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Ultra-sensitive refractive index detection with gold-coated PCF-based SPR sensor
IF 4.1 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-12-01 DOI: 10.1016/j.talo.2024.100384
Amit Das , Md Abu Huraiya , Vinoth Raj R , Hitoshi Tabata , Sankar Ganesh Ramaraj
This study introduces an innovative photonic crystal fiber (PCF) surface plasmon resonance (SPR) biosensor, notable for its sophisticated design and exceptional performance, utilizing gold as the plasmonic material. The sensor offers an expanded detection range and outstanding sensitivity, operating within a refractive index range of 1.27 to 1.43. It achieves a remarkable wavelength sensitivity of 157,000 nm/RIU with a resolution of 6.37 × 10⁻⁷ RIU and an amplitude sensitivity of 1263 RIU⁻¹ with a resolution of 7.92 × 10⁻⁵ RIU. Additionally, it boasts a figure of merit (FOM) of 1648, underscoring its superior capability in detecting biomolecular interactions. The suggested design is numerically analysed using the finite element method (FEM) of a gold-coated PCF-based SPR sensor designed for detecting changes in the refractive index (RI) within the range of 1.27 to 1.43. This range is related to various biological and chemical samples, including proteins, DNA, and biochemical analytes typically used in biomedical diagnostics and environmental monitoring. The integration of gold plasmonic elements enhances the sensor's sensitivity and stability while extending its detection capabilities across a broader range, allowing for versatile applications in biomedicine, environmental monitoring, and beyond. This research significantly advances optical biosensing technologies by offering a robust platform for high-precision detection across diverse domains. The sensor's advanced design and performance make it an invaluable tool for applications requiring accurate and reliable detection, driving innovations in areas such as biomedical diagnostics, environmental monitoring, food safety, and pharmaceutical quality control.
{"title":"Ultra-sensitive refractive index detection with gold-coated PCF-based SPR sensor","authors":"Amit Das ,&nbsp;Md Abu Huraiya ,&nbsp;Vinoth Raj R ,&nbsp;Hitoshi Tabata ,&nbsp;Sankar Ganesh Ramaraj","doi":"10.1016/j.talo.2024.100384","DOIUrl":"10.1016/j.talo.2024.100384","url":null,"abstract":"<div><div>This study introduces an innovative photonic crystal fiber (PCF) surface plasmon resonance (SPR) biosensor, notable for its sophisticated design and exceptional performance, utilizing gold as the plasmonic material. The sensor offers an expanded detection range and outstanding sensitivity, operating within a refractive index range of 1.27 to 1.43. It achieves a remarkable wavelength sensitivity of 157,000 nm/RIU with a resolution of 6.37 × 10⁻⁷ RIU and an amplitude sensitivity of 1263 RIU⁻¹ with a resolution of 7.92 × 10⁻⁵ RIU. Additionally, it boasts a figure of merit (FOM) of 1648, underscoring its superior capability in detecting biomolecular interactions. The suggested design is numerically analysed using the finite element method (FEM) of a gold-coated PCF-based SPR sensor designed for detecting changes in the refractive index (RI) within the range of 1.27 to 1.43. This range is related to various biological and chemical samples, including proteins, DNA, and biochemical analytes typically used in biomedical diagnostics and environmental monitoring. The integration of gold plasmonic elements enhances the sensor's sensitivity and stability while extending its detection capabilities across a broader range, allowing for versatile applications in biomedicine, environmental monitoring, and beyond. This research significantly advances optical biosensing technologies by offering a robust platform for high-precision detection across diverse domains. The sensor's advanced design and performance make it an invaluable tool for applications requiring accurate and reliable detection, driving innovations in areas such as biomedical diagnostics, environmental monitoring, food safety, and pharmaceutical quality control.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"10 ","pages":"Article 100384"},"PeriodicalIF":4.1,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142747035","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
High-sensitive ethanol gas sensor using Ag modified ZnO nanosheets
IF 4.1 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-12-01 DOI: 10.1016/j.talo.2024.100386
Yi-Hsing Liu , Sheng-Joue Young , Liang-Wen Ji , Yen-Lin Chu , Shoou-Jinn Chang
In this study, an ethanol gas sensor was developed using ZnO nanosheets synthesized through an aqueous solution method, with Ag nanoparticles modified on the surface via chemical reduction to enhance ethanol gas sensing capabilities. We discuss the optimal sensitivity, selectivity, stability and optimal operating temperature conditions of Ag/ZnO samples. The selectivity measurement included methanol, ethanol, isopropanol and propanol, and the results showed that Ag/ZnO sample has the best selectivity for ethanol gas and the best sensitivity to ethanol gas (100 ppm, 28.78) when the device operates at 270 °C compared to ZnO sample (100 ppm, 2.27). The flaky structure of the ZnO nanosheets provides a high surface-to-volume ratio, which is beneficial for gas sensing. The addition of Ag nanoparticles further improves the gas sensor performance due to the Ag nanoparticles can more readily capture electrons. The results indicate that the Ag-modified ZnO nanosheet gas sensor exhibits the highest selectivity, excellent stability, and high responsiveness to ethanol gas compared to the ZnO sensor.
