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An Easily Operated Signal Amplification Sensor System for the Determination of Chloramphenicol Residues 用于测定氯霉素残留量的易操作信号放大传感器系统
IF 1 4区 化学 Q4 CHEMISTRY, ANALYTICAL Pub Date : 2024-12-14 DOI: 10.1134/S1061934824701326
Fengxia Cui, Ying Zhang, Yutong Liu, Hao Li

Misuse of chloramphenicol (CAP) could lead to its residue in animal-sourced food and subsequently harm human health through the food chain. Therefore, it is urgently needed to effectively determine CAP residues in animal-sourced food. Here, an easily operated target recycling strategy for the determination of CAP was developed based on a CAP-specific aptamer. The CAP-specific aptamer was hybridized with a complementary short chain modified with fluorescent and quenching groups at both ends. Upon addition of CAP, the aptamer would be separated from its complementary probe and bind with CAP. The fluorescent and quenching groups labeled on the complementary probe were separated by exonuclease I (Exo I) digestion to release a fluorescent signal. Meanwhile, Exo I also digested the aptamer, and CAP was released from the complex, triggering the determination signal amplification based on CAP recycling. Factors (i.e., NaCl concentration and Exo I digestion time) that would affect the determination performance of this sensor system were optimized. Under the optimized conditions, the developed sensor system exhibited high determination sensitivity toward CAP with a limit of detection of 0.08 ng/mL (linear range from 0.1 to 5 ng/mL). Moreover, this sensor system was applied to determine CAP in real spiked milk, and the recovery rates ranged from 97.2 to 100.0%. Meanwhile, this sensor system also suggested cost efficiency with a determination cost of only $0.29 per sample. Results presented here and the high specificity of the aptamer suggested by the previous work indicated the application potential of this developed aptamer-based sensor system for the determination of CAP residue in animal-sourced food.

氯霉素(CAP)的滥用可能导致其残留在动物源性食品中,并随后通过食物链危害人类健康。因此,迫切需要有效地检测动物源性食品中CAP的残留。在此,基于CAP特异性适配体,开发了一种易于操作的目标回收策略,用于确定CAP。将cap特异性适配体与互补短链杂交,并在两端修饰荧光基团和猝灭基团。添加CAP后,适体将与其互补探针分离并与CAP结合。标记在互补探针上的荧光基团和猝灭基团通过外切酶I (Exo I)酶切分离,释放荧光信号。同时,Exo I也消化了适体,CAP从复合物中释放出来,触发基于CAP循环的测定信号放大。对影响该传感器系统测定性能的因素(即NaCl浓度和Exo I消解时间)进行了优化。在优化条件下,该传感器系统对CAP的检测灵敏度较高,检出限为0.08 ng/mL (0.1 ~ 5 ng/mL线性范围内)。将该传感器系统应用于实际加标牛奶中CAP的测定,回收率为97.2 ~ 100.0%。同时,该传感器系统还具有成本效益,每个样品的检测成本仅为0.29美元。本研究的结果和先前研究提出的适配体的高特异性表明,该基于适配体的传感器系统在动物源食品中CAP残留检测方面具有应用潜力。
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引用次数: 0
Optimizing Fabrication Method and Surface Modification of Polyvinyl Acetate-Benzophenone Emission Filters for Complementary Metal-Oxide-Semiconductor Imager Chips towards Biosensing Applications 面向生物传感应用的互补金属-氧化物-半导体成像仪芯片中聚乙烯醇-二苯甲酮发射滤波器的优化制备方法及表面改性
IF 1 4区 化学 Q4 CHEMISTRY, ANALYTICAL Pub Date : 2024-12-14 DOI: 10.1134/S1061934824701363
Narayan Yadav, Pooja Kumari, Snehlata Yadav, Sushmitha Paulraj, Parul Chaurasia, Aftab Anwar, Sanjeev Kumar Mahto

