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A novel Six Sigma approach and eco-friendly RP-HPLC technique for determination of pimavanserin and its degraded products: Application of Box–Behnken design 一种新颖的六西格玛方法和环保型 RP-HPLC 技术用于测定匹马色林及其降解产物:方框-贝肯设计的应用
IF 4.3 3区 化学 Q2 Chemistry Pub Date : 2024-01-01 DOI: 10.1515/revac-2023-0073
Hossam M. Nassef, Hoda A. Ahmed, A. Bashal, Mohamed A. El-Atawy, Tahani Y. A. Alanazi, Samar M. Mahgoub, Mahmoud A. Mohamed
A green analytical chemistry study attempts to generate environmentally friendly alternatives to dangerous compounds while reducing waste output. The study thoroughly analyzed eight green tools to determine their greenness. Given its importance in treating hallucinations and delusions produced by Parkinson’s disease psychosis, it is critical to have a reliable and precise method for identifying pimavanserin (PVS) in both pure form and pharmaceutical formulations. The current study used a straightforward approach to forced degradation experiments to establish a novel reversed-phase high-performance liquid chromatography method for evaluating stability. The method was executed on the Agilent Zorbax Eclipse Plus C18 column (100 × 4.6 mm, 3.5 μm particle size) with ultraviolet detection at 226 nm. The Box–Behnken design is the ultimate solution for identifying optimal chromatographic conditions in a timely and efficient manner, with minimal trials required. The study investigated the impact of three factors: acetonitrile ratio, column oven temperature, and flow rate on various responses, namely, retention time, tailing factor, and theoretical plates. Desirability and overlay plots were utilized to forecast the best mobile phase containing a buffer solution: acetonitrile: tetrahydrofuran in a ratio of (65: 20: 15, v/v/v), which proved highly effective in the experiments. Linearity was conducted for PVS in the 3–50 µg·mL−1 range with an R 2 coefficient of determination of 0.9997. PVS had detection and quantification limits of 1.1 and 3.5 µg·mL−1, respectively, indicating a highly significant correlation between the variables studied. PVS’s recovery percentage was determined to be 101.30%. We also used the Six Sigma lean technique to ensure precision and productivity. PVS was tested for acid, base, oxidative hydrolysis, photodegradation, and heat, as per International Council for Harmonisation guidelines. The highest degradation was obtained from oxidative hydrolysis and thermal degradation.
一项绿色分析化学研究试图生产危险化合物的环保型替代品,同时减少废物产出。这项研究全面分析了八种绿色工具,以确定其绿色程度。鉴于其在治疗帕金森氏病精神错乱所产生的幻觉和妄想方面的重要性,拥有一种可靠而精确的方法来鉴定纯品和药物制剂中的匹马伐林(PVS)至关重要。本研究采用直接的强制降解实验方法,建立了一种新型反相高效液相色谱法,用于评估稳定性。该方法采用 Agilent Zorbax Eclipse Plus C18 色谱柱(100 × 4.6 mm,3.5 μm 粒径),紫外检测波长为 226 nm。方框-贝肯设计是及时有效地确定最佳色谱条件的最终解决方案,只需进行最少的试验。该研究调查了乙腈比例、色谱柱烘箱温度和流速这三个因素对保留时间、拖尾因子和理论平板等各种反应的影响。利用可取性图和叠加图预测了最佳流动相,流动相含有缓冲溶液:乙腈:四氢呋喃,比例为(65:20:15,v/v/v),实验证明该流动相非常有效。PVS 在 3-50 µg-mL-1 范围内呈线性关系,R 2 测定系数为 0.9997。PVS 的检测限和定量限分别为 1.1 微克-毫升-1 和 3.5 微克-毫升-1,这表明所研究的变量之间存在高度显著的相关性。经测定,PVS 的回收率为 101.30%。我们还采用了六西格玛精益技术,以确保精度和生产率。根据国际协调理事会的指导方针,对 PVS 进行了酸、碱、氧化水解、光降解和热测试。氧化水解和热降解的降解率最高。
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引用次数: 0
Recent advance in electrochemical immunosensors for lung cancer biomarkers sensing 用于肺癌生物标记物检测的电化学免疫传感器的最新进展
IF 4.3 3区 化学 Q2 Chemistry Pub Date : 2024-01-01 DOI: 10.1515/revac-2023-0068