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引用次数: 0
High-throughput detection of bottle materials of agave spirits using 3D-printed cartridges for paper-spray ionization mass spectrometry
IF 4.1 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-12-01 DOI: 10.1016/j.talo.2024.100387
Leonardo Daniel Soto-Rodríguez , Nancy Shyrley García-Rojas , Carmelo Hernández-Caricio , Héctor Guillén-Alonso , Alexander DeLuna , Eugenio Mancera , Robert Winkler
The material of storage containers affects the shelf life and the chemical composition of food. Artisanal agave spirits, such as mezcal and bacanora, might be filled into low-cost plastic bottles that compromise product quality. We developed an analytical platform to identify the bottle materials of agave spirits, which employs 3D-printed cartridges, and the robotic platform Open LabBot/Open SprayBot for paper-spray ionization mass spectrometry (PS-MS). The bottle material of 102 fresh samples could be identified with a 2 % error. Samples stored for two years at −20 °C in glass vials still were classified correctly in 76 % of the cases. Therefore, the spirits still appear adulterated for a prolonged time after re-bottling into inert containers. The measurement time is about 30 s/sample. Thus, the 3D-PS-MS strategy can be applied for the high-throughput screening for bottle materials of agave spirits and other alcoholic beverages.
{"title":"High-throughput detection of bottle materials of agave spirits using 3D-printed cartridges for paper-spray ionization mass spectrometry","authors":"Leonardo Daniel Soto-Rodríguez ,&nbsp;Nancy Shyrley García-Rojas ,&nbsp;Carmelo Hernández-Caricio ,&nbsp;Héctor Guillén-Alonso ,&nbsp;Alexander DeLuna ,&nbsp;Eugenio Mancera ,&nbsp;Robert Winkler","doi":"10.1016/j.talo.2024.100387","DOIUrl":"10.1016/j.talo.2024.100387","url":null,"abstract":"<div><div>The material of storage containers affects the shelf life and the chemical composition of food. Artisanal agave spirits, such as mezcal and bacanora, might be filled into low-cost plastic bottles that compromise product quality. We developed an analytical platform to identify the bottle materials of agave spirits, which employs 3D-printed cartridges, and the robotic platform Open LabBot/Open SprayBot for paper-spray ionization mass spectrometry (PS-MS). The bottle material of 102 fresh samples could be identified with a 2 % error. Samples stored for two years at −20 °C in glass vials still were classified correctly in 76 % of the cases. Therefore, the spirits still appear adulterated for a prolonged time after re-bottling into inert containers. The measurement time is about 30 s/sample. Thus, the 3D-PS-MS strategy can be applied for the high-throughput screening for bottle materials of agave spirits and other alcoholic beverages.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"10 ","pages":"Article 100387"},"PeriodicalIF":4.1,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142747037","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
MCM-41 based dispersive micro-solid phase extraction of selected cephalosporin antibiotic residues from water samples prior to liquid chromatographic quantification 基于 MCM-41 的分散微固相萃取技术在液相色谱定量前萃取水样中的部分头孢菌素类抗生素残留物
IF 4.1 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-11-19 DOI: 10.1016/j.talo.2024.100382
