Pub Date : 2024-10-22DOI: 10.1134/S1061934824700862
A. S. Gubin, P. T. Sukhanov, A. A. Kushnir, Kh. S. Shikhaliev, M. A. Potapov
A sorbent with magnetic properties, functionalized with humates, in combination with gas chromatography–mass spectrometry is proposed for the determination of phenolic xenoestrogens (ED) in bottom sediments. The octylphenol (OP), nonylphenol (NP), and bisphenol A (BPA) ED are chosen as test samples. Along with ED, the distribution of the naturally occurring estrogen, 17β-estradiol (ES), is studied. Sorption preconcentration is carried out under dynamic conditions: a sorbent weighing 0.5 g is placed in a borosilicate glass column, on both sides of which magnets are placed to immobilize the sorbent. The analytical characteristics of the determination method are established using model samples of bottom sediments selected in a background area with a minimal anthropogenic impact. The limit of quantification for ED is 30–60 ng/kg (dry weight). In analyzing real samples, the sensitivity of the method is reduced by 3–4 times due to matrix effects of the presence of petroleum products in waters. The ED content of bottom sediments at the site of wastewater discharge into the river Don near the city of Voronezh, as well as on the Black Sea coast of the Caucasus (area of the city of Tuapse and the village of Olginka) was monitored. The maximum concentrations of OP, NP, BPA, and ES in bottom sediments were found in the area of the port of Tuapse, where they were 5.7, 8.1, 6.2 and 0.9 µg/kg, respectively.
本研究提出了一种具有磁性的吸附剂,该吸附剂具有腐殖酸盐功能,并结合气相色谱-质谱法测定底层沉积物中的酚类异雌激素(ED)。测试样品包括辛基酚(OP)、壬基酚(NP)和双酚 A(BPA)。除了 ED 之外,还研究了天然雌激素 17β-estradiol (ES) 的分布情况。吸附预富集是在动态条件下进行的:将重 0.5 克的吸附剂放入硼硅酸盐玻璃柱中,在柱子两侧放置磁铁以固定吸附剂。这种测定方法的分析特性是通过在人为影响极小的背景地区选取底层沉积物模型样本确定的。ED 的定量限为 30-60 纳克/千克(干重)。在分析实际样品时,由于水体中存在石油产品的基质效应,该方法的灵敏度降低了 3-4 倍。在沃罗涅日市附近向顿河排放废水的地点以及高加索黑海沿岸(图阿普谢市和奥尔金卡村地区),对底层沉积物中的 ED 含量进行了监测。在图阿普谢港地区发现,底层沉积物中 OP、NP、BPA 和 ES 的浓度最高,分别为 5.7、8.1、6.2 和 0.9 微克/千克。
{"title":"Using a Humate-Based Magnetic Sorbent and GC–MS for the Determination of Phenolic Xenoestrogens in Bottom Sediments","authors":"A. S. Gubin, P. T. Sukhanov, A. A. Kushnir, Kh. S. Shikhaliev, M. A. Potapov","doi":"10.1134/S1061934824700862","DOIUrl":"10.1134/S1061934824700862","url":null,"abstract":"<p>A sorbent with magnetic properties, functionalized with humates, in combination with gas chromatography–mass spectrometry is proposed for the determination of phenolic xenoestrogens (<b>ED</b>) in bottom sediments. The octylphenol (<b>OP</b>), nonylphenol (<b>NP</b>), and bisphenol A (<b>BPA</b>) ED are chosen as test samples. Along with ED, the distribution of the naturally occurring estrogen, 17β-estradiol (<b>ES</b>), is studied. Sorption preconcentration is carried out under dynamic conditions: a sorbent weighing 0.5 g is placed in a borosilicate glass column, on both sides of which magnets are placed to immobilize the sorbent. The analytical characteristics of the determination method are established using model samples of bottom sediments selected in a background area with a minimal anthropogenic impact. The limit of quantification for ED is 30–60 ng/kg (dry weight). In analyzing real samples, the sensitivity of the method is reduced by 3–4 times due to matrix effects of the presence of petroleum products in waters. The ED content of bottom sediments at the site of wastewater discharge into the river Don near the city of Voronezh, as well as on the Black Sea coast of the Caucasus (area of the city of Tuapse and the village of Olginka) was monitored. The maximum concentrations of OP, NP, BPA, and ES in bottom sediments were found in the area of the port of Tuapse, where they were 5.7, 8.1, 6.2 and 0.9 µg/kg, respectively.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":1.0,"publicationDate":"2024-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142518433","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-22DOI: 10.1134/S1061934824700825
A. A. Pupyshev, P. V. Kel’, M. Yu. Burylin, A. G. Abakumov, P. G. Abakumov