Several techniques are available to determine an analyte, but the most preferred technique is fluorescence-based sensing owing to its sensitivity and selectivity. One of the main components of fluorescent-based sensors is a filter that allows a specific range of wavelengths to pass through and reach the sensing element. Existing filters still lack certain aspects such as durability, interference, cost, integration with a sensing element, biocompatibility, etc. This research aims to design and develop a polyvinyl acetate (PVAc)-benzophenone-based emission filter by spin coating and integrating it with a complementary metal-oxide semiconductor imaging sensor for use as a portable biochemical sensing device. In addition, the fabricated filter is intended to allow the conjugation of recognition elements necessary for biosensing using plasma oxidation. In this study, PVAc and benzophenone concentrations were optimized to fabricate an emission filter (EF) with precise thickness and uniformity. Subsequently, the fabricated EF underwent analysis using a single-beam UV-Vis spectrophotometer. Additionally, plasma treatment was administered to the EF, enabling further examination using fluorescein isothiocyanate dye under a fluorescent microscope. These examinations collectively suggest that the prepared filter possesses dual properties, i.e., it not only serves as an emission filter but also facilitates surface modification through plasma oxidation for the conjugation of chemical groups that can selectively bind to target analytes for biosensing purposes.

有几种技术可用于确定分析物,但由于其灵敏度和选择性,最优选的技术是基于荧光的传感。基于荧光的传感器的主要组成部分之一是一个过滤器,它允许特定范围的波长通过并到达传感元件。现有的过滤器仍然缺乏某些方面,如耐用性、干扰、成本、与传感元件的集成、生物相容性等。本研究旨在通过自旋镀膜的方法,设计和开发一种基于聚醋酸乙烯酯(PVAc)-二苯甲酮的发射滤波器,并将其与互补金属氧化物半导体成像传感器集成,作为便携式生化传感装置。此外,所制备的过滤器旨在允许使用等离子体氧化进行生物传感所需的识别元件的偶联。在本研究中,优化了聚乙烯醇和二苯甲酮的浓度,制备了具有精确厚度和均匀性的发射滤光片。随后,用单束紫外-可见分光光度计对制备的EF进行分析。此外,对EF进行血浆治疗,以便在荧光显微镜下使用异硫氰酸荧光素染料进行进一步检查。这些试验共同表明,所制备的过滤器具有双重性质,即,它不仅可以作为发射过滤器,还可以通过等离子体氧化促进表面修饰,以偶联化学基团,这些化学基团可以选择性地结合到目标分析物上,用于生物传感目的。
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引用次数: 0
Erratum to: Novel Highly Hydrophilic Resins with Attached Polymer Layers for Liquid Chromatography 勘误:用于液相色谱的附着聚合物层的新型高亲水性树脂
IF 1 4区 化学 Q4 CHEMISTRY, ANALYTICAL Pub Date : 2024-12-14 DOI: 10.1134/S1061934824120013
A. V. Gorbovskaia, A. A. Timichev, A. V. Chernobrovkina, A. S. Uzhel, O. A. Shpigun
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引用次数: 0
Ultrasound-Assisted Extraction Combined with Dispersive Liquid-Liquid Microextraction Using Low-Density Solvent—a Novel Approach to Determine Fenvalerate in Strawberry Samples 超声辅助萃取结合使用低密度溶剂的分散液-液微萃取--测定草莓样品中氰戊菊酯含量的新方法
IF 1 4区 化学 Q4 CHEMISTRY, ANALYTICAL Pub Date : 2024-12-14 DOI: 10.1134/S1061934824701272
Mohammad Rezaee

A new, fast, and environmentally friendly method based on ultrasound-assisted extraction combined with dispersive liquid-liquid microextraction using a low-density solvent was developed and optimized for assessing the levels of fenvalerate in strawberry samples. Variables affecting the performance of both steps were thoroughly investigated. Under the optimum conditions, relative recoveries for strawberry samples were in the range of 88.0–98.0%. The calibration graph was linear in the range of 10–1000 µg/kg, and the limits of detection and quantification were 3 and 10 µg/kg, respectively. The relative standard deviation for 40.0 µg/kg of fenvalerate in strawberry samples was 8.1% (n = 5). The obtained results show that the proposed method is a fast and simple method for the determination of fenvalerate in strawberry samples.