Li Fu, Xiaozhu Liu, Junyi Cao, Huan Li, Anyou Xie, Yue Liu
Lung cancer has a high mortality rate largely due to late-stage diagnosis. Detecting protein and genetic biomarkers through electrochemical immunosensors enables non-invasive early diagnosis. This review discusses recent advances in electrochemical immunosensors for detecting clinically relevant lung cancer biomarkers. The use of nanomaterials like graphene, carbon nanotubes, metal nanoparticles, and conducting polymers in sensor fabrication improves electron transfer kinetics, enhances signal transduction, and allows higher antibody loading. Smart surface immobilization strategies optimize antibody orientation and binding capacity. Amplification approaches utilizing nanomaterials, enzymes, polymers, dendrimers, and DNA nanostructures are applied to enhance output signal per binding event. Various electroanalytical techniques including amperometry, potentiometry, impedance spectroscopy, and voltammetry are employed for quantitative monitoring. Recent immunosensors showcase low detection limits and wide linear ranges for measurement of major biomarkers like carcinoembryonic antigen, neuron specific enolase, and cytokeratin fragment 21-1. Emerging biomarkers such as microRNAs and circulating tumor cells have also been targeted. However, reproducibility, selectivity, multiplexing, and integration with point-of-care platforms need improvement for widespread clinical translation. Overall, electrochemical immunosensors hold immense potential for sensitive, affordable lung cancer diagnosis if ongoing efforts can address current limitations.
肺癌的死亡率很高,主要是因为诊断较晚。通过电化学免疫传感器检测蛋白质和基因生物标志物可实现无创早期诊断。本综述讨论了用于检测临床相关肺癌生物标志物的电化学免疫传感器的最新进展。在传感器制造过程中使用石墨烯、碳纳米管、金属纳米颗粒和导电聚合物等纳米材料可改善电子转移动力学、增强信号传导并提高抗体负载量。智能表面固定策略可优化抗体定向和结合能力。利用纳米材料、酶、聚合物、树枝状聚合物和 DNA 纳米结构的放大方法可提高每次结合事件的输出信号。定量监测采用了各种电分析技术,包括安培计、电位计、阻抗光谱法和伏安法。最近推出的免疫传感器在测量癌胚抗原、神经元特异性烯醇化酶和细胞角蛋白片段 21-1 等主要生物标记物时,检测限低、线性范围宽。微 RNA 和循环肿瘤细胞等新出现的生物标记物也已成为目标。不过,要广泛应用于临床,还需要改进可重复性、选择性、多重性以及与护理点平台的整合。总之,如果目前的努力能解决目前的局限性,电化学免疫传感器在灵敏、经济的肺癌诊断方面具有巨大的潜力。
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引用次数: 0
Quantitative methods in the analysis of clozapine in human matrices – A scoping review 人体基质中氯氮平的定量分析方法--范围综述
IF 4.3 3区 化学 Q2 Chemistry Pub Date : 2024-01-01 DOI: 10.1515/revac-2023-0066
Jia Le Lim, M. Rajagopal, G. Akowuah, F. Keshavarzi, Khaled Mohammed Ahmed Alakhali
Clozapine (CLZ) has retained its clinical utility in the management of schizophrenia despite the discovery of novel antipsychotics, as it possesses unique efficacy in the setting of treatment resistant schizophrenia while causing minimal extrapyramidal symptoms. However, these benefits are offset by the risk of agranulocytosis and other side effects, and therapeutic drug monitoring (TDM) is routinely recommended for patients undergoing treatment with CLZ. A multitude of approaches for the quantification of CLZ have been developed for different settings such as TDM, quality control of pharmaceutical dosage forms, and toxicology studies. Primarily, these approaches fall under one of three branches of analysis, namely, chromatography, electrochemical analysis, and spectrophotometry. This study provides a scoping review of the recent advances in the methods of quantification for CLZ and highlights the potential utility of novel methods in the field of drug quantification.
