosphoric acid is proposed for industrial use, and differs from the viscose method of producing cellophane and other known methods for producing cellulose gas separation membranes without gaseous emissions and wastewater. It is shown that new composite cellulose membranes on a viscose fabric substrate are characterized by high productivity and selectivity for O2/ N2 pairs, comparable to the values obtained for known membranes made of synthetic polymers, as well as increased mechanical strength. The developed composite membranes demonstrate an inverse selectivity for the CH4/CO2 pair, which is not typical for gas separation membranes described in the literature with cellulose-based selective layers.","PeriodicalId":17303,"journal":{"name":"Journal of the Belarusian State University. Chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77281444","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 : 2019-02-21DOI: 10.33581/2520-257x-2019-1-78-85
Pavel G. Shahoika, Aliaksandr A. Ahabalayeu, Olga N. Tchekhovskaya, Y. Pakhadnia, S. A. Beliaev, S. Leschev
Nandrolone is an anabolic androgenic steroid. The use of this substance is prohibited by World Anti-Doping Agency (WADA). In National Anti-Doping Laboratory, we have developed method for quantitative determination of major nandrolone metabolite – 19-norandrosterone in human urine by GC/MS technique (Agilent 7000). Proposed method includes sample preparation of urine samples with enzymatic hydrolysis, liquid-liquid extraction followed by derivatization step with MSTFA. Deuterated 19-norandrosterone has been used as internal standard. Total run time comprised 16 min. Lower limit of quantitation accounted for 1 ng/mL. Spiked urine samples were prepared by mixing blank urine with standard solutions of 19-norandrosterone in range 1–30 ng/mL, correlation coefficient larger than 0.99. Method was verified to following validation parameters: selectivity, linearity, repeatability, accuracy, matrix effect, stability and robustness. Furthermore, measurement uncertainty was estimated. Thus, proposed method is able to detect threshold 19-norandrosterone in human urine and carry out its quantitation conforming WADA requirements.
{"title":"Quantitative determination of major nandrolone metabolite in human urine by gas chromatography/mass spectrometry","authors":"Pavel G. Shahoika, Aliaksandr A. Ahabalayeu, Olga N. Tchekhovskaya, Y. Pakhadnia, S. A. Beliaev, S. Leschev","doi":"10.33581/2520-257x-2019-1-78-85","DOIUrl":"https://doi.org/10.33581/2520-257x-2019-1-78-85","url":null,"abstract":"Nandrolone is an anabolic androgenic steroid. The use of this substance is prohibited by World Anti-Doping Agency (WADA). In National Anti-Doping Laboratory, we have developed method for quantitative determination of major nandrolone metabolite – 19-norandrosterone in human urine by GC/MS technique (Agilent 7000). Proposed method includes sample preparation of urine samples with enzymatic hydrolysis, liquid-liquid extraction followed by derivatization step with MSTFA. Deuterated 19-norandrosterone has been used as internal standard. Total run time comprised 16 min. Lower limit of quantitation accounted for 1 ng/mL. Spiked urine samples were prepared by mixing blank urine with standard solutions of 19-norandrosterone in range 1–30 ng/mL, correlation coefficient larger than 0.99. Method was verified to\u0000following validation parameters: selectivity, linearity, repeatability, accuracy, matrix effect, stability and robustness. Furthermore, measurement uncertainty was estimated. Thus, proposed method is able to detect threshold 19-norandrosterone in human urine and carry out its quantitation conforming WADA requirements.","PeriodicalId":17303,"journal":{"name":"Journal of the Belarusian State University. Chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74302018","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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