为了评估草莓样品中氰戊菊酯的含量,研究人员开发并优化了一种新型、快速、环保的方法,该方法基于超声辅助萃取和分散液-液微萃取(使用低密度溶剂)。对影响这两个步骤性能的变量进行了深入研究。在最佳条件下,草莓样品的相对回收率在 88.0-98.0% 之间。校准图在 10-1000 µg/kg 范围内呈线性,检出限和定量限分别为 3 µg/kg 和 10 µg/kg。草莓样品中的氰戊菊酯含量为 40.0 µg/kg 时,相对标准偏差为 8.1%(n = 5)。结果表明,所提出的方法是测定草莓样品中氰戊菊酯含量的一种快速、简便的方法。
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引用次数: 0
Determination of Polystyrene Nanoparticles in Aqueous Solutions by Dual-Beam Thermal Lens Spectrometry 双光束热透镜光谱法测定水溶液中聚苯乙烯纳米颗粒
IF 1 4区 化学 Q4 CHEMISTRY, ANALYTICAL Pub Date : 2024-12-14 DOI: 10.1134/S1061934824701351
V. R. Khabibullin, N. N. Shevchenko, M. A. Proskurnin

Polymer micro- and nanoparticles, commonly known as microplastics, are significant environmental pollutants. Even low concentrations of microplastics can affect ecosystems and human health, underscoring the urgent need in detecting these particles in low concentrations while simultaneously assessing the physicochemical parameters of the studied systems. Thermal lens spectrometry (TLS) has effectively detected polystyrene particles measuring 65 and 80 nm within a concentration range of 0.0005–0.15 mg/L in their aqueous dispersions. The comprehensive TLS data also facilitated the evaluation of the thermal diffusivity of these solutions. An increase in the concentration of polystyrene nanoparticles in water results in a nonlinear change in thermal diffusivity.

聚合物微粒和纳米微粒(俗称微塑料)是重要的环境污染物。即使是低浓度的微塑料也会影响生态系统和人类健康,因此迫切需要在检测低浓度微粒的同时评估所研究系统的理化参数。热透镜光谱法(TLS)可有效检测水分散液中 65 纳米和 80 纳米的聚苯乙烯颗粒,浓度范围为 0.0005-0.15 毫克/升。全面的 TLS 数据还有助于评估这些溶液的热扩散率。聚苯乙烯纳米颗粒在水中浓度的增加会导致热扩散率的非线性变化。
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引用次数: 0
Cloud Point Extraction and Spectrophotometric Determination of Carbendazim Fungicide in Vegetable and Environmental Samples 浊点萃取-分光光度法测定蔬菜和环境样品中多菌灵杀菌剂
IF 1 4区 化学 Q4 CHEMISTRY, ANALYTICAL Pub Date : 2024-12-14 DOI: 10.1134/S1061934824701260
Naruesorn Samanpong, Yuthapong Udnan, Ajchara lmkum Putkum, Wipharat Chuachuad Chaiyasith, Richmond Jerry Ampiah-Bonney

A micelle-mediated cloud point extraction for carbendazim determination in vegetable and environmental samples using UV-Vis spectrophotometry was developed. Parameters of the proposed method (i.e., pH, extraction time, concentration of surfactant, concentration of ferricyanide, concentration of ferric chloride, extraction temperature, and sample volume) were optimized by UV-Vis spectrophotometry. In this study, the developed method was based on the oxidation reaction of carbendazim by the ferric ion (Fe3+) under acidic conditions, combined with potassium ferricyanide (K3[Fe(CN)6]) to form potassium hexacyanoferrate complexes or the Turnbull’s blue product quantitatively. The final products were solubilized into surfactant micelles, and carbendazim was determined by UV-Vis spectrophotometry at 685 nm after cloud point extraction. The analytical performance of the proposed method was obtained under optimal conditions. The limits of detection and quantification were found to be 0.12 and 0.41 mg/L, respectively. Precision factors were expressed as intra-day (1.6%) and inter-day (7.2%) variations over three replications. Furthermore, the proposed method was applied to the determination of carbendazim in environmental samples such as tap water, underground water, surface water, and in vegetable samples such as garlic, shallot, dried chili, celery, and peanuts. Recovery was obtained in the range of 83–113%.

