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Nanogram-level green spectrofluorimetric method for simultaneous quantification of tadalafil and silodosin in pharmaceuticals, environmental matrices and content uniformity testing 纳克级绿色荧光光谱法同时定量药品、环境基质中他达拉非和西洛多辛含量均匀性试验
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-27 DOI: 10.1016/j.talo.2025.100534
Aya Saad Radwan , Mohamed Hefnawy , Talha Bin Emran , Mohamed M. Salim
A novel, eco-friendly spectrofluorimetric method has been developed and validated for the first time for simultaneous determination of tadalafil (TDF) and silodosin (SLD) in pharmaceutical dosage forms and environmental water samples without the need for prior separation. This innovative approach exploits the emission fluorescence of both drugs, employing excitation at 270 nm and emission detection at 328 nm for TDF and 454 nm for SLD. The method demonstrated excellent linearity across the concentration ranges of 50.0–1200.0 ng mL-1 for TDF and 1.0–300.0 ng mL-1 for SLD (r > 0.9999), with remarkable limits of detection of 10.94 ng mL-1 and 0.28 ng mL-1, respectively. The high sensitivity and precision (RSD < 0.70 %), with recovery rates ranging from 99.50 % to 101.00 % in pharmaceuticals and 97.31 % to 102.83 % in environmental water emphasize the method’s robustness and practical applicability for therapeutic drug monitoring and environmental surveillance. Application to content uniformity testing of tablet formulations, in accordance with British Pharmacopoeia guidelines, further demonstrates the method’s versatility. Greenness assessments using the AGREE and complex moGAPI metrics, alongside operational efficiency evaluation through the Click Analytical Chemistry Index (CACI), confirm the method’s sustainability and minimal environmental impact. Fully compliant with ICH Q2(R1) guidelines, this validated protocol offers a pioneering, rapid, and sustainable alternative for routine quality control and environmental monitoring.
本文首次建立了一种新型、环保的荧光光谱法,可同时测定药物剂型和环境水样中的他达拉非(TDF)和西洛多辛(SLD),而无需事先分离。这种创新的方法利用了两种药物的发射荧光,采用270 nm的激发和328 nm的发射检测,TDF和454 nm的SLD。该方法在TDF浓度范围为50.0 ~ 1200.0 ng mL-1和SLD浓度范围为1.0 ~ 300.0 ng mL-1 (r > 0.9999)具有良好的线性关系,检测限分别为10.94 ng mL-1和0.28 ng mL-1。该方法具有较高的灵敏度和精密度(RSD < 0.70%),在药品和环境水中的回收率分别为99.50% ~ 101.00%和97.31% ~ 102.83%,具有较好的鲁棒性和实用性。应用于片剂配方的含量均匀性测试,根据英国药典指南,进一步证明了该方法的通用性。使用AGREE和复杂的moGAPI指标进行的绿色评估,以及通过点击分析化学指数(CACI)进行的操作效率评估,证实了该方法的可持续性和最小的环境影响。该方案完全符合ICH Q2(R1)指南,为常规质量控制和环境监测提供了一种开创性、快速和可持续的替代方案。
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引用次数: 0
Material matters: evaluating polymer 96-well plates to reduce DAMGO loss in LC-MS/MS-based in vitro μ-opioid structure affinity assay 材料问题:评价聚合物96孔板在LC-MS/MS-based体外μ-阿片结构亲和测定中减少DAMGO损失
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-26 DOI: 10.1016/j.talo.2025.100543
Gaia Alluisetti , Emma Van Impe , Wolfgang Weinmann , Katharina Elisabeth Grafinger
The peptide DAMGO has been used for decades to determine binding affinity at the μ-opioid receptor in numerous types of receptor binding assays utilizing radiolabeled DAMGO, and more recently, liquid chromatography tandem mass spectrometry (LC-MS/MS)-based procedures with unlabeled DAMGO. While previously there have been numerous reports of non-specific adsorption (NSA) at plastic surfaces of various peptides, this study reports for the first time the NSA of DAMGO at polymer 96-well plates used in receptor binding affinity assays. In the present study, seven different types of polypropylene and one modified polystyrene 96-well plates were assessed for DAMGO NSA. The number of solution transfers, two different incubation temperatures and times were evaluated. NSA and DAMGO signal loss were observed for six out of eight tested plates. Best results were obtained with Thermo Scientific (Cat. No 60180-P133) 96-well deep-well plates, for which no significant signal deviation could be observed compared to the blanks even after six sequential transfers. Coated microtiter plates from Greiner Bio-One (Cat. No 655901) showed significant signal enhancement compared to the blanks, which may also cause issues when performing quantitative analysis of results. This study highlights the necessity of testing laboratory equipment for NSA during assay development, since peptide or analyte adsorption may not be immediately apparent, leading to the issue going unnoticed.
几十年来,在利用放射性标记DAMGO的多种受体结合试验中,肽DAMGO已被用于确定μ-阿片受体的结合亲和力,最近,基于液相色谱-串联质谱(LC-MS/MS)的方法使用未标记的DAMGO。虽然之前有许多关于各种多肽在塑料表面非特异性吸附(NSA)的报道,但本研究首次报道了DAMGO在聚合物96孔板上的非特异性吸附(NSA)用于受体结合亲和力测定。在本研究中,对七种不同类型的聚丙烯和一种改性聚苯乙烯96孔板进行了DAMGO NSA的评估。评估了溶液转移次数、两种不同的孵育温度和孵育时间。在8个测试板中有6个观察到NSA和DAMGO信号丢失。使用Thermo Scientific (Cat。没有60180-P133) 96孔深井板,即使经过六次连续转移,也没有观察到与空白相比的显著信号偏差。包被微量滴度板来自Greiner Bio-One (Cat)。No 655901)与空白相比显示出显著的信号增强,这也可能在进行定量分析结果时引起问题。本研究强调了在分析开发过程中测试NSA实验室设备的必要性,因为肽或分析物吸附可能不会立即显现,导致问题被忽视。
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引用次数: 0
Recent advances in photoelectrochemical sensing of tetracyclines 四环素类化合物光电传感研究进展
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-26 DOI: 10.1016/j.talo.2025.100542
Yali Cui , Yanyuan Zhang , Lin Wang , Yuanqiang Hao
Tetracyclines (TCs) are widely used antibiotics whose residues pose environmental and health risks, necessitating sensitive and selective detection. Photoelectrochemical (PEC) sensors have emerged as promising analytical tools due to their high sensitivity, low background noise, and cost-effective instrumentation. This review systematically summarizes recent advances in PEC sensing of TCs. We begin by categorizing the photoactive materials employed in PEC sensing and examining their structural design strategies, heterojunction engineering, and photoelectric properties. Subsequently, we elaborate on the fundamental signal transduction mechanisms, including the intrinsic redox activity of TCs, steric hindrance-induced current suppression, and coordination-mediated modulation of interfacial charge transfer. Furthermore, we highlight representative PEC sensing systems reported for TCs detection, classifying them based on recognition strategies such as aptamer binding, molecular imprinting, electrostatic adsorption, and site-specific coordination—each linked to distinct signal generation modes. Finally, current limitations and promising strategies for further performance enhancement of PEC sensors are discussed. This review provides a comprehensive perspective on PEC strategies for TCs detection and offers guidance for future innovations in environmental and food safety monitoring.
四环素类抗生素是一种广泛使用的抗生素,其残留具有环境和健康风险,需要进行灵敏和选择性的检测。光电化学(PEC)传感器因其高灵敏度、低背景噪声和低成本的仪器仪表而成为有前途的分析工具。本文系统地综述了近年来在tc的PEC传感方面的研究进展。我们首先对光电感应中使用的光活性材料进行分类,并研究它们的结构设计策略、异质结工程和光电性能。随后,我们详细阐述了基本的信号转导机制,包括TCs的内在氧化还原活性、位阻诱导的电流抑制和配位介导的界面电荷转移调制。此外,我们重点介绍了用于TCs检测的代表性PEC传感系统,并根据适配体结合、分子印迹、静电吸附和位点特异性协调等识别策略对它们进行了分类,每个策略都与不同的信号产生模式相关。最后,讨论了目前PEC传感器性能进一步提高的局限性和有前途的策略。本文综述了用于TCs检测的PEC策略的全面观点,并为未来环境和食品安全监测的创新提供了指导。
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引用次数: 0
Quality-by-design optimized HPLC approach for the therapeutic drug monitoring of isosorbide dinitrate and sildenafil in human plasma samples HPLC法监测人血浆样品中硝酸异山梨酯和西地那非的质量设计优化
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-23 DOI: 10.1016/j.talo.2025.100540
Mohamed A. Momtaz , Hanaa S. El-Desoky , Ahmed Rehab , Fathalla Belal
Isosorbide dinitrate (ISDN) and sildenafil citrate (SIL) are reported to have a potential drug-drug interaction when co-administered clinically. ISDN is indicated as first-line therapy for the long-term management of chronic stable angina. Sildenafil is the first oral treatment for erectile dysfunction. It is contra-indicated in patients who may require organic nitrates, such as ISDN, because this combination may cause a sudden drop in blood pressure by inhibiting the phosphodiesterase type 5 enzyme. Additionally, sildenafil is effective in treating cardiovascular disorders secondary to endothelial dysfunctions. Therefore, a sensitive, simple, and selective HPLC method is urgently needed for their simultaneous determination in plasma samples for monitoring their therapeutic blood concentration levels in emergency cases. The current study introduces the first HPLC approach for their simultaneous estimation in less than 10 minutes. The optimal separation was achieved using Nova-Pack® C18, 4 µm column at room temperature, with a mobile phase consisting of acetonitrile and acetate buffer (5 mM; pH 5, 39:61 % v/v), delivered at a flow rate of 1.1 mL/min. The injection volume was set at 50 µL, and detection was accomplished at 214 nm. The method demonstrated excellent linearity for ISDN(0.01–10.0µg/mL) and SIL (0.025–10.0µg/mL), with LOQ of 0.01 µg/mL and 0.020 µg/mL, respectively. The proposed method was successfully applied to analyze spiked human samples with recovery rates (104.9 and 105.55%) for ISDN and SIL respