Pub Date : 2024-07-19DOI: 10.1134/s0020168524700079
E. B. Kovaleva, S. G. Dyachkova, A. A. Ganina, I. E. Kuzora, V. A. Sergeev
Abstract
The octane number for gaseous components (GC) is currently determined using the calculation method proceeding from the hydrocarbon composition. The method provides determination of the research octane number (RON) only. A discrepancy between the actual and predicted values of the octane number thus determined leads to an overestimated introduction of these components into the fuel which results in the reduced fuel performance and economic indicators of the production. In this regard, the development of a new approach to the determination of the blending octane number of low-boiling components is extremely important for designing optimal formulations of motor fuels. A method for determining the blending octane numbers (both RON and MON) of motor gasoline gaseous components has been improved owing to preliminary sample preparation by bubbling which provided taking into account the proportion of involvement of fractions of C4 hydrocarbon and pentane–amylene along with the chemical nature of the base fuel components. It is shown that the value of the blending octane number for gaseous components depends on the hydrocarbon composition of the base component. Application of the developed method to determining the blending octane number of gaseous components of motor fuels allowed us to obtain optimal formulations of gasoline with the involvement of low-boiling by-products and increase the accuracy of forecasting the composition of fuels, thus improving the economic performance of the production.
{"title":"A New Approach to Determining the Blending Octane Number of Gaseous Components of Motor Gasolines","authors":"E. B. Kovaleva, S. G. Dyachkova, A. A. Ganina, I. E. Kuzora, V. A. Sergeev","doi":"10.1134/s0020168524700079","DOIUrl":"https://doi.org/10.1134/s0020168524700079","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>The octane number for gaseous components (GC) is currently determined using the calculation method proceeding from the hydrocarbon composition. The method provides determination of the research octane number (RON) only. A discrepancy between the actual and predicted values of the octane number thus determined leads to an overestimated introduction of these components into the fuel which results in the reduced fuel performance and economic indicators of the production. In this regard, the development of a new approach to the determination of the blending octane number of low-boiling components is extremely important for designing optimal formulations of motor fuels. A method for determining the blending octane numbers (both RON and MON) of motor gasoline gaseous components has been improved owing to preliminary sample preparation by bubbling which provided taking into account the proportion of involvement of fractions of C<sub>4</sub> hydrocarbon and pentane–amylene along with the chemical nature of the base fuel components. It is shown that the value of the blending octane number for gaseous components depends on the hydrocarbon composition of the base component. Application of the developed method to determining the blending octane number of gaseous components of motor fuels allowed us to obtain optimal formulations of gasoline with the involvement of low-boiling by-products and increase the accuracy of forecasting the composition of fuels, thus improving the economic performance of the production.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"31 1","pages":""},"PeriodicalIF":0.8,"publicationDate":"2024-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141738959","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-07-19DOI: 10.1134/s002016852470002x
A. V. Brown, U. A. Bliznyuk, P. Yu. Borshchegovskaya, V. S. Ipatova, O. Yu. Khmelevsky, A. P. Chernyaev, I. A. Ananyeva, I. A. Rodin
Abstract
A method is proposed for the high-performance liquid chromatography–mass spectrometry quantification of the effect of an ionizing radiation dose on the structural characteristics of bovine serum albumin (BSA) in an aqueous solution by identifying unique peptides of the protein domain structures. BSA with an initial concentration of 500 mg/L in the physiological solution is irradiated with an accelerated electron beam with the maximum energy of 1 MeV and an average beam current of 1 pA at a dose rate of 18.5 Gy/s. The dose absorbed in the sample volume is estimated with a Fricke (ferrous sulfate) dosimeter. After irradiation of the BSA solution at doses of 0.3, 0.6, 1, 8, and 20 kGy, the structural integrity of the protein native form is analyzed and the protein content is quantified. To do this, the compounds with a mass of more than 30 kDa are removed by centrifugation, and then, BSA is subjected to enzymatic hydrolysis with addition of the trypsin solution, and the resulting peptides with a mass of more than 10 kDa are repeatedly removed. The samples obtained are examined by high-performance liquid chromatography–mass spectrometry. After that, the content of intact protein molecules is estimated by determining the concentrations of unique peptides corresponding to each of the three domains formed from the BSA amino acid sequence. Using the developed technique, a change in the natural conformation of the investigated protein (its denaturation) in water samples induced by ionizing radiation at a dose ranging from 0.3 to 20 kGy is established, on average, for 71% of protein molecules exposed to doses of up to 1 kGy, 79% of molecules exposed to doses of 4 kGy, and 99–100% of molecules exposed to doses of 8 and 20 kGy.