A possibility of studying effects of the main background ions formed by the main elements of inductively coupled plasma (H, N, O, and Ar) at the working parameters of the normal (“hot”) plasma mode by thermodynamic modeling is assessed. Such ions, responsible for the strongest spectral interferences in the mass spectra are always observed upon the injection of aqueous (“wet”) sample solutions into inductively coupled plasma mass spectrometers (ICP MS). The quantitative composition of the main background ions in an ICP MS is calculated as a function of plasma temperature in the temperature range from 3000 to 8000 K using thermodynamic modeling. The results of modeling were compared with the experimental data on the measured mass spectra of the main background ions and a high degree of correlation between the theoretical and experimental results was shown. The agreement between the results of calculations the experimental data validates the thermodynamic model of thermochemical processes in an ICP MS used and its applicability to subsequent calculations in fulfilling analytical tasks. A possibility of the unambiguous assessment of gas-kinetic plasma temperature is confirmed by comparing the theoretical and experimental mass spectra of the main ICP background ions in a normal mode. It was found that the calculated and experimental data on the concentration of only NO+ ions do not agree with the regularities noticed for the other background ions in the normal ICP mode.
通过热力学建模评估了在正常("热")等离子体模式工作参数下研究由电感耦合等离子体主要元素(H、N、O 和 Ar)形成的主要背景离子影响的可能性。将水性("湿")样品溶液注入电感耦合等离子体质谱仪(ICP MS)时,总能观察到这些离子,它们对质谱产生最强的光谱干扰。利用热力学模型计算出了在 3000 至 8000 K 温度范围内,ICP MS 中主要背景离子的定量组成与等离子体温度的函数关系。建模结果与主要背景离子质谱测量的实验数据进行了比较,结果表明理论结果与实验结果高度相关。计算结果与实验数据之间的一致性验证了所使用的 ICP MS 热化学过程热力学模型及其在完成分析任务的后续计算中的适用性。通过比较正常模式下主要 ICP 背景离子的理论和实验质谱,证实了对气体动力学等离子体温度进行明确评估的可能性。结果发现,只有 NO+ 离子浓度的计算和实验数据与正常 ICP 模式下其他背景离子的规律性不一致。
{"title":"Thermodynamic Modeling of the Composition of the Main Background Ions and Determination of Gas-Kinetic Temperature in the Normal (“Hot”) Inductively Coupled Plasma","authors":"A. A. Pupyshev, P. V. Kel’, M. Yu. Burylin, A. G. Abakumov, P. G. Abakumov","doi":"10.1134/S1061934824700825","DOIUrl":"10.1134/S1061934824700825","url":null,"abstract":"<p>A possibility of studying effects of the main background ions formed by the main elements of inductively coupled plasma (H, N, O, and Ar) at the working parameters of the normal (“hot”) plasma mode by thermodynamic modeling is assessed. Such ions, responsible for the strongest spectral interferences in the mass spectra are always observed upon the injection of aqueous (“wet”) sample solutions into inductively coupled plasma mass spectrometers (<b>ICP MS</b>). The quantitative composition of the main background ions in an ICP MS is calculated as a function of plasma temperature in the temperature range from 3000 to 8000 K using thermodynamic modeling. The results of modeling were compared with the experimental data on the measured mass spectra of the main background ions and a high degree of correlation between the theoretical and experimental results was shown. The agreement between the results of calculations the experimental data validates the thermodynamic model of thermochemical processes in an ICP MS used and its applicability to subsequent calculations in fulfilling analytical tasks. A possibility of the unambiguous assessment of gas-kinetic plasma temperature is confirmed by comparing the theoretical and experimental mass spectra of the main ICP background ions in a normal mode. It was found that the calculated and experimental data on the concentration of only NO<sup>+</sup> ions do not agree with the regularities noticed for the other background ions in the normal ICP mode.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":1.0,"publicationDate":"2024-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142518393","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-22DOI: 10.1134/S1061934824700722
V. D. Luzanova, N. B. Rozhmanova, S. N. Lanin, P. N. Nesterenko
Inorganic zeolites, or microporous crystalline aluminosilicates, possess high porosity, well-developed specific surface area, uniform pores, and ion-exchange properties, which determine their molecular sieve and adsorption properties. The use of zeolites as catalysts, desiccants for solvents and gases, and selective adsorbents for the separation of low-molecular-weight compounds is widely known. Zeolites also serve extensively as packing materials for chromatographic columns in gas-adsorption chromatography. However, their application to high-performance liquid chromatography (HPLC) is less recognized. In HPLC, the retention of adsorbates depends not only on