建立了胶束介导的浊点萃取紫外-可见分光光度法测定蔬菜和环境样品中多菌灵的方法。采用紫外可见分光光度法对提取工艺参数(pH、提取时间、表面活性剂浓度、氰化铁浓度、氯化铁浓度、提取温度、样品体积)进行优化。本研究开发的方法是基于铁离子(Fe3+)在酸性条件下对多菌灵的氧化反应,与铁氰化钾(K3[Fe(CN)6])结合,定量生成六氰高铁酸钾配合物或特恩布尔蓝产物。将最终产物溶于表面活性剂胶束中,经浊点萃取,采用紫外可见分光光度法在685 nm处测定多菌灵的含量。在最优条件下,该方法具有良好的分析性能。检测限为0.12 mg/L,定量限为0.41 mg/L。精度因子表示为三个重复的日内(1.6%)和日内(7.2%)变化。此外,该方法还可用于自来水、地下水、地表水等环境样品以及大蒜、大葱、干辣椒、芹菜、花生等蔬菜样品中多菌灵的测定。回收率在83 ~ 113%之间。
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引用次数: 0
Adsorption and Preconcentration of Anionic Azo Dyes on Nanomagnetite Modified with Cationic Polyelectrolytes 阳离子聚电解质修饰的纳米磁铁矿对阴离子偶氮染料的吸附和预富集
IF 1 4区 化学 Q4 CHEMISTRY, ANALYTICAL Pub Date : 2024-12-14 DOI: 10.1134/S1061934824701296
K. O. Kazimirova, S. N. Shtykov

Magnetic nanoparticles of magnetite (MNPs) with surfaces modified by biocompatible cationic polyelectrolytes polyethyleneimine (PEI) and chitosan (CS) are synthesized by the chemical coprecipitation method. The magnetic nanoparticles were characterized by transmission electron microscopy and measurements of zeta (ζ) potential. The initial MNPs exhibit shapes close to spherical, with an average size of 10 ± 3 nm. The immobilization of a polyelectrolyte on the surface of MNPs results in the formation of aggregates with an interconnected porous network (shell) around individual particles with average sizes of 12 ± 2 nm for Fe3O4@PEI and 15 ± 2 nm for Fe3O4@CS, respectively. The effect of various experimental parameters, such as pH, extraction time, amount of adsorbent, and initial concentration of the dye, on the adsorption and desorption of food azo dyes Allura Red AC (E129) and Black Brilliant BN (E151) has been thoroughly investigated. The results demonstrate that, under optimal conditions, the recovery of these dyes from aqueous solutions reaches 96–100%, at a concentration factor of 2.7 × 103 and adsorption capacities of 56 and 94 mg/g for Fe3O4@PEI, and 46 and 69 mg/g for Fe3O4@CS for E129 and E151, respectively. A comparison of the adsorption isotherms and kinetics of the process indicates that the Langmuir model and pseudo-second-order kinetics are preferable for describing the dye adsorption process. In the acidic and neutral pH ranges, electrostatic interactions primarily drive the adsorption process, while in the alkaline region, hydrogen bonding and hydrophobic interactions also play significant roles. The proposed adsorbents can be utilized for both the adsorption and preconcentration of the dyes in chemical analysis and the treatment of wastewaters for the dye removal. The preferred material for use is polyethyleneimine-modified nanomagnetite, which enables the adsorption and preconcentration of dyes across a wide pH range of 6–9.

采用化学共沉淀法合成了表面由生物相容性阳离子聚电解质聚乙烯亚胺(PEI)和壳聚糖(CS)修饰的磁铁矿磁性纳米颗粒(MNPs)。通过透射电子显微镜和ζ (ζ)电位测量对磁性纳米颗粒进行了表征。初始MNPs的形状接近球形,平均尺寸为10±3 nm。将聚电解质固定在MNPs表面,在单个颗粒周围形成具有相互连接的多孔网络(壳)的聚集体,其平均尺寸分别为Fe3O4@PEI(12±2 nm)和Fe3O4@CS(15±2 nm)。研究了pH、萃取时间、吸附剂用量、染料初始浓度等实验参数对食品偶氮染料Allura Red AC (E129)和Black Brilliant BN (E151)吸附和解吸的影响。结果表明,在最佳条件下,E129和E151对Fe3O4@PEI的吸附量分别为56和94 mg/g, Fe3O4@CS的吸附量分别为46和69 mg/g,对E129和E151的回收率为96 ~ 100%。吸附等温线和动力学比较表明,Langmuir模型和拟二级动力学更适合于描述染料吸附过程。在酸性和中性pH范围内,静电相互作用主要驱动吸附过程,而在碱性区域,氢键和疏水相互作用也起重要作用。所述吸附剂既可用于化学分析中染料的吸附和预富集,也可用于废水的脱色处理。首选材料是聚乙烯亚胺修饰的纳米磁铁矿,它可以在6-9的宽pH范围内吸附和预富集染料。
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引用次数: 0
Microextraction-Chromatographic Determination of Furan Derivatives in Transformer Oil 微萃取色谱法测定变压器油中的呋喃衍生物
IF 1 4区 化学 Q4 CHEMISTRY, ANALYTICAL Pub Date : 2024-12-14 DOI: 10.1134/S1061934824701375
P. A. Godunov, A. Yu. Shishov, A. V. Bulatov

A rapid and an environmentally friendly method is developed for the microextraction of furan derivatives from transformer oil for their determination by high-performance liquid chromatography with ultraviolet spectrophotometric detection. Various hydrophilic eutectic solvents were studied as extractants to implement vortex-assisted dispersive liquid–liquid microextraction. The results indicate that a three-component eutectic solvent composed of choline chloride, acetic acid, and water achieves the highest recoveries, ranging from 85 to 96%. The rapid spontaneous phase separation eliminated the need in centrifugation. Limits of detection (3σ) were achieved between 1 and 5 µg/L.

本研究开发了一种快速、环保的方法,用于微萃取变压器油中的呋喃衍生物,并通过高效液相色谱法和紫外分光光度法进行检测。研究了多种亲水共晶溶剂作为萃取剂,以实现涡流辅助分散液-液微萃取。结果表明,由氯化胆碱、乙酸和水组成的三组分共晶溶剂的回收率最高,达到 85% 至 96%。快速的自发相分离消除了离心的需要。检测限 (3σ) 在 1 至 5 µg/L 之间。
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引用次数: 0
Voltammetric DNA Sensors for the DNA Damage Detection Using Poly(Acridine Orange) Coatings Deposited from Reline and Glyceline 基于聚吖啶橙涂层的DNA损伤检测伏安传感器
IF 1 4区 化学 Q4 CHEMISTRY, ANALYTICAL Pub Date : 2024-12-14 DOI: 10.1134/S1061934824701466
A. V. Porfireva, Z. F. Khusnutdinova, G. A. Evtyugin

A voltammetric DNA sensor has been developed to detect DNA damage from calf thymus by measuring changes in redox signals in cyclic voltammograms of poly(Acridine Orange) (PAO) coatings. This polymer was synthesized on a carbon printed electrode from deep eutectic solvents—reline and glyceline—and a phosphate buffer solution. The optimal conditions for immobilizing DNA on each of the polymer coatings have been found. The effect of the polymerization medium on the electrochemical characteristics of the polyacridine dye layer and the polymer sensitivity to the thermal and oxidative damage of DNA has been identified. With the optimal composition of the surface layer the DNA sensor based on poly(Acridine Orange) synthesized from aqueous media (PAO1) reliably detected only chemical DNA oxidation. In contrast, the PAO synthesized from reline (PAO2) and glyceline (PAO3) demonstrated increased sensitivity to the incorporation of calf thymus DNA, which allows to discriminate between native, thermally denatured, and chemically oxidized DNA.

通过测量聚(吖啶橙)(PAO)涂层循环伏安图中氧化还原信号的变化,开发出了一种伏安 DNA 传感器,用于检测小牛胸腺的 DNA 损伤。这种聚合物是用深共晶溶剂--line 和甘氨酸--以及磷酸盐缓冲溶液在碳印刷电极上合成的。在每种聚合物涂层上固定 DNA 的最佳条件已经找到。聚合介质对聚吖啶染料层的电化学特性以及聚合物对 DNA 的热损伤和氧化损伤的敏感性的影响已经确定。在表层成分最佳的情况下,基于水介质合成的聚(吖啶橙)DNA 传感器(PAO1)只能可靠地检测 DNA 的化学氧化。与此相反,由reline(PAO2)和glyceline(PAO3)合成的聚吖啶橙(PAO)对加入小牛胸腺 DNA 的灵敏度更高,可以区分原生 DNA、热变性 DNA 和化学氧化 DNA。
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引用次数: 0
Adsorption Preconcentration of Flavonoids on Ordered Mesoporous Silica Synthesized in the Presence of a Potential Adsorbate 有序介孔二氧化硅合成物在潜在吸附剂作用下对黄酮类化合物的吸附预富集
IF 1 4区 化学 Q4 CHEMISTRY, ANALYTICAL Pub Date : 2024-12-14 DOI: 10.1134/S1061934824701259
A. S. Zavalyueva, S. I. Karpov, V. F. Selemenev

The application of nanostructured adsorbents in sample preparation (extraction and preconcentration) of multicomponent mixtures in the solid-phase extraction of organic compounds is gaining significant interest. This study examines the adsorption properties of ordered mesoporous analogues of SBA-15, synthesized in the presence of quercetin as a potential adsorbate. The work explores the specific features of the adsorption-based recovery and preconcentration of quercetin, dihydroquercetin, naringin, and rutin under dynamic conditions from acetonitrile solutions using the breakthrough curve method. The use of the generalized optimization criterion of adsorption preconcentration CE, within the framework of the Venitsianov–Tsysin model of dynamic adsorption preconcentration, taking into account the limiting (mixed-diffusion) stage of adsorption kinetics, enabled the evaluation of the efficiency of the adsorption preconcentration of flavonoids on the studied adsorbents. The results demonstrate that the use of ordered silica synthesized in the presence of a potential adsorbate significantly enhances concentration efficiency compared to nonstructured silicas or unmodified SBA-15 analogue samples.

纳米结构吸附剂在有机化合物固相萃取中多组分混合物的样品制备(萃取和预富集)中的应用越来越受到人们的关注。本研究考察了在槲皮素存在下合成的SBA-15有序介孔类似物的吸附性能。采用突破曲线法研究了动态条件下从乙腈溶液中吸附回收和富集槲皮素、二氢槲皮素、柚皮素和芦丁的具体特点。在动态吸附预富集的Venitsianov-Tsysin模型框架内,考虑到吸附动力学的极限(混合扩散)阶段,利用吸附预富集CE的广义优化准则,对黄酮类化合物在所研究吸附剂上的吸附预富集效率进行了评价。结果表明,与非结构化二氧化硅或未经改性的SBA-15类似样品相比,在潜在吸附物存在下合成的有序二氧化硅显著提高了浓缩效率。
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引用次数: 0
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Journal of Analytical Chemistry
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