{"title":"High-Performance Liquid Chromatography–Mass Spectrometry Study of the Effect of Accelerated Electrons on the Structure of Bovine Serum Albumin","authors":"A. V. Brown, U. A. Bliznyuk, P. Yu. Borshchegovskaya, V. S. Ipatova, O. Yu. Khmelevsky, A. P. Chernyaev, I. A. Ananyeva, I. A. Rodin","doi":"10.1134/s002016852470002x","DOIUrl":"https://doi.org/10.1134/s002016852470002x","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>A method is proposed for the high-performance liquid chromatography–mass spectrometry quantification of the effect of an ionizing radiation dose on the structural characteristics of bovine serum albumin (BSA) in an aqueous solution by identifying unique peptides of the protein domain structures. BSA with an initial concentration of 500 mg/L in the physiological solution is irradiated with an accelerated electron beam with the maximum energy of 1 MeV and an average beam current of 1 pA at a dose rate of 18.5 Gy/s. The dose absorbed in the sample volume is estimated with a Fricke (ferrous sulfate) dosimeter. After irradiation of the BSA solution at doses of 0.3, 0.6, 1, 8, and 20 kGy, the structural integrity of the protein native form is analyzed and the protein content is quantified. To do this, the compounds with a mass of more than 30 kDa are removed by centrifugation, and then, BSA is subjected to enzymatic hydrolysis with addition of the trypsin solution, and the resulting peptides with a mass of more than 10 kDa are repeatedly removed. The samples obtained are examined by high-performance liquid chromatography–mass spectrometry. After that, the content of intact protein molecules is estimated by determining the concentrations of unique peptides corresponding to each of the three domains formed from the BSA amino acid sequence. Using the developed technique, a change in the natural conformation of the investigated protein (its denaturation) in water samples induced by ionizing radiation at a dose ranging from 0.3 to 20 kGy is established, on average, for 71% of protein molecules exposed to doses of up to 1 kGy, 79% of molecules exposed to doses of 4 kGy, and 99–100% of molecules exposed to doses of 8 and 20 kGy.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"1 1","pages":""},"PeriodicalIF":0.8,"publicationDate":"2024-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141738956","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-07-19DOI: 10.1134/s0020168524700080
V. G. Amelin, I. V. Batov, O. I. Lavrukhina, A. V. Tretyakov, L. K. Kish
Abstract
A fast method of screening of samples and determination of 80 veterinary drug residues in food safety assessment is proposed. The stage of solid-phase extraction for the purification of the extract in the sample preparation is excluded; here, the matrix effect is neutralized by using isotope-labeled standards. The application of the isotope dilution method makes it possible to exclude the stage of construction of matrix calibration curves and to calculate the concentrations using correction coefficients found from standard aqueous solutions of analytes with a limited number of isotope-labeled standards (one standard each for each class of compounds under determination). The limits of detection of medicinal products (cmin = 0.1–10 ng/g) make it possible to determine their residues at the level of maximum allowable concentrations for food.
{"title":"Screening and Simultaneous Determination of 80 Veterinary Drug Residues in Food by HPLC-MS/MS","authors":"V. G. Amelin, I. V. Batov, O. I. Lavrukhina, A. V. Tretyakov, L. K. Kish","doi":"10.1134/s0020168524700080","DOIUrl":"https://doi.org/10.1134/s0020168524700080","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>A fast method of screening of samples and determination of 80 veterinary drug residues in food safety assessment is proposed. The stage of solid-phase extraction for the purification of the extract in the sample preparation is excluded; here, the matrix effect is neutralized by using isotope-labeled standards. The application of the isotope dilution method makes it possible to exclude the stage of construction of matrix calibration curves and to calculate the concentrations using correction coefficients found from standard aqueous solutions of analytes with a limited number of isotope-labeled standards (one standard each for each class of compounds under determination). The limits of detection of medicinal products (<i>c</i><sub>min</sub> = 0.1–10 ng/g) make it possible to determine their residues at the level of maximum allowable concentrations for food.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"46 1","pages":""},"PeriodicalIF":0.8,"publicationDate":"2024-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141738943","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-07-19DOI: 10.1134/s0020168524700122
N. A. Korotkova, K. V. Petrova, V. B. Baranovskaya
Abstract
A method for analyzing iron garnets of the composition Y3–xCexFe5–yGayO12, where x = 0.4–0.5 and y = 2.4–2.6, using inductively coupled plasma atomic emission spectroscopy (ICP-AES) with preliminary decomposition of the sample in microwave system is described. During the investigation, conditions for microwave decomposition of samples are studied and selected—the composition of acid mixtures (HCl/HNO3) and modes of microwave heating (holding time and temperature) providing complete dissolution of the samples. Conditions for ICP-AES analysis of cerium-doped yttrium iron garnets and the effect of matrix components (Y, Ce, Fe, and Ga) on the determination of impurity elements are studied. The operating parameters of the spectrometer (high-frequency generator power and argon spray flow rate) making it possible to reduce the matrix effect when determining Na, Mg, Al, Si, P, K, Ca, Sc, Cr, Mn, Co, Ni, Cu, Zn, Se, Cd, Sn, Te, La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, and Pb impurities in yttrium iron garnets using ICP-AES are selected in order to minimize the matrix effect. ICP-AES studies are carried out in axial and radial modes for impurity elements and in radial modes for matrix elements. The limits of quantification (LOQs) of most analytes are in the range from n × 10–5 to n × 10–4 wt %. The accuracy is confirmed by the “spike–recovery” method, as well as by the analysis of samples with certified element contents. The standard deviation is in the range from 1 to 5% depending on the selected plasma viewing mode and the elements being detected. The developed method makes it possible to determine macro- and microcomponents in yttrium iron garnets in a wide range of concentrations with a high accuracy.
{"title":"Analysis of Cerium-Substituted Yttrium Iron Garnets Using Inductively Coupled Plasma Atomic Emission Spectrometry with Preliminary Decomposition in a Microwave System","authors":"N. A. Korotkova, K. V. Petrova, V. B. Baranovskaya","doi":"10.1134/s0020168524700122","DOIUrl":"https://doi.org/10.1134/s0020168524700122","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>A method for analyzing iron garnets of the composition Y<sub>3–<i>x</i></sub>Ce<sub><i>x</i></sub>Fe<sub>5–<i>y</i></sub>Ga<sub><i>y</i></sub>O<sub>12</sub>, where <i>x</i> = 0.4–0.5 and <i>y</i> = 2.4–2.6, using inductively coupled plasma atomic emission spectroscopy (ICP-AES) with preliminary decomposition of the sample in microwave system is described. During the investigation, conditions for microwave decomposition of samples are studied and selected—the composition of acid mixtures (HCl/HNO<sub>3</sub>) and modes of microwave heating (holding time and temperature) providing complete dissolution of the samples. Conditions for ICP-AES analysis of cerium-doped yttrium iron garnets and the effect of matrix components (Y, Ce, Fe, and Ga) on the determination of impurity elements are studied. The operating parameters of the spectrometer (high-frequency generator power and argon spray flow rate) making it possible to reduce the matrix effect when determining Na, Mg, Al, Si, P, K, Ca, Sc, Cr, Mn, Co, Ni, Cu, Zn, Se, Cd, Sn, Te, La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, and Pb impurities in yttrium iron garnets using ICP-AES are selected in order to minimize the matrix effect. ICP-AES studies are carried out in axial and radial modes for impurity elements and in radial modes for matrix elements. The limits of quantification (LOQs) of most analytes are in the range from <i>n</i> × 10<sup>–5</sup> to <i>n</i> × 10<sup>–4</sup> wt %. The accuracy is confirmed by the “spike–recovery” method, as well as by the analysis of samples with certified element contents. The standard deviation is in the range from 1 to 5% depending on the selected plasma viewing mode and the elements being detected. The developed method makes it possible to determine macro- and microcomponents in yttrium iron garnets in a wide range of concentrations with a high accuracy.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"81 1","pages":""},"PeriodicalIF":0.8,"publicationDate":"2024-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141738955","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-07-19DOI: 10.1134/s0020168524700110
A. V. Egoshina, G. B. Slepchenko
Abstract
Alloys based on platinum group metals have high chemical resistance, which causes a number of difficulties when dissolving them. Currently, among hydrometallurgical methods, dissolution in aqua regia is one of the most effective methods for opening corrosion-resistant alloys. The main disadvantage of this method is the release of toxic gases such as nitrosyl chloride and nitrogen oxides. To reduce the volume of released gases without reducing the oxidation-reduction potential (ORP) of the system, a method for dissolving a Pt–Rh alloy in HCl–HNO3 with dosed addition of HNO3 at a given value of the redox potential of the system is proposed in this study. The system potential chosen on the basis of the potentials of the HNO3–HCl–Pt and HNO3–HCl–Rh systems is 0.85 and 0.9 V. The influence of dispersion and defectiveness of the Pt–Rh alloy on its dissolution indices is also investigated. As a result, it is shown that the dissolution of the Pt–Rh alloy with a rhodium content of 15% in HCl–HNO3 at a constant ORP value of 0.9 V compared to the use of classical mixture (HCl : HNO3 = 1 : 3 (vol)) decreases the nitric acid consumption by 40%, reduces the process time, and increases the recovery factor as for platinum, and for rhodium, and also reduces the volume of released nitrogen oxides by half (theoretical calculation). It is established that the process of mechanical activation of the alloy reduces the dissolution time and leads to almost quantitative dissolution of the sample.