Andisiwe Bangani , Mthokozisi Mnguni , Thollwana Andretta Makhetha , Elisabete Oliveira , José Luis Capelo-Martínez , Carlos Lodeiro , Philiswa Nosizo Nomngongo
The occurrence of antibiotics in water bodies is of concern owing to the serious risk they pose to the environment, water security, aquatic organisms, and human health. In this study, mesoporous silica (MCM-41) nanostructured material was synthesised and characterized by various analytical techniques to determine its morphology and dimension, functional groups, surface charge, and textural properties. The nanostructured MCM-41 was used as an adsorbent in ultrasound-assisted dispersive micro solid-phase extraction (UA-D-µ-SPE) of cefadroxil (CFDX) and cephalexin (CPLX) in water samples. The concentration of the analytes in aqueous solution and real water samples was determined using high-performance liquid chromatography coupled with diode array detection (HPLC-DAD). The developed method for CFDX and CPLX in various water samples exhibited relative linear ranges of 0.1–600 µg/L and 0.1–550 µg/L, respectively, and correlation coefficients ranging from 0.9923–0.9993. Under optimum condition, the UA-D-µ-SPE/HPLC-DAD method displayed low limits of detection (LOD) and quantification (LOQ), with values ranging from 0.02–0.16 µg/L and 0.067–0.53 µg/L, respectively. The investigated intraday and interday accuracy in spiked water samples showed acceptable extraction efficiencies with a range of 73.5–98.1% and a relative standard deviation less than 6.0%. Moreover, the performance of MCM-41 was also assessed for the removal of cephalosporin antibiotics aqueous solutions. The kinetic and isotherm studies revealed that the adsorption process followed pseudo-second order and the Langmuir model, respectively. Furthermore, the maximum adsorption capacities for CFDX and CPLX were 43.2 and 47.8 mg/g. Lastly, the UA-D-µ-SPE/HPLC-DAD method was successfully applied in extracting, preconcentrating, separating and determining CFDX and CPLX in wastewater and surface water samples. These results demonstrated that MCM-41 can be applied in the removal of cephalosporin antibiotics from aquatic environments.
由于抗生素对环境、水安全、水生生物和人类健康构成严重威胁,水体中抗生素的出现令人担忧。本研究合成了介孔二氧化硅(MCM-41)纳米结构材料,并通过各种分析技术确定了其形态和尺寸、官能团、表面电荷和纹理特性。纳米结构 MCM-41 被用作超声辅助分散微固相萃取(UA-D-µ-SPE)的吸附剂,用于萃取水样中的头孢羟氨苄(CFDX)和头孢氨苄(CPLX)。采用高效液相色谱-二极管阵列检测法(HPLC-DAD)测定了水溶液和实际水样中分析物的浓度。所建立的方法在不同水样中CFDX和CPLX的相对线性范围分别为0.1-600 µg/L和0.1-550 µg/L,相关系数为0.9923-0.9993。在最佳条件下,UA-D-µ-SPE/HPLC-DAD 方法的检出限(LOD)和定量限(LOQ)较低,分别为 0.02-0.16 µg/L 和 0.067-0.53 µg/L。在加标水样中进行的日内和日间准确度调查显示,萃取效率在 73.5-98.1% 之间,相对标准偏差小于 6.0%。此外,还评估了 MCM-41 去除头孢类抗生素水溶液的性能。动力学和等温线研究表明,吸附过程分别遵循伪二阶和 Langmuir 模型。此外,CFDX 和 CPLX 的最大吸附容量分别为 43.2 和 47.8 毫克/克。最后,UA-D-µ-SPE/HPLC-DAD 方法成功地用于提取、预浓缩、分离和测定废水和地表水样品中的 CFDX 和 CPLX。这些结果表明,MCM-41 可用于去除水生环境中的头孢类抗生素。
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引用次数: 0
Bone fragility in Type 2 Diabetes Mellitus. Influence of sex and cardiovascular disease in a pilot study using metabolomics 2 型糖尿病患者的骨脆性。一项利用代谢组学进行的试点研究中性别和心血管疾病的影响
IF 4.1 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-11-17 DOI: 10.1016/j.talo.2024.100381
Nicolás Redecilla-Montoya , Cristina García-Fontana , Tomás Clive Barker-Tejeda , Andrea Macías-Camero , Francisco Andújar-Vera , María Fernanda Rey-Stolle , Luis Martínez-Heredia , Iván Iglesias-Baena , Ana Gradillas , Coral Barbas , Beatriz García-Fontana , Manuel Muñoz-Torres , Alma Villaseñor