尽管新型抗精神病药物不断问世,但氯氮平(CLZ)在治疗精神分裂症方面仍有其临床用途,因为它在治疗耐药精神分裂症方面具有独特疗效,同时导致的锥体外系症状极少。然而,粒细胞减少和其他副作用的风险抵消了这些优点,因此建议对接受 CLZ 治疗的患者进行治疗药物监测 (TDM)。针对不同的情况,如 TDM、药物剂型的质量控制和毒理学研究,已开发出多种用于定量 CLZ 的方法。这些方法主要分为三个分析分支,即色谱法、电化学分析法和分光光度法。本研究概述了 CLZ 定量方法的最新进展,并强调了新型方法在药物定量领域的潜在用途。
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引用次数: 0
Microfabricated potentiometric sensor based on a carbon nanotube transducer layer for selective Bosentan determination 基于碳纳米管传感器层的微加工电位传感器,用于选择性测定波生坦
IF 4.3 3区 化学 Q2 Chemistry Pub Date : 2024-01-01 DOI: 10.1515/revac-2023-0071
Y. A. Trabik, Reham Abd El-Aziz Ismail, M. Ayad, L. Hussein, A. M. Mahmoud
In this work, a solid-state electrochemical sensor relying on potentiometric transduction was constructed and optimized to detect Bosentan (BOS) in its pharmaceutical dosage form and human plasma. BOS is useful in pulmonary hypertension management as a nonselective endothelin receptor antagonist. A printed circuit board has been constructed and used as a substrate for microfabricated Cu electrodes. In comparison to a microfabricated control (Cu/ISM) electrode, the sensor potential signal drift was enhanced, and the response time was reduced by using multi-walled carbon nanotubes (MWCNTs) as an ion-to-electron transducer layer. According to IUPAC requirements, the suggested BOS sensors have been electrochemically characterized, and the linear dynamic range is (1.0 × 10−8 to 1.0 × 10−5) M with a limit of detection of 6.28 × 10−9 M and 6.12 × 10−9 M for MWCNT-based sensor (Cu/CNT-NC/ISM) and control sensor (Cu/ISM), respectively. The described sensors have been used successfully to selectively determine BOS in dosage form and human plasma without any pre-treatment steps.
这项研究构建并优化了一种依赖于电位转换的固态电化学传感器,用于检测药物剂型和人体血浆中的波生坦(BOS)。BOS 是一种非选择性内皮素受体拮抗剂,可用于治疗肺动脉高压。我们制作了一块印刷电路板,并将其用作微加工铜电极的基底。与微加工对照(Cu/ISM)电极相比,使用多壁碳纳米管(MWCNTs)作为离子-电子转换层,传感器电位信号漂移增强,响应时间缩短。根据 IUPAC 的要求,对所建议的 BOS 传感器进行了电化学表征,基于 MWCNT 的传感器(Cu/CNT-NC/ISM)和控制传感器(Cu/ISM)的线性动态范围为(1.0 × 10-8 至 1.0 × 10-5)M,检测限分别为 6.28 × 10-9 M 和 6.12 × 10-9 M。所述传感器已成功用于选择性检测剂型和人体血浆中的 BOS,无需任何预处理步骤。
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引用次数: 0
Latest trends in honey contaminant analysis, challenges, and opportunities for green chemistry development 蜂蜜污染物分析的最新趋势、挑战和绿色化学发展的机遇
IF 4.3 3区 化学 Q2 Chemistry Pub Date : 2024-01-01 DOI: 10.1515/revac-2023-0072
A. Sixto, S. Niell, M. Cesio, Horacio Heinzen
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引用次数: 0
Greenness of dispersive microextraction using molecularly imprinted polymers 使用分子印迹聚合物进行分散微萃取的绿色环保性
IF 4.3 3区 化学 Q2 Chemistry Pub Date : 2024-01-01 DOI: 10.1515/revac-2023-0070
Tamara Tadić, Bojana Markovic, Sandra Bulatović, Jelena Lukić, Jelena Radulović, A. Nastasović, A. Onjia
Molecularly imprinted polymers (MIPs) as materials with determined levels of selectivity and specificity for designated analytes have recently gained much attention in various application fields. However, with the growing adoption of green analytical chemistry (GAC) principles, it is essential to investigate the greenness of MIP synthesis and its subsequent application in sample preparation, as well as to evaluate the “green” nature of the developed analytical methodologies, such as dispersive solid-phase microextraction (DSPME). Accordingly, the main objective of this research was to evaluate the greenness of MIP-based glycidyl methacrylate synthesis and MIP use as a DSPME sorbent prior to high-performance liquid chromatography with mass spectrometry (HPLC-MS). The green perspective of MIP-DSPME prior to HPLC-MS was investigated using various analytical metric tools such as the Analytical Eco-Scale, the Green Analytical Procedure Index, and Analytical GREEnness (AGREE). Since these analytical tools are not fully implementable for the assessment of the greenness of the MIP synthesis, some alternative approaches were used to optimize the synthesis parameters to make the MIP DSPME sorbent as close as possible to the GAC principles. The calculated AGREE score (0.62) and 91 points in the Analytical Eco-Scale for the proposed DSPME technique using MIP indicated a high level of greenness.