adsorption interactions but also on the molecular sieve effect in the micropores and kinetically selective effects. Additional interactions with the mobile phase components alter the thermodynamic parameters of the adsorbates interaction with the zeolite, decrease effective pore size, and hinder the diffusion of the separated compounds into the adsorbent’s pores. Despite these challenges, zeolites remain promising adsorbents due to their strictly determined pore size (dpore) and geometry, as well as their customizable polarities, which ensure high selectivity for the separation of low-molecular-weight compounds. The most promising zeolites for HPLC are wide-pore zeolites (dpore 0.6–0.8 nm) with 8, 10, 12, and 14-member ring channels. This review offers a concise overview of the classification, composition, and structure of zeolites and their impact on the adsorption properties of these adsorbents. Data on the use of zeolites in HPLC are also systematized.
{"title":"Application of Zeolites in High-Performance Liquid Chromatography","authors":"V. D. Luzanova, N. B. Rozhmanova, S. N. Lanin, P. N. Nesterenko","doi":"10.1134/S1061934824700722","DOIUrl":"10.1134/S1061934824700722","url":null,"abstract":"<p>Inorganic zeolites, or microporous crystalline aluminosilicates, possess high porosity, well-developed specific surface area, uniform pores, and ion-exchange properties, which determine their molecular sieve and adsorption properties. The use of zeolites as catalysts, desiccants for solvents and gases, and selective adsorbents for the separation of low-molecular-weight compounds is widely known. Zeolites also serve extensively as packing materials for chromatographic columns in gas-adsorption chromatography. However, their application to high-performance liquid chromatography (HPLC) is less recognized. In HPLC, the retention of adsorbates depends not only on adsorption interactions but also on the molecular sieve effect in the micropores and kinetically selective effects. Additional interactions with the mobile phase components alter the thermodynamic parameters of the adsorbates interaction with the zeolite, decrease effective pore size, and hinder the diffusion of the separated compounds into the adsorbent’s pores. Despite these challenges, zeolites remain promising adsorbents due to their strictly determined pore size (<i>d</i><sub>pore</sub>) and geometry, as well as their customizable polarities, which ensure high selectivity for the separation of low-molecular-weight compounds. The most promising zeolites for HPLC are wide-pore zeolites (<i>d</i><sub>pore</sub> 0.6–0.8 nm) with 8, 10, 12, and 14-member ring channels. This review offers a concise overview of the classification, composition, and structure of zeolites and their impact on the adsorption properties of these adsorbents. Data on the use of zeolites in HPLC are also systematized.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":1.0,"publicationDate":"2024-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142518398","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-22DOI: 10.1134/S1061934824700850
A. S. Gubin, A. A. Kushnir, P. T. Sukhanov
An original bench-scale installation based on the principles of online magnetic solid-phase extraction is developed. The setup includes a borosilicate glass column packed with Fe3O4@MIP-BPA, which is fixed with two neodymium magnets. Compared to using one magnet, a design with two magnets ensures the uniform distribution of the sorbent over the entire cross-section of the column. The highest concentration factors (EF = 3216) and the degree of desorption of bisphenol A (BPA) are achieved, respectively, at a volumetric solution flow rate (W) of 2.0 mL/min and with eluting BPA with methanol (W = 0.4 mL/min). The determination of BPA in concentrates from model media by GC−MS provides high sensitivity of the developed method for determining BPA. In analyzing model solutions prepared in distilled water, the limit of detection (LOD) is 0.3 ng/L. In analyzing river water, the LOD increases by approximately 2 times. In analyzing soils, LOD = 2.2 ng/kg dry weight. Soils, compared to water bodies, contain a larger number of interfering components; the sensitivity of the method is reduced by 7–8 times. Bottom sediments are even more contaminated; the LOD more than doubles compared to the determination of BPA in soils.