Type 2 diabetes mellitus (T2DM) is one of the most common worldwide metabolic disorders, characterized by insulin resistance (IR) and defective insulin secretion by pancreatic β-cells which leads to multiple complications such as bone fragility. This complication might be influenced by other factors such as gender and cardiovascular disease (CVD). However, it is unclear why a certain T2DM group develops bone fragility, and what the molecular mechanism is. Metabolomics is a powerful approach to the study of human metabolism, especially in complex diseases such as T2DM. Thus, this study aimed to identify significant metabolites associated with bone fragility in T2DM patients. To achieve this, 81 individuals were enrolled and classified as T2DM patients (D, n=28), T2DM with bone fragility (D-Frag, n=25), or age-matched non-diabetic subjects (ND, n=28) as the control group. Serum samples were collected and analyzed using liquid chromatography and gas chromatography, both coupled to mass spectrometry (LC-MS and GC-MS, respectively). Samples were compared within four different scenarios: 1) the classical comparison of D vs ND to corroborate previous studies; 2) D-Frag vs D to explore the metabolites mainly associated with bone fragility; 3) the same comparison using male data (MD-Frag vs MD) to study as a more homogeneous model of bone fragility as in women, bone fragility could be mainly associated with hormonal stage and pregnancy; and 4) MD-Frag-CVD vs MD-CVD to explore the influence of bone fragility in the male-based model with CVD considering that most of the T2DM patients suffer from CVD. After analysis of these scenarios, our results suggest that acylcarnitines and glycerophospholipids, among other metabolites, are involved in the development of bone fragility in T2DM.
2 型糖尿病(T2DM)是全球最常见的代谢性疾病之一,其特点是胰岛素抵抗(IR)和胰岛β细胞胰岛素分泌缺陷,从而导致骨质脆弱等多种并发症。这种并发症可能受到性别和心血管疾病(CVD)等其他因素的影响。然而,目前还不清楚为什么某些 T2DM 群体会出现骨质疏松,其分子机制又是什么。代谢组学是研究人体代谢,尤其是 T2DM 等复杂疾病代谢的有力方法。因此,本研究旨在确定与 T2DM 患者骨质脆弱相关的重要代谢物。为此,研究人员招募了 81 人,并将其分为 T2DM 患者(D,28 人)、T2DM 伴骨质脆弱者(D-Frag,25 人)或年龄匹配的非糖尿病受试者(ND,28 人)作为对照组。收集血清样本并使用液相色谱法和气相色谱法进行分析,两者均与质谱联用(分别为液相色谱法和气相色谱法)。在四种不同情况下对样本进行比较:1)D 与 ND 的经典比较,以证实先前的研究;2)D-Frag 与 D 的比较,以探索主要与骨脆性相关的代谢物;3)使用男性数据(MD-Frag 与 MD)进行相同的比较,以研究骨脆性的更同质模型,因为在女性中,骨脆性可能主要与荷尔蒙阶段和妊娠有关;4)MD-Frag-CVD 与 MD-CVD,以探索骨脆性在以男性为基础的心血管疾病模型中的影响,因为大多数 T2DM 患者都患有心血管疾病。对这些方案进行分析后,我们的结果表明,酰基肉碱和甘油磷脂等代谢物参与了 T2DM 骨脆性的形成。
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引用次数: 0
Molecularly imprinted biomimetic plasmonic sensor decorated with gold nanoparticles for selective and sensitive detection of bisphenol A 用金纳米粒子装饰的分子印迹仿生质子传感器,用于选择性灵敏检测双酚 A
IF 4.1 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-11-13 DOI: 10.1016/j.talo.2024.100379
Ilgım Göktürk , Süleyman Aşır , Deniz Türkmen , Adil Denizli , Fatma Yılmaz
Molecularly imprinted polymers inspired by antigen-antibody interactions have received substantial interest as a biomimetic artificial receptor system in environmental applications. Herein, we present a molecularly imprinted surface plasmon resonance sensor integrated with gold nanoparticles for the identification of bisphenol A (BPA), an endocrine-disrupting chemical. We synthesized BPA-imprinted nanofilm consisting of amino acid-based functional monomers to selectively detect BPA from synthetic wastewater