{"title":"Intensification of Opening a Thrust Alloy Based on Platinum and Rhodium","authors":"A. V. Egoshina, G. B. Slepchenko","doi":"10.1134/s0020168524700110","DOIUrl":"https://doi.org/10.1134/s0020168524700110","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>Alloys based on platinum group metals have high chemical resistance, which causes a number of difficulties when dissolving them. Currently, among hydrometallurgical methods, dissolution in aqua regia is one of the most effective methods for opening corrosion-resistant alloys. The main disadvantage of this method is the release of toxic gases such as nitrosyl chloride and nitrogen oxides. To reduce the volume of released gases without reducing the oxidation-reduction potential (ORP) of the system, a method for dissolving a Pt–Rh alloy in HCl–HNO<sub>3</sub> with dosed addition of HNO<sub>3</sub> at a given value of the redox potential of the system is proposed in this study. The system potential chosen on the basis of the potentials of the HNO<sub>3</sub>–HCl–Pt and HNO<sub>3</sub>–HCl–Rh systems is 0.85 and 0.9 V. The influence of dispersion and defectiveness of the Pt–Rh alloy on its dissolution indices is also investigated. As a result, it is shown that the dissolution of the Pt–Rh alloy with a rhodium content of 15% in HCl–HNO<sub>3</sub> at a constant ORP value of 0.9 V compared to the use of classical mixture (HCl : HNO<sub>3</sub> = 1 : 3 (vol)) decreases the nitric acid consumption by 40%, reduces the process time, and increases the recovery factor as for platinum, and for rhodium, and also reduces the volume of released nitrogen oxides by half (theoretical calculation). It is established that the process of mechanical activation of the alloy reduces the dissolution time and leads to almost quantitative dissolution of the sample.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"253 1","pages":""},"PeriodicalIF":0.8,"publicationDate":"2024-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141738958","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-07-19DOI: 10.1134/s0020168524700109
V. I. Vershinin, L. S. Bazhenova
Abstract
The total content (cΣ) of toxic phenols in waters is usually determined by methods involving the introduction of a group reagent, measurement of the generalized signal (AΣ) at a selected wavelength, and estimation of cΣ in terms of C6H5OH. The use of diazotized sulfanilic acid as a group reagent allows one to determine cΣ with errors not exceeding 30 rel %. Further reduction of errors is possible with transition to multiple-wavelength measurements and multivariate calibrations, but for the determination of phenolic toxicants, these techniques have not been used before. To test this possibility, model mixtures (colored aqueous solutions) were prepared, simultaneously containing up to five different phenols with their total concentration from 15 to 70 μmol/L. The generalized signals were measured at m wavelengths in the UV region of the spectrum 10 min after mixing the solutions. Inverted multivariate calibrations were constructed on the basis of the AΣ values of n mixtures of the same type that formed the training set. Under optimized conditions (m = 7, n = 10), systematic errors (δc) in determining the amount of phenols in mixtures from the test sample did not exceed 13 rel %, which is half as much as when recalculating the signal to a standard substance. Obviously, it is advisable to use multivariate calibrations for a generalized assessment of phenolic pollution of water bodies instead of calculating total indices. However, in cases where the samples contained phenols that were not taken into account when constructing the calibration, an increase in systematic errors was observed, reaching as high as 80 rel % (in absolute value). Therefore, to use multivariate calibrations in hydrochemical analysis, a preliminary study of the qualitative composition of phenolic mixtures in waters of different types and taking into account the expected composition of samples when forming a training set are necessary.