根据在线磁性固相萃取的原理,开发了一种独创的台式装置。该装置包括一个装有 Fe3O4@MIP-BPA 的硼硅玻璃柱,柱子用两块钕磁铁固定。与使用一块磁铁相比,使用两块磁铁的设计可确保吸附剂在整个色谱柱横截面上的均匀分布。在体积溶液流速(W)为 2.0 mL/min 和用甲醇洗脱双酚 A 时(W = 0.4 mL/min),双酚 A 的浓度系数(EF = 3216)和解吸程度分别达到最高。利用气相色谱-质谱法测定模型介质浓缩物中的双酚 A,为所开发的双酚 A 测定方法提供了高灵敏度。在分析蒸馏水制备的模型溶液时,检测限(LOD)为 0.3 ng/L。在分析河水时,检测限提高了约 2 倍。在分析土壤时,检测限 = 2.2 纳克/千克干重。与水体相比,土壤中含有更多的干扰成分;该方法的灵敏度降低了 7-8 倍。底层沉积物的污染程度更高;与测定土壤中的双酚 A 相比,检测限增加了一倍多。
{"title":"Online Preconcentration of Bisphenol A on a Magnetic Molecularly Imprinted Sorbent and its Determination in Natural Media","authors":"A. S. Gubin, A. A. Kushnir, P. T. Sukhanov","doi":"10.1134/S1061934824700850","DOIUrl":"10.1134/S1061934824700850","url":null,"abstract":"<p>An original bench-scale installation based on the principles of online magnetic solid-phase extraction is developed. The setup includes a borosilicate glass column packed with Fe<sub>3</sub>O<sub>4</sub>@MIP-BPA, which is fixed with two neodymium magnets. Compared to using one magnet, a design with two magnets ensures the uniform distribution of the sorbent over the entire cross-section of the column. The highest concentration factors (<i>EF</i> = 3216) and the degree of desorption of bisphenol A (<b>BPA</b>) are achieved, respectively, at a volumetric solution flow rate (<i>W</i>) of 2.0 mL/min and with eluting BPA with methanol (<i>W</i> = 0.4 mL/min). The determination of BPA in concentrates from model media by GC−MS provides high sensitivity of the developed method for determining BPA. In analyzing model solutions prepared in distilled water, the limit of detection (<b>LOD</b>) is 0.3 ng/L. In analyzing river water, the LOD increases by approximately 2 times. In analyzing soils, LOD = 2.2 ng/kg dry weight. Soils, compared to water bodies, contain a larger number of interfering components; the sensitivity of the method is reduced by 7–8 times. Bottom sediments are even more contaminated; the LOD more than doubles compared to the determination of BPA in soils.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":1.0,"publicationDate":"2024-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142518435","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-22DOI: 10.1134/S1061934824700758
A. E. Margaryan, I. A. Platonov, I. N. Kolesnichenko, E. A. Novikova, A. S. Karsunkina
A technology is developed for manufacturing planar microfluidic chips (MFCs) based on Silgard 8040, encompassing template fabrication, mold production, sealing, and adsorbent filling. These MFCs, filled with a Porapak-Q adsorbent, facilitate sample preparation and calibration under uniform conditions, integrating both sample collection and preconcentration stages. Experimental investigations have identified optimal conditions for acetone preconcentration using Silgard 8040-based MFCs, achieving a maximum concentration factor of 43 at adsorption temperature (Tads) of 0°C, desorption temperature (Tdes) of 70°C, adsorption volume (Vads) of 45 mL, and desorption time (tdes) of 1 s. The feasibility of using MFCs for sample collection and preparation, taking into account sample storage time, has been evaluated. The procedure maintains accuracy within 6–10% over 8 h without a necessity for additional drying of the collected samples from exhaled air.