samples. BPA-spiked synthetic wastewater samples were analyzed to ensure the method's reliability and feasibility. Under ideal conditions, the suggested approach performed well in terms of analytical performance to bisphenol A, with a wide linear range of 0.1 to 10 µg/L and LOD of 10 ng/L. The sensor results align well with the Langmuir adsorption model. It has also been shown that repeated use of the sensor can be achieved. According to selectivity studies, bisphenol A adsorbed within the imprinted cavities favorably compared to 4-nitrophenol and phenol. The produced bisphenol A-imprinted surface plasmon resonance sensor provides improved sensitivity based on the signal amplification strategy, unconjugated sensing without the need for labelling, real-time sensing, low sample consumption rates, quantifiable assessment, and outstanding kinetic rate constant calculation in actual samples. Also, because the produced sensor is reusable with relative standard deviations (RSD)<1.25, indicating the sensor's precision, the surface plasmon resonance-based biomimetic BPA sensor is simple to practice and a cost-effective option.
受抗原-抗体相互作用的启发,分子印迹聚合物作为一种生物仿生人工受体系统在环境应用中受到了广泛关注。在此,我们介绍了一种与金纳米粒子集成的分子印迹表面等离子体共振传感器,用于识别干扰内分泌的化学物质双酚 A(BPA)。我们合成了由氨基酸功能单体组成的双酚 A 压印纳米薄膜,可选择性地检测合成废水样品中的双酚 A。为了确保该方法的可靠性和可行性,我们对添加了双酚 A 的合成废水样品进行了分析。在理想条件下,所建议的方法对双酚 A 的分析性能良好,线性范围为 0.1 至 10 µg/L,LOD 为 10 ng/L。传感器的结果与 Langmuir 吸附模型十分吻合。研究还表明,该传感器可以重复使用。根据选择性研究,与 4-硝基苯酚和苯酚相比,双酚 A 在压印腔内的吸附效果更好。这种双酚 A 印迹表面等离子体共振传感器采用信号放大策略,提高了灵敏度,无需标记即可实现非共轭传感,具有实时传感、低样品消耗率、可量化评估和出色的实际样品动力学速率常数计算等特点。此外,由于生产的传感器可重复使用,相对标准偏差 (RSD)<1.25 表明了传感器的精度,因此基于表面等离子体共振的生物仿生双酚 A 传感器操作简单,是一种具有成本效益的选择。
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引用次数: 0
Post-burn and post-blast rapid detection of trace and bulk energetics by 3D-printed cone spray ionization mass spectrometry 利用 3D 打印锥喷电离质谱仪快速检测焚烧后和爆炸后的痕量和大体积能量物质
IF 4.1 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-11-08 DOI: 10.1016/j.talo.2024.100377
Ryan M. Bain , TJ Pinedo , Doug J. Klapec , Christopher C. Mulligan , Patrick W. Fedick
Forensic analysis of post-blast and post-burn materials can be critical to a law enforcement or military investigation. 3D-printed cone spray ionization (3D-PCSI) coupled to a field portable mass spectrometer (MS) has been demonstrated as a rapid and low-cost alternative to traditional laboratory-based techniques (high resolution liquid or gas chromatography mass spectrometry) for the detection and analysis of energetic materials. 3D-PCSI-MS can sample trace or bulk energetics within or upon solid matrices with no sample preparation. Solid samples, in this case post-blast or post-burn energetics, are placed within the hollow cavity of the cone that has an approximately 100 µm spray-based emitter at the apex. An extraction/spray solvent is added, and a high voltage is subsequently applied. When coupled to a field portable MS, post-burn and post-blast analyses can be performed in the field. Double base propellant was burned on a variety of substrates and examined via 3D-PCSI-MS. An energetic material and stabilizers used in propellants were detected from the post-burn samples with no sample preparation. Trinitrotoluene (TNT, used in military and commercial explosives) and triacetone triperoxide (TATP, a homemade explosive) were examined post-blast on the US ton scale and the gram scale, respectively.