分子印迹聚合物(MIPs)作为一种对指定分析物具有确定选择性和特异性的材料,近年来在各个应用领域受到广泛关注。然而,随着绿色分析化学(GAC)原则的日益广泛采用,研究 MIP 合成及其在样品制备中的后续应用的绿色性,以及评估已开发的分析方法(如分散固相微萃取(DSPME))的 "绿色 "性就显得尤为重要。因此,本研究的主要目的是评估基于 MIP 的甲基丙烯酸缩水甘油酯合成以及 MIP 用作高效液相色谱-质谱法(HPLC-MS)前的 DSPME 吸附剂的绿色环保性。使用各种分析度量工具(如分析生态尺度、绿色分析程序指数和分析 GREEnness (AGREE))对 HPLC-MS 前 MIP-DSPME 的绿色前景进行了研究。由于这些分析工具无法完全用于评估 MIP 合成的绿色程度,因此采用了一些替代方法来优化合成参数,以使 MIP DSPME 吸附剂尽可能接近 GAC 原理。计算得出的 AGREE 分数(0.62)和分析生态尺度中的 91 分表明,使用 MIP 的 DSPME 技术具有很高的绿色水平。
{"title":"Greenness of dispersive microextraction using molecularly imprinted polymers","authors":"Tamara Tadić, Bojana Markovic, Sandra Bulatović, Jelena Lukić, Jelena Radulović, A. Nastasović, A. Onjia","doi":"10.1515/revac-2023-0070","DOIUrl":"https://doi.org/10.1515/revac-2023-0070","url":null,"abstract":"\u0000 Molecularly imprinted polymers (MIPs) as materials with determined levels of selectivity and specificity for designated analytes have recently gained much attention in various application fields. However, with the growing adoption of green analytical chemistry (GAC) principles, it is essential to investigate the greenness of MIP synthesis and its subsequent application in sample preparation, as well as to evaluate the “green” nature of the developed analytical methodologies, such as dispersive solid-phase microextraction (DSPME). Accordingly, the main objective of this research was to evaluate the greenness of MIP-based glycidyl methacrylate synthesis and MIP use as a DSPME sorbent prior to high-performance liquid chromatography with mass spectrometry (HPLC-MS). The green perspective of MIP-DSPME prior to HPLC-MS was investigated using various analytical metric tools such as the Analytical Eco-Scale, the Green Analytical Procedure Index, and Analytical GREEnness (AGREE). Since these analytical tools are not fully implementable for the assessment of the greenness of the MIP synthesis, some alternative approaches were used to optimize the synthesis parameters to make the MIP DSPME sorbent as close as possible to the GAC principles. The calculated AGREE score (0.62) and 91 points in the Analytical Eco-Scale for the proposed DSPME technique using MIP indicated a high level of greenness.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":4.3,"publicationDate":"2024-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140525438","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Enantiomeric separation of four pairs of alkaloids by using a C18 column tandem polysaccharide-based chiral column 使用 C18 柱串联多糖手性色谱柱分离四对生物碱对映体
IF 4.3 3区 化学 Q2 Chemistry Pub Date : 2024-01-01 DOI: 10.1515/revac-2023-0074
Xiaoxi Si, Yu Tian, Shu-Teng Xu, Chunbo Liu, Zhenjie Li, Ji Yang, Ying Guan, Yangzhou Xie, Xiaoqing Shi, Zhigang Xu, Zhihua Liu
Alkaloid enantiomers have different physiological and pharmacological effects, and different chiral compositions have a large impact on cigarette sensory and use safety. Studying the effects of different configurations of alkaloid enantiomers on cigarette sensory is important for the development of tobacco products, but the chiral separation of alkaloid enantiomers has become the core problem. Here, the application of a C18 column coupled with a polysaccharide-based chiral column to separate and detect four pairs of alkaloid enantiomers in tobacco and cigarette smoke of different brands was investigated. Results showed that the tandem technology of the two columns enabled the baseline separation of four pairs of alkaloid enantiomers. The resolution of enantiomers of alkaloids in different tobacco samples differed in content and ratio, showing different chiral distribution characteristics. According to the different distribution characteristics of alkaloid enantiomers, tobacco samples of different brands can be distinguished and real cigarettes can be identified.