{"title":"Application of Inverted Multivariate Calibrations to Determine the Total Content of Phenols","authors":"V. I. Vershinin, L. S. Bazhenova","doi":"10.1134/s0020168524700109","DOIUrl":"https://doi.org/10.1134/s0020168524700109","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>The total content (<i>c</i><sub>Σ</sub>) of toxic phenols in waters is usually determined by methods involving the introduction of a group reagent, measurement of the generalized signal (<i>A</i><sub>Σ</sub>) at a selected wavelength, and estimation of <i>c</i><sub>Σ</sub> in terms of C<sub>6</sub>H<sub>5</sub>OH. The use of diazotized sulfanilic acid as a group reagent allows one to determine <i>c</i><sub>Σ</sub> with errors not exceeding 30 rel %. Further reduction of errors is possible with transition to multiple-wavelength measurements and multivariate calibrations, but for the determination of phenolic toxicants, these techniques have not been used before. To test this possibility, model mixtures (colored aqueous solutions) were prepared, simultaneously containing up to five different phenols with their total concentration from 15 to 70 μmol/L. The generalized signals were measured at <i>m</i> wavelengths in the UV region of the spectrum 10 min after mixing the solutions. Inverted multivariate calibrations were constructed on the basis of the <i>A</i><sub>Σ</sub> values of <i>n</i> mixtures of the same type that formed the training set. Under optimized conditions (<i>m</i> = 7, <i>n</i> = 10), systematic errors (δ<i>c</i>) in determining the amount of phenols in mixtures from the test sample did not exceed 13 rel %, which is half as much as when recalculating the signal to a standard substance. Obviously, it is advisable to use multivariate calibrations for a generalized assessment of phenolic pollution of water bodies instead of calculating total indices. However, in cases where the samples contained phenols that were not taken into account when constructing the calibration, an increase in systematic errors was observed, reaching as high as 80 rel % (in absolute value). Therefore, to use multivariate calibrations in hydrochemical analysis, a preliminary study of the qualitative composition of phenolic mixtures in waters of different types and taking into account the expected composition of samples when forming a training set are necessary.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"42 1","pages":""},"PeriodicalIF":0.8,"publicationDate":"2024-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141738960","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-07-19DOI: 10.1134/s0020168524700092
E. V. Bizina, A. A. Polosina, O. V. Farafonova, S. A. Eremin, T. N. Ermolaeva
Abstract
This article describes a method for detection of aristolochic acid (AA) in food products using a piezoelectric immunosensor, the recognition layer of which was magnetic carbon nanocomposites (MCNCs) with AA protein conjugates immobilized on their surface. Methods for the synthesis of magnetic Fe3O4 nuclei and their fixation on the surface of multiwalled carbon nanotubes (CNTs) have been studied. Using IR spectroscopy, it was established that the formation of the recognition layer of the sensor occurs owing to the formation of covalent bonds between the amino groups of AA conjugates and the carboxyl groups of CNTs. The concentrations of protein conjugates based on ovalbumin (OVA) and bovine serum albumin (BSA) (0.3 and 0.2 mg/mL) and the degree of dilution of antibodies (0.25) providing optimal characteristics of the piezoelectric immunosensor were determined. The metrological characteristics of the determination of AA using the proposed method have been established: the range of determined contents and the detection limit of AA when using a piezoelectric immunosensor with a recognition layer based on MCNC/AA-OVA and MCNC/AA-BSA are 50–400 and 10 ng/mL and 100–300 and 50 ng/mL, respectively. The sensor was tested upon determination of AA in samples of Chinese herbal tea and dietary supplements for weight loss. No acid was found in the tea, but in the dietary supplements, its content is 3.2 μg/g.
摘要 本文介绍了一种利用压电免疫传感器检测食品中马兜铃酸（AA）的方法，该传感器的识别层是磁性碳纳米复合材料（MCNCs），其表面固定有 AA 蛋白共轭物。研究了磁性 Fe3O4 核的合成方法以及将其固定在多壁碳纳米管（CNT）表面的方法。利用红外光谱法确定了传感器识别层的形成是由于 AA 共轭物的氨基与 CNT 的羧基之间形成了共价键。确定了基于卵清蛋白（OVA）和牛血清白蛋白（BSA）的蛋白共轭物的浓度（0.3 和 0.2 mg/mL）以及抗体的稀释度（0.25），从而使压电免疫传感器具有最佳特性。确定了使用拟议方法测定 AA 的计量特性：使用基于 MCNC/AA-OVA 和 MCNC/AA-BSA 的带有识别层的压电免疫传感器测定 AA 的含量范围和检测限分别为 50-400 和 10 纳克/毫升，以及 100-300 和 50 纳克/毫升。对传感器进行了测试，以测定中草药茶和减肥膳食补充剂样品中的 AA 含量。在茶叶中没有发现酸，但在膳食补充剂中，其含量为 3.2 微克/克。
{"title":"Detection of Aristolochic Acid Using a Piezoelectric Immunosensor Based on Magnetic Carbon Nanocomposites","authors":"E. V. Bizina, A. A. Polosina, O. V. Farafonova, S. A. Eremin, T. N. Ermolaeva","doi":"10.1134/s0020168524700092","DOIUrl":"https://doi.org/10.1134/s0020168524700092","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>This article describes a method for detection of aristolochic acid (AA) in food products using a piezoelectric immunosensor, the recognition layer of which was magnetic carbon nanocomposites (MCNCs) with AA protein conjugates immobilized on their surface. Methods for the synthesis of magnetic Fe<sub>3</sub>O<sub>4</sub> nuclei and their fixation on the surface of multiwalled carbon nanotubes (CNTs) have been studied. Using IR spectroscopy, it was established that the formation of the recognition layer of the sensor occurs owing to the formation of covalent bonds between the amino groups of AA conjugates and the carboxyl groups of CNTs. The concentrations of protein conjugates based on ovalbumin (OVA) and bovine serum albumin (BSA) (0.3 and 0.2 mg/mL) and the degree of dilution of antibodies (0.25) providing optimal characteristics of the piezoelectric immunosensor were determined. The metrological characteristics of the determination of AA using the proposed method have been established: the range of determined contents and the detection limit of AA when using a piezoelectric immunosensor with a recognition layer based on MCNC/AA-OVA and MCNC/AA-BSA are 50–400 and 10 ng/mL and 100–300 and 50 ng/mL, respectively. The sensor was tested upon determination of AA in samples of Chinese herbal tea and dietary supplements for weight loss. No acid was found in the tea, but in the dietary supplements, its content is 3.2 μg/g.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"9 1","pages":""},"PeriodicalIF":0.8,"publicationDate":"2024-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141738775","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-07-19DOI: 10.1134/s0020168524700043
D. Kh. Kitaeva, O. L. Lependina, V. N. Talanova, I. V Karandi, A. G. Buyanovskaya
Abstract
In the course of the synthesis of new metalloorganic compounds, there is a need for rapid monitoring of the elemental composition of the resulting substances at different stages of the process. In the microanalysis laboratory of the Nesmeyanov Institute of Organoelement Compounds, the metal content in the composition of substances determined using the XRF method is based on the external reference method with dilution of the sample with emulsion polystyrene. When preparing analyzed reflector samples, accurate weighing of the sample and diluent is required, since the dilution coefficient is required to calculate the content of elements. In cases where chemists involved in chemical synthesis are not interested in the exact elemental composition of the resulting compound, but in the atomic ratio of metals included in the organic matrix, when preparing analyzed samples, we propose to eliminate the lengthy weighing procedure and use approximately selected amounts of substances. The technique was tested in the analysis of a number of ferrocene derivatives containing platinum atoms, and a rapid weightless method for determining the atomic ratios of Fe and Pt in synthesis products using the FeKα and PtLα lines was proposed. The metal content in the emitter samples was determined using calibration equations. Simplification of the analysis procedure and the absence of weighing significantly speeds up the analyst’s work. The proposed method can be used as a preliminary criterion for the success of the synthesis of the expected product before its full elemental analysis is carried out.
{"title":"Rapid Weightless Determination of the Atomic Ratio of Iron and Platinum in Ferrocene Derivatives by X-Ray Fluorescence Analysis","authors":"D. Kh. Kitaeva, O. L. Lependina, V. N. Talanova, I. V Karandi, A. G. Buyanovskaya","doi":"10.1134/s0020168524700043","DOIUrl":"https://doi.org/10.1134/s0020168524700043","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>In the course of the synthesis of new metalloorganic compounds, there is a need for rapid monitoring of the elemental composition of the resulting substances at different stages of the process. In the microanalysis laboratory of the Nesmeyanov Institute of Organoelement Compounds, the metal content in the composition of substances determined using the XRF method is based on the external reference method with dilution of the sample with emulsion polystyrene. When preparing analyzed reflector samples, accurate weighing of the sample and diluent is required, since the dilution coefficient is required to calculate the content of elements. In cases where chemists involved in chemical synthesis are not interested in the exact elemental composition of the resulting compound, but in the atomic ratio of metals included in the organic matrix, when preparing analyzed samples, we propose to eliminate the lengthy weighing procedure and use approximately selected amounts of substances. The technique was tested in the analysis of a number of ferrocene derivatives containing platinum atoms, and a rapid weightless method for determining the atomic ratios of Fe and Pt in synthesis products using the Fe<i>K</i>α and Pt<i>L</i>α lines was proposed. The metal content in the emitter samples was determined using calibration equations. Simplification of the analysis procedure and the absence of weighing significantly speeds up the analyst’s work. The proposed method can be used as a preliminary criterion for the success of the synthesis of the expected product before its full elemental analysis is carried out.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"6 1","pages":""},"PeriodicalIF":0.8,"publicationDate":"2024-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141738957","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-07-19DOI: 10.1134/s0020168524700018
E. G. Kulapina, R. K. Mursalov, O. I. Kulapina, V. D. Ankina, E. N. Cherdakova
Abstract
Planar screen-printed potentiometric sensors sensitive to cefepime, a fourth-generation cephalosporine antibiotic, have been developed. Cefepime is an amphoteric antibiotic with the carboxyl and aminothiazole groups, which exists as a cation in strongly acidic media, a zwitterion in weakly acidic and neutral media, and an anion in alkaline media. The interval of pH 1.5–2.0 for obtaining the cationic electrode functions for the determination of cefepime has been established. The cefepime–tetraphenylborate associates have been used as electrode-active components; the optimum content of the latter for planar sensors is 2–3%. For the unmodified cefepime sensors, the electrode functions are linear in the range of 1 × 10–5–1 × 10–2 M, the angular coefficients are 50 ± 2 mV/pC, and the response time is 20 s. The role of the modifier, ZnO nanoparticles, in improving the electroanalytical properties of the sensors is shown. The introduction of a binary mixture of zinc oxide and cetylpyridinium chloride into carbon-based ink reduces the cefepime detection limit (1 × 10–6 M) and increases the angular coefficient (58 ± 1 mV/pC), the interval of linearity of the electrode functions (1 × 10–6–1 × 10–2 M), and the sensor response time (17 s). A surfactant used as an electrode surface co-modifier stabilizes the nanoparticle dispersion. The use of the modified screen-printed sensors for the cefepime determination in medicinal and biological media, in particular, in saliva, is demonstrated.
{"title":"Modified Planar Sensors for Determination of Cefepime","authors":"E. G. Kulapina, R. K. Mursalov, O. I. Kulapina, V. D. Ankina, E. N. Cherdakova","doi":"10.1134/s0020168524700018","DOIUrl":"https://doi.org/10.1134/s0020168524700018","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>Planar screen-printed potentiometric sensors sensitive to cefepime, a fourth-generation cephalosporine antibiotic, have been developed. Cefepime is an amphoteric antibiotic with the carboxyl and aminothiazole groups, which exists as a cation in strongly acidic media, a zwitterion in weakly acidic and neutral media, and an anion in alkaline media. The interval of pH 1.5–2.0 for obtaining the cationic electrode functions for the determination of cefepime has been established. The cefepime–tetraphenylborate associates have been used as electrode-active components; the optimum content of the latter for planar sensors is 2–3%. For the unmodified cefepime sensors, the electrode functions are linear in the range of 1 × 10<sup>–5</sup>–1 × 10<sup>–2</sup> M, the angular coefficients are 50 ± 2 mV/p<i>C</i>, and the response time is 20 s. The role of the modifier, ZnO nanoparticles, in improving the electroanalytical properties of the sensors is shown. The introduction of a binary mixture of zinc oxide and cetylpyridinium chloride into carbon-based ink reduces the cefepime detection limit (1 × 10<sup>–6</sup> M) and increases the angular coefficient (58 ± 1 mV/p<i>C</i>), the interval of linearity of the electrode functions (1 × 10<sup>–6</sup>–1 × 10<sup>–2</sup> M), and the sensor response time (17 s). A surfactant used as an electrode surface co-modifier stabilizes the nanoparticle dispersion. The use of the modified screen-printed sensors for the cefepime determination in medicinal and biological media, in particular, in saliva, is demonstrated.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"55 1","pages":""},"PeriodicalIF":0.8,"publicationDate":"2024-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141738779","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-07-19DOI: 10.1134/s0020168524700031
I. V. Nikolaeva, S. V. Palesskiy
Abstract
Two microwave systems MARS-5 and UltraWAVE are compared in the efficiency with regard to the digestion of silicate rocks with subsequent determination of 32 elements (Sc, V, Cr, Co, Ni, Cu, Zn, Rb, Sr, Y, Nb, Ta, Cs, Ba, 14 REEs, Hf, Ta, Th, U) by inductively coupled plasma mass spectrometry (ICP-MS). The development of digestion methods and validation of the obtained results have been carried out using international reference materials—basalts BHVO-2 and BCR-2, serpentinite UB-N, and peridotite JP-1. Microwave digestion included a two-stage treatment of samples with a mixture of concentrated acids HF, HNO3, and HCl in MARS-5 (T = 190°C, P = 20 bar) and UltraWAVE (T = 240°C, P = 80 bar) with the distillation of excess fluorides in the form of SiF4 between microwave digestion stages. The determination of concentrations in the obtained solutions was carried out on an ELEMENT high-resolution mass spectrometer in low and medium resolution according to external calibration with the internal standard (In), taking into account the acid composition of the analyzed solutions. The detection limits of the analytes after acid digestion in MARS-5 and UltraWAVE are comparable and provide the determination of all specified elements, except for Ta in JP-1. The use of the developed sample preparation procedure in MARS-5 ensures the complete decomposition of BHVO-2, BCR-2, and UB-N followed by ICP-MS determination of 32 specified elements in the obtained solutions without additional preconcentration steps. The relative standard deviations for the determined elements are 2–9% for the reference materials BHVO-2 and BCR-2 and 3–12% for UB-N with an increase to 16–25% (Nb, Ta) due to the approach to the detection limit. The more efficient microwave digestion in UltraWAVE compared to MARS-5 was proved by the complete decomposition of JP-1 with the transfer of all the elements, including Cr, into the solution.
{"title":"Application of MARS-5 and UltraWAVE Microwave Systems to the Digestion of Silicate Rocks Followed by ICP-MS Analysis","authors":"I. V. Nikolaeva, S. V. Palesskiy","doi":"10.1134/s0020168524700031","DOIUrl":"https://doi.org/10.1134/s0020168524700031","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>Two microwave systems MARS-5 and UltraWAVE are compared in the efficiency with regard to the digestion of silicate rocks with subsequent determination of 32 elements (Sc, V, Cr, Co, Ni, Cu, Zn, Rb, Sr, Y, Nb, Ta, Cs, Ba, 14 REEs, Hf, Ta, Th, U) by inductively coupled plasma mass spectrometry (ICP-MS). The development of digestion methods and validation of the obtained results have been carried out using international reference materials—basalts BHVO-2 and BCR-2, serpentinite UB-N, and peridotite JP-1. Microwave digestion included a two-stage treatment of samples with a mixture of concentrated acids HF, HNO<sub>3</sub>, and HCl in MARS-5 (<i>T</i> = 190°C, <i>P</i> = 20 bar) and UltraWAVE (<i>T</i> = 240°C, <i>P</i> = 80 bar) with the distillation of excess fluorides in the form of SiF<sub>4</sub> between microwave digestion stages. The determination of concentrations in the obtained solutions was carried out on an ELEMENT high-resolution mass spectrometer in low and medium resolution according to external calibration with the internal standard (In), taking into account the acid composition of the analyzed solutions. The detection limits of the analytes after acid digestion in MARS-5 and UltraWAVE are comparable and provide the determination of all specified elements, except for Ta in JP-1. The use of the developed sample preparation procedure in MARS-5 ensures the complete decomposition of BHVO-2, BCR-2, and UB-N followed by ICP-MS determination of 32 specified elements in the obtained solutions without additional preconcentration steps. The relative standard deviations for the determined elements are 2–9% for the reference materials BHVO-2 and BCR-2 and 3–12% for UB-N with an increase to 16–25% (Nb, Ta) due to the approach to the detection limit. The more efficient microwave digestion in UltraWAVE compared to MARS-5 was proved by the complete decomposition of JP-1 with the transfer of all the elements, including Cr, into the solution.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"25 1","pages":""},"PeriodicalIF":0.8,"publicationDate":"2024-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141738953","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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