爆炸后和焚烧后材料的法医分析对于执法或军事调查至关重要。三维打印锥形喷雾离子化(3D-PCSI)与现场便携式质谱仪(MS)相结合,已被证明可快速、低成本地替代传统的实验室技术(高分辨率液相或气相色谱质谱法),用于检测和分析高能材料。3D-PCSI-MS 可对固体基质内或固体基质上的痕量或大量高能物质进行采样,无需进行样品制备。固体样品(在本例中为爆炸后或燃烧后的高能物质)被放置在锥体的空腔中,锥体顶端有一个约 100 微米的喷雾发射器。加入萃取/喷雾溶剂,然后施加高压。与现场便携式质谱仪连接后,可在现场进行燃烧后和爆炸后分析。双基推进剂在各种基质上燃烧,并通过 3D-PCSI-MS 进行检测。从焚烧后的样品中检测到了推进剂中使用的一种高能材料和稳定剂,无需进行样品制备。三硝基甲苯(TNT,用于军用和商用炸药)和三丙酮三过氧化物(TATP,一种自制炸药)在爆炸后分别按美国吨级和克级进行了检测。
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引用次数: 0
Development of engineered Zn-MOF/g-C3N4 based photoelectrochemical system for real-time sensors and removal of naproxen in wastewater 开发基于 Zn-MOF/g-C3N4 的工程光电化学系统,用于实时传感器和去除废水中的萘普生
IF 4.1 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-11-07 DOI: 10.1016/j.talo.2024.100371
Abera D. Ambaye , Sithembela A. Zikalala , Karabo C. Mashiloane , Jemal F. Nure , Mesfin A. Kebede , Touhami Mokrani , Edward N. Nxumalo
Naproxen-contaminated water may lead to the accumulation of the drug in aquatic organisms and can pose high risks to an aquatic environment and human beings. Therefore, this work aimed to develop photoelectrochemical sensing and degradation of naproxen (NPX) using zinc-metal organic framework /graphitic carbon nitride thin film-based fluorine-doped tin oxide (Zn-MOF/g-C3N4/FTO) as anode material for the sensing and degradation of naproxen (NPX). The surface morphology, structure, surface property, surface area, optical property, photocurrent, and charge transfer kinetics abilities were studied using different techniques. The nanocomposites showed a superior photocurrent response (0.815 mA cm-2) compared to the original g-C3N4 (0.328 mA cm-2). The photo-anode made of Zn-MOF@g-C3N4/FTO displayed the highest photocurrent value, indicating that the alignment of the two semiconductor bands prevented the quick recombination of electron-hole pairs. Owing to these attractive features, the Zn-MOF/g-C3N4/FTO electrode was applied for photoelectrochemical detection of NPX using chronoamperometry. Interestingly, the nanocomposites-based FTO ascribed a lower detection limit (2.3 ng l-1) with a wide linear range concentration of NPX (0.5 to 200 µg l-1). Additionally, the analytical assessment of repeatability and reproducibility demonstrated robust performance, with commendable relative standard deviations (RSD%) of 2.54 % and 2.40 %, respectively. On the other hand, a remarkable degradation efficiency of 97.52 % was attained when employing a bias potential of 0.1 V during a 2 h photoelectrocatalytic oxidation of NPX. The degradation process was primarily driven by the active participation of holes and hydroxyl radicals in ring opening and subsequent cleavage of by-products. The notable effectiveness of this degradation can be attributed to the combined and synergistic effects of both electrochemical and photocatalytic degradation techniques. The current state demonstrates its effectiveness in the photoelectrochemical sensing and removal of NPX using MOF/g-C3N4 nanocomposites-based electrode materials in wastewater.