生物碱对映体具有不同的生理和药理作用,不同的手性组成对卷烟的感官和使用安全性有很大影响。研究不同构型的生物碱对映体对卷烟感官的影响对烟草产品的开发具有重要意义,但生物碱对映体的手性分离成为核心问题。本文研究了如何应用 C18 色谱柱和多糖手性色谱柱分离检测不同品牌烟草和卷烟中的四对生物碱对映体。结果表明,这两种色谱柱的串联技术实现了四对生物碱对映体的基线分离。不同烟草样品中生物碱对映体的解析含量和比例不同,表现出不同的手性分布特征。根据生物碱对映体的不同分布特征,可以区分不同品牌的烟草样品,鉴别真假卷烟。
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引用次数: 0
Major biochemical constituents of Withania somnifera (ashwagandha) extract: A review of chemical analysis Withania somnifera (ashwagandha)提取物主要生化成分的化学分析综述
IF 4.3 3区 化学 Q2 Chemistry Pub Date : 2023-01-01 DOI: 10.1515/revac-2022-0055
Mahmoud Tareq Abdelwahed, Maha A. Hegazy, Ekram H Mohamed
Abstract Ashwagandha (Withania somnifera) is a very popular medicinal herb originated mainly in India and found in the Middle East and parts of Africa. Ashwagandha has gained recognition as the most revered plant in Ayurvedic medicine. Studies indicated that it is used as anxiolytic, anti-inflammatory, antioxidant, adaptogen, memory enhancer, and possess an effect on neurodegenerative diseases. Additionally, it was revealed that the plant exerts antibacterial, antiviral, antitumor, aphrodisiac, and cardiovascular protection activities. Due to the biological and nutritional importance of nutraceuticals, particularly ashwagandha, and as part of the ongoing research of the natural products and its bioactive phytochemicals, this review aims to summarize the recent analytical techniques that have been reported for the determination of different chemical constituents of Withania somnifera quantitatively and qualitatively, and to highlight new challenges.
Ashwagandha (Withania somnifera)是一种非常流行的草药,主要起源于印度,在中东和非洲部分地区发现。阿什瓦甘达被认为是阿育吠陀医学中最受尊敬的植物。研究表明,它被用作抗焦虑、抗炎、抗氧化、适应原、记忆增强剂,并对神经退行性疾病有作用。此外,该植物还具有抗菌、抗病毒、抗肿瘤、壮阳和心血管保护活性。由于营养保健品,特别是印度烟的生物学和营养重要性,以及作为天然产物及其生物活性植物化学物质正在进行的研究的一部分,本文旨在总结近年来已报道的测定Withania somnifera不同化学成分的定量和定性分析技术,并指出新的挑战。
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引用次数: 3
A brief review of the application of microextraction by packed sorbent for antibiotics analysis from biological, food, and environmental samples 简要综述了包装吸附剂微萃取法在生物、食品和环境样品中抗生素分析中的应用
IF 4.3 3区 化学 Q2 Chemistry Pub Date : 2023-01-01 DOI: 10.1515/revac-2023-0057
G. Granados-Guzmán, Mónica Díaz-Hernández, R. Álvarez-Román, Norma Cavazos-Rocha, Omar J. Portillo-Castillo
Abstract Currently, sample preparation is the most laborious part of the analytical process, requiring the most time and being susceptible to the most errors. In this context, numerous investigations have focused on the miniaturization of these techniques to reduce work time, costs, and errors. In this regard, microextraction by packed sorbent (MEPS) is a simple, fast, and robust sample preparation technique suitable for easy automation in several analytical systems and is applied to a wide variety of samples. Antibiotics are among the most commonly used drugs; however, their extensive and inappropriate use has garnered significant attention in the environment, human health, and food safety. This brief review is intended to provide an overview of recently reported antibiotic extraction methods based on MEPS, with a special interest in those applied to the analysis of biological, environmental, and food samples. In addition, the sample pretreatment step before extraction by the MEPS device was highlighted, as was the description of the sample-related steps within the MEPS procedure, such as extraction, washing, and elution.