{"title":"Silagerm 8040-Based Planar Microfluidic Chips for Sampling and Sample Preparation in the Analysis of Gas Media","authors":"A. E. Margaryan, I. A. Platonov, I. N. Kolesnichenko, E. A. Novikova, A. S. Karsunkina","doi":"10.1134/S1061934824700758","DOIUrl":"10.1134/S1061934824700758","url":null,"abstract":"<p>A technology is developed for manufacturing planar microfluidic chips (MFCs) based on Silgard 8040, encompassing template fabrication, mold production, sealing, and adsorbent filling. These MFCs, filled with a Porapak-Q adsorbent, facilitate sample preparation and calibration under uniform conditions, integrating both sample collection and preconcentration stages. Experimental investigations have identified optimal conditions for acetone preconcentration using Silgard 8040-based MFCs, achieving a maximum concentration factor of 43 at adsorption temperature (<i>T</i><sub>ads</sub>) of 0°C, desorption temperature (<i>T</i><sub>des</sub>) of 70°C, adsorption volume (<i>V</i><sub>ads</sub>) of 45 mL, and desorption time (<i>t</i><sub>des</sub>) of 1 s. The feasibility of using MFCs for sample collection and preparation, taking into account sample storage time, has been evaluated. The procedure maintains accuracy within 6–10% over 8 h without a necessity for additional drying of the collected samples from exhaled air.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":1.0,"publicationDate":"2024-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142518395","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-22DOI: 10.1134/S1061934824700771
I. I. Timofeeva, M. A. Kochetkova, D. D. Dvoinykh, Ya. V. Safinskaya, E. A. Zubakina, A. V. Bulatov
A micellar microextraction technique has been developed for the preconcentration and spectrophotometric determination of phosphate ions in aqueous media. This method is based on the formation of a reduced form of molybdophosphoric heteropolyacid and its extraction from the aqueous phase into a supramolecular solvent. The supramolecular solvent phase is formed in situ by introducing an amphiphile and a coacervation agent into the acidic aqueous phase. The feasibility of using biodegradable alkyl polyglucoside (C8–C10) as an amphiphile and carboxylic acids as coacervation agents has been investigated. In the acidic medium required for the formation of the reduced form of molybdophosphoric heteropolyacid, the phase of the supramolecular solvent is separated. The maximum absorbance of the extract is achieved using pivalic acid as the coacervation agent. The procedure is characterized by the limit of detection (3σ) for phosphate ions 5 µg/L. The technique is environmentally friendly and does not require the use of expensive equipment.
{"title":"Micellar Microextraction with Alkyl Polyglucosides for the Preconcentration and Spectrophotometric Determination of Phosphate Ions in Aqueous Media","authors":"I. I. Timofeeva, M. A. Kochetkova, D. D. Dvoinykh, Ya. V. Safinskaya, E. A. Zubakina, A. V. Bulatov","doi":"10.1134/S1061934824700771","DOIUrl":"10.1134/S1061934824700771","url":null,"abstract":"<p>A micellar microextraction technique has been developed for the preconcentration and spectrophotometric determination of phosphate ions in aqueous media. This method is based on the formation of a reduced form of molybdophosphoric heteropolyacid and its extraction from the aqueous phase into a supramolecular solvent. The supramolecular solvent phase is formed in situ by introducing an amphiphile and a coacervation agent into the acidic aqueous phase. The feasibility of using biodegradable alkyl polyglucoside (C<sub>8</sub>–C<sub>10</sub>) as an amphiphile and carboxylic acids as coacervation agents has been investigated. In the acidic medium required for the formation of the reduced form of molybdophosphoric heteropolyacid, the phase of the supramolecular solvent is separated. The maximum absorbance of the extract is achieved using pivalic acid as the coacervation agent. The procedure is characterized by the limit of detection (3σ) for phosphate ions 5 µg/L. The technique is environmentally friendly and does not require the use of expensive equipment.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":1.0,"publicationDate":"2024-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142518359","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-22DOI: 10.1134/S1061934824700898
M. Amayreh, M. Esaifan, M. K. Hourani
The presented work focused on the preparation of a voltammetric sensor for hydroquinone (HQ) determination using a polycrystalline platinum electrode modified with Alizarin Red S (ARS). The electrode was prepared by electropolymerization of ARS on a platinum electrode through the application of 100 cyclic voltammetric segments between –0.4 and 1.2 V against Ag/AgCl (quasi-reference electrode). The modified poly (ARS)-Pt electrode was characterized in terms of stability and cyclic voltammetric behavior as a sensor for HQ in aqueous media. The modified electrode showed excellent stability and higher current than the unmodified electrode for the electrooxidation of HQ. Thus, the oxidation of HQ at poly (ARS)-Pt electrode exhibits notable electrocatalytic performance. The limit of detection is 0.16 µM, and the standard curve exhibits a linear relationship over the range from 0.25 to 15 µM (R2 = 0.999). Investigation of the response to some potential interferences indicated that the electrode is unresponsive to Na+, K+, Mg2+, Ca2+, Zn2+, Mn2+, Mo2+, Co2+, Bi2+, Cd2+, Ni2+, Al3+, ({text{NO}}_{3}^{ - }), ({text{SO}}_{4}^{{2 - }}), Cl–, phenol and resorcinol, but shows marginal change towards Hg2+ and Cu2+. Recovery tests indicated recovery values between 97.0% and 100.81% when analyzing real samples at the modified electrode.