萘普生污染的水可能会导致该药物在水生生物体内蓄积,并对水生环境和人类构成高风险。因此,本研究旨在利用锌-金属有机框架/石墨化氮化碳薄膜基掺氟氧化锡(Zn-MOF/g-C3N4/FTO)作为阳极材料,开发萘普生(NPX)的光电化学传感和降解技术。采用不同的技术对纳米复合材料的表面形貌、结构、表面性质、表面积、光学性质、光电流和电荷转移动力学能力进行了研究。纳米复合材料的光电流响应(0.815 mA cm-2)优于原始 g-C3N4(0.328 mA cm-2)。由 Zn-MOF@g-C3N4/FTO 制成的光阳极显示出最高的光电流值,这表明两个半导体带的排列防止了电子-空穴对的快速重组。由于这些诱人的特性,Zn-MOF/g-C3N4/FTO 电极被应用于使用时标法进行 NPX 的光电化学检测。有趣的是,基于纳米复合材料的 FTO 具有较低的检测限(2.3 纳克/升),NPX 的线性范围较宽(0.5 至 200 微克/升)。此外,对可重复性和再现性的分析评估也显示出了良好的性能,相对标准偏差(RSD%)分别为 2.54 % 和 2.40 %,值得称赞。另一方面,在对 NPX 进行 2 小时的光电催化氧化过程中,当采用 0.1 V 的偏置电位时,降解效率高达 97.52%。降解过程主要由空穴和羟基自由基积极参与开环和随后的副产物裂解所驱动。这种降解的显著效果可归因于电化学和光催化降解技术的综合协同效应。目前的研究表明,使用基于 MOF/g-C3N4 纳米复合材料的电极材料在废水中进行光电化学传感和去除 NPX 是有效的。
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引用次数: 0
Continuous-flow analysis of nitrogen compounds in environmental water using a copper–zinc reduction coil 利用铜锌还原线圈对环境水中的氮化合物进行连续流分析
IF 4.1 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-11-07 DOI: 10.1016/j.talo.2024.100378
Satoshi Morikubo , Nodoka Takahashi , Yorihiro Kumazawa , Yasuhiko Takuma , Daisuke Enomoto , Takashi Nishimura , Ryosei Kanno , Suguru Okunishi , Hiroto Maeda
The copper–cadmium reduction method has been applied to determine nitrogen compounds in heavily contaminated environmental water. However, there is an international demand to reduce the use of cadmium because it is harmful to humans and environment. Hence, a copper–zinc reduction continuous flow analysis system without using cadmium was developed for nitrogen-compound determination. However, the effects of seawater contaminants on this analytical method remains unknown. Therefore, in this study, the effects of contaminants on the developed method are investigated, and the applicability of the method to environmental water analysis is examined. Resultantly, interference due to magnesium precipitation is confirmed; however, this could be prevented by adjusting the concentration of the analytical reagent, i.e.,. ethylenediaminetetraacetic acid disodium. The measurement of certified reference materials under the new conditions, with precipitation countermeasures, show good results, with an accuracy of over 96 %. Additionally, a recovery study using actual environmental water afforded good results, with recovery of >95 % for all samples. These results indicate that the proposed method is an excellent, cadmium-free analytical method capable of analyzing environmental water as effectively as conventional methods.
铜镉还原法已被用于测定严重污染环境水体中的氮化合物。然而,由于镉对人体和环境有害,国际上要求减少镉的使用。因此,我们开发了一种不使用镉的铜锌还原连续流动分析系统,用于测定氮化合物。然而,海水污染物对这种分析方法的影响仍然未知。因此,本研究调查了污染物对所开发方法的影响,并考察了该方法在环境水分析中的适用性。结果证实,镁沉淀造成了干扰;不过,可以通过调整分析试剂(即乙二胺四乙酸二钠)的浓度来防止这种干扰。在采取沉淀对策的新条件下,对经认证的标准物质进行的测量结果显示效果良好,准确度超过 96%。此外,使用实际环境水进行的回收研究也取得了良好的结果,所有样品的回收率均达到 95%。这些结果表明,所提出的方法是一种出色的无镉分析方法,能够与传统方法一样有效地分析环境水。
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引用次数: 0
Enhancing isomer specificity in mass spectrometry by combining silver ion adduction and ion mobility 结合银离子吸附和离子迁移率提高质谱分析中异构体的特异性
IF 4.1 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-11-03 DOI: 10.1016/j.talo.2024.100373
Varun V. Sharma , Danjo De Chavez , Susan E. Slade , Ingela Lanekoff

Background

Identification and characterization of steroids from complex mixtures with isomeric precision is key to studying endocrine-related metabolism and disorders. Whereas the golden standard chromatography, including liquid chromatography and gas chromatography, can be coupled with mass spectrometry to separate steroids prior to ionization, this separation is time-consuming. Contrarily, direct infusion techniques can offer increased throughput; however, these are often hampered by limited structural specificity. Thus, it is important to develop new analytical tools for direct infusion mass spectrometry that will provide isomeric specificity.

Results

Herein, we show that direct infusion with electrospray ionization in combination with silver adduction and cyclic ion mobility mass spectrometry (cIMS) enables mobility separation and improves the detectability of steroid isomers. Specifically, silver ion adduction of steroids increases instrumental response up to 14 times and enables almost baseline mobility separation of closely related structural steroid isomers even at low cIMS resolution. By combining experimental and theoretical data, we show that the silver interacts with the steroid isomer at single or multiple sites, which introduces conformational changes that enable mobility separation. Moreover, we show that the combination of cIMS and silver adduct fragmentation in tandem mass spectrometry provides an additional dimension for annotation of steroid isomers. Thus, the simple introduction of silver ions into the electrospray solvent provides a great gain in the analytical discernment of steroid isomers.

Significance

For the first time, we show that the use of silver adduction introduces a conformational change in steroids that allows for them to be separated with low-resolution ion mobility spectrometry without any prior derivatization, chromatographic separation, or instrumental modification. This is a new and important tool for analyzing steroid isomers that can unravel their importance in biological systems.
背景以同分异构体的精度从复杂混合物中鉴定和表征类固醇是研究内分泌相关代谢和疾病的关键。虽然黄金标准色谱法(包括液相色谱法和气相色谱法)可与质谱联用,在离子化之前分离类固醇,但这种分离耗时较长。与此相反,直接输注技术可以提高处理量,但其结构特异性往往有限。因此,为直接注入质谱法开发新的分析工具以提供同分异构体的特异性是非常重要的。结果在本文中,我们展示了直接注入与电喷雾离子化、银离子加成和循环离子淌度质谱法(cIMS)相结合,可实现淌度分离并提高类固醇同分异构体的可检测性。具体来说,类固醇的银离子加成可将仪器响应提高 14 倍,即使在 cIMS 分辨率较低的情况下,也能对结构密切相关的类固醇异构体进行几乎基线的迁移率分离。通过结合实验和理论数据,我们发现银在单个或多个位点与类固醇异构体相互作用,从而引入构象变化,实现迁移率分离。此外,我们还证明了串联质谱中 cIMS 与银加成碎片的结合为类固醇异构体的注释提供了一个额外的维度。意义我们首次展示了银加成在类固醇中的构象变化,这种变化使类固醇可以在不进行任何衍生、色谱分离或仪器改装的情况下通过低分辨率离子迁移谱进行分离。这是分析类固醇异构体的一种新的重要工具,可以揭示它们在生物系统中的重要性。
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Talanta Open
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