目前,样品制备是分析过程中最费力的部分,需要最多的时间,容易产生最多的错误。在这种情况下,许多调查都集中在这些技术的小型化上,以减少工作时间、成本和错误。在这方面,填充吸附剂微萃取(MEPS)是一种简单、快速、可靠的样品制备技术,适用于多种分析系统的自动化,适用于各种样品。抗生素是最常用的药物之一;然而,它们的广泛和不当使用引起了环境、人类健康和食品安全方面的重大关注。这篇简短的综述旨在提供最近报道的基于MEPS的抗生素提取方法的概述,特别关注那些应用于生物,环境和食品样品分析的方法。此外,强调了MEPS设备提取前的样品预处理步骤,以及MEPS过程中样品相关步骤的描述,如提取、洗涤和洗脱。
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引用次数: 0
Progress of sensitive materials in chemiresistive sensors for detecting chemical warfare agent simulants: A review 用于化学战剂模拟物探测的化学传感器敏感材料研究进展
IF 4.3 3区 化学 Q2 Chemistry Pub Date : 2023-01-01 DOI: 10.1515/revac-2022-0052
Liu Yang, Molin Qin, Genwei Zhang, Jie Yang, Junchao Yang, Jiang Zhao
Abstract Chemical warfare agents (CWAs) are chemical substances intended for use in military operations to kill, injure, or incapacitate an enemy. It is very important to detect toxic CWAs at trace levels on site. Compared with traditional CWA analysis instrument methods, chemiresistive gas sensors present advantages of being small, fast, and inexpensive. Chemiresistive gas sensors are still an important research topic with the development of nanofabrication technology and new kinds of sensing materials, including carbon nanotubes, graphene, and black phosphorus (BP). Chemiresistive gas sensors are divided into three categories according to the type of sensitive materials: carbon- and BP-based materials, conductive polymers, and metal oxide semiconductors. A brief analysis was carried out on fabrication strategies using sensitive materials, including hydrogen bonding strategies, nanostructures, morphology, doping effects, composite materials, and other material application methods, and the sensitive materials and detection effects are summarized in this study. This review aims to provide guidance in the development of chemiresistive sensors for the detection of CWAs. Graphical abstract
化学战剂(CWAs)是在军事行动中用于杀死、伤害或使敌人丧失行动能力的化学物质。在现场检测痕量的有毒CWAs是非常重要的。与传统的CWA分析仪器方法相比,化学电阻式气体传感器具有体积小、速度快、价格便宜等优点。随着纳米制造技术和新型传感材料(如碳纳米管、石墨烯、黑磷等)的发展,化学电阻式气体传感器仍然是一个重要的研究课题。化学电阻式气体传感器根据敏感材料的类型分为三类:碳基和bp基材料、导电聚合物和金属氧化物半导体。简要分析了敏感材料的制备策略,包括氢键策略、纳米结构、形貌、掺杂效应、复合材料以及其他材料的应用方法,并对敏感材料和检测效果进行了总结。本文综述旨在为CWAs检测的化学电阻传感器的发展提供指导。图形抽象
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引用次数: 2
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Reviews in Analytical Chemistry
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