{"title":"Voltammetric Determination of Hydroquinone in Water Samples Using Platinum Electrode Modified with Poly(Alizarin Red S)","authors":"M. Amayreh, M. Esaifan, M. K. Hourani","doi":"10.1134/S1061934824700898","DOIUrl":"10.1134/S1061934824700898","url":null,"abstract":"<p>The presented work focused on the preparation of a voltammetric sensor for hydroquinone (<b>HQ</b>) determination using a polycrystalline platinum electrode modified with Alizarin Red S (<b>ARS</b>). The electrode was prepared by electropolymerization of ARS on a platinum electrode through the application of 100 cyclic voltammetric segments between –0.4 and 1.2 V against Ag/AgCl (quasi-reference electrode). The modified poly (ARS)-Pt electrode was characterized in terms of stability and cyclic voltammetric behavior as a sensor for HQ in aqueous media. The modified electrode showed excellent stability and higher current than the unmodified electrode for the electrooxidation of HQ. Thus, the oxidation of HQ at poly (ARS)-Pt electrode exhibits notable electrocatalytic performance. The limit of detection is 0.16 µM, and the standard curve exhibits a linear relationship over the range from 0.25 to 15 µM (<i>R</i><sup>2</sup> = 0.999). Investigation of the response to some potential interferences indicated that the electrode is unresponsive to Na<sup>+</sup>, K<sup>+</sup>, Mg<sup>2+</sup>, Ca<sup>2+</sup>, Zn<sup>2+</sup>, Mn<sup>2+</sup>, Mo<sup>2+</sup>, Co<sup>2+</sup>, Bi<sup>2+</sup>, Cd<sup>2+</sup>, Ni<sup>2+</sup>, Al<sup>3+</sup>, <span>({text{NO}}_{3}^{ - })</span>, <span>({text{SO}}_{4}^{{2 - }})</span>, Cl<sup>–</sup>, phenol and resorcinol, but shows marginal change towards Hg<sup>2+</sup> and Cu<sup>2+</sup>. Recovery tests indicated recovery values between 97.0% and 100.81% when analyzing real samples at the modified electrode.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":1.0,"publicationDate":"2024-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142518437","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-22DOI: 10.1134/S1061934824700801
V. I. Mardanova, Kh. D. Nagiev, F. M. Chyragov
Complex formation of vanadium(V) with 4-(2',3',4'-trihydroxyphenyl)-3-nitro-5-sulfoazobenzene (R) in the presence of cationic surfactants (CS), cetylpyridinium chloride (CPCl), cetylpyridinium bromide (CPBr), and cetyltrimethylammonium bromide (CTMABr), is studied. Vanadium(V) and R form a colored complex at a component ratio of 1 : 2 and pH of 5.0–5.5. The absorbance maximum of the complex is at 449 nm, while the reagent under these conditions absorbs light at 395 nm. In the presence of cationic surfactants, mixed-ligand complexes with a component ratio of V(V) : R : CS = 1 : 2 : 2 are formed, which results in a bathochromic shift of the absorbance maximum. Additionally, the pH value for the maximum complex formation shifts to a more acidic medium compared to the homoligand V(V)–R complex. The absorbance of the V(V) : R : CPCl, V(V): R : CPBr, and V(V) : R : CTMABr complexes is maximal at 457, 461, and 466 nm, respectively. The yield of these complexes is the highest at pH of 3.5–4.0 for VV(V) : R : CPCl and V(V): R : CPBr, and at a pH of 2.5–3.0 for V(V) : R : CTMABr. The formation of both homoligand and mixed-ligand vanadium(V) complexes depends on the reaction time, temperature, and concentrations of the reacting components. The determined stability constants indicate the high stability of the resulting mixed-ligand complexes. The specific conductivity of the complexes under the optimal conditions of complex formation was determined using conductometric titration. Calibration curves for the determination of vanadium(V) as homoligand and mixed-ligand complexes are linear. The effect of foreign ions and masking agents on the determination of V(V) as homoligand and mixed-ligand complexes was analyzed; it was shown that the presence of cationic surfactants significantly increases the selectivity of the reaction. An analysis of water samples from Lake Khanbulan, Lankaran District, Azerbaijan Republic using the developed procedure showed the presence of small amounts of vanadium(V).
{"title":"Interaction of Vanadium(V) with 4-(2',3',4'-Trihydroxyphenyl)-3-Nitro-5-Sulfoazobenzene in the Presence of Cationic Surfactants","authors":"V. I. Mardanova, Kh. D. Nagiev, F. M. Chyragov","doi":"10.1134/S1061934824700801","DOIUrl":"10.1134/S1061934824700801","url":null,"abstract":"<p>Complex formation of vanadium(V) with 4-(2',3',4'-trihydroxyphenyl)-3-nitro-5-sulfoazobenzene (R) in the presence of cationic surfactants (CS), cetylpyridinium chloride (CPCl), cetylpyridinium bromide (CPBr), and cetyltrimethylammonium bromide (CTMABr), is studied. Vanadium(V) and R form a colored complex at a component ratio of 1 : 2 and pH of 5.0–5.5. The absorbance maximum of the complex is at 449 nm, while the reagent under these conditions absorbs light at 395 nm. In the presence of cationic surfactants, mixed-ligand complexes with a component ratio of V(V) : R : CS = 1 : 2 : 2 are formed, which results in a bathochromic shift of the absorbance maximum. Additionally, the pH value for the maximum complex formation shifts to a more acidic medium compared to the homoligand V(V)–R complex. The absorbance of the V(V) : R : CPCl, V(V): R : CPBr, and V(V) : R : CTMABr complexes is maximal at 457, 461, and 466 nm, respectively. The yield of these complexes is the highest at pH of 3.5–4.0 for VV(V) : R : CPCl and V(V): R : CPBr, and at a pH of 2.5–3.0 for V(V) : R : CTMABr. The formation of both homoligand and mixed-ligand vanadium(V) complexes depends on the reaction time, temperature, and concentrations of the reacting components. The determined stability constants indicate the high stability of the resulting mixed-ligand complexes. The specific conductivity of the complexes under the optimal conditions of complex formation was determined using conductometric titration. Calibration curves for the determination of vanadium(V) as homoligand and mixed-ligand complexes are linear. The effect of foreign ions and masking agents on the determination of V(V) as homoligand and mixed-ligand complexes was analyzed; it was shown that the presence of cationic surfactants significantly increases the selectivity of the reaction. An analysis of water samples from Lake Khanbulan, Lankaran District, Azerbaijan Republic using the developed procedure showed the presence of small amounts of vanadium(V).</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":1.0,"publicationDate":"2024-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142518363","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-03DOI: 10.1134/S1061934824700655
N. O. Goncharov, V. V. Tolmacheva, T. V. Lazarevich, A. O. Melekhin, I. D. Puryskin, V. V. Apyari, S. G. Dmitrienko
A magnetic solid-phase extraction method with the dispersion of magnetic hypercrosslinked polystyrene (MHCPS) by carbon dioxide is proposed for the extraction and preconcentration of amphenicols (chloramphenicol, florfenicol, and thiamphenicol) from honey and milk before their determination by HPLC–MS/MS. Effervescent tablets, consisting of sodium bicarbonate, citric acid, and MHCPS in the case of honey and sodium bicarbonate and MHCPS in the case of milk, were used. The conditions for obtaining tablets were selected (the amount and ratio of the acid, base, and MHCPS in the composition of a tablet and its mass), ensuring the quantitative release of amphenicols. Procedures for the determination of amphenicols in honey and milk with the dispersion of the sorbent by carbon dioxide and the subsequent determination of the compounds by HPLC–MS/MS are developed. The limits of detection are 0.3–1 and 0.02–0.05 μg/kg for honey and milk, respectively.
{"title":"Magnetic Solid-Phase Extraction with Dispersion of Magnetic Hypercrosslinked Polystyrene by Carbon Dioxide for the Extraction of Amphenicols from Honey and Milk in Their Determination by HPLC–MS/MS","authors":"N. O. Goncharov, V. V. Tolmacheva, T. V. Lazarevich, A. O. Melekhin, I. D. Puryskin, V. V. Apyari, S. G. Dmitrienko","doi":"10.1134/S1061934824700655","DOIUrl":"10.1134/S1061934824700655","url":null,"abstract":"<p>A magnetic solid-phase extraction method with the dispersion of magnetic hypercrosslinked polystyrene (<b>MHCPS</b>) by carbon dioxide is proposed for the extraction and preconcentration of amphenicols (chloramphenicol, florfenicol, and thiamphenicol) from honey and milk before their determination by HPLC–MS/MS. Effervescent tablets, consisting of sodium bicarbonate, citric acid, and MHCPS in the case of honey and sodium bicarbonate and MHCPS in the case of milk, were used. The conditions for obtaining tablets were selected (the amount and ratio of the acid, base, and MHCPS in the composition of a tablet and its mass), ensuring the quantitative release of amphenicols. Procedures for the determination of amphenicols in honey and milk with the dispersion of the sorbent by carbon dioxide and the subsequent determination of the compounds by HPLC–MS/MS are developed. The limits of detection are 0.3–1 and 0.02–0.05 μg/kg for honey and milk, respectively.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":1.0,"publicationDate":"2024-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142177614","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-03DOI: 10.1134/S1061934824700588
T. A. Kuchmenko, D. Yu. Vandyshev, V. N. Skorikov, R. U. Umarkhanov, Kh. S. Shikhaliev, P. V. Seredin, V. V. Yagov, V. I. Mikhalev
The results of an experiment assessing the applicability of solutions of 6-oxo-2-phenylimidazo[1,2-b]pyrido[4,3-e][1,2,4]triazine-7(6H)-yl)acetic acid on plates and cellulose substrates for detecting excessive levels of volatile organic compounds associated with endometritis inflammation relative to biologically normal levels are considered. The fluorescent properties of the dye are studied using gynecological mucus from cows collected in various periods (pre- and post-partum) and nasal mucus from newborn calves. The test system responses were compared with clinically established diagnoses and the results of a microbiological study. An evaluation of the test systems revealed a false positive rate of no more than 11% and a false negative rate of 2%. Other characteristics, such as specificity, accuracy, and precision of the test systems based on 6-oxo-2-phenylimidazo[1,2-b]pyrido[4,3-e][1,2,4]triazine-7(6H)-yl)acetic acid were also assessed. The potential application of this fluorophore to the rapid on-site diagnosis of endometritis inflammation in cows is considered promising based on these findings.
{"title":"Azolotriazine-Based Fluorescent Test Systems for the Field Diagnosis of Endometritis in Cows","authors":"T. A. Kuchmenko, D. Yu. Vandyshev, V. N. Skorikov, R. U. Umarkhanov, Kh. S. Shikhaliev, P. V. Seredin, V. V. Yagov, V. I. Mikhalev","doi":"10.1134/S1061934824700588","DOIUrl":"10.1134/S1061934824700588","url":null,"abstract":"<p>The results of an experiment assessing the applicability of solutions of 6-oxo-2-phenylimidazo[1,2-<i>b</i>]pyrido[4,3-<i>e</i>][1,2,4]triazine-7(6<i>H</i>)-yl)acetic acid on plates and cellulose substrates for detecting excessive levels of volatile organic compounds associated with endometritis inflammation relative to biologically normal levels are considered. The fluorescent properties of the dye are studied using gynecological mucus from cows collected in various periods (pre- and post-partum) and nasal mucus from newborn calves. The test system responses were compared with clinically established diagnoses and the results of a microbiological study. An evaluation of the test systems revealed a false positive rate of no more than 11% and a false negative rate of 2%. Other characteristics, such as specificity, accuracy, and precision of the test systems based on 6-oxo-2-phenylimidazo[1,2-<i>b</i>]pyrido[4,3-<i>e</i>][1,2,4]triazine-7(6<i>H</i>)-yl)acetic acid were also assessed. The potential application of this fluorophore to the rapid on-site diagnosis of endometritis inflammation in cows is considered promising based on these findings.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":1.0,"publicationDate":"2024-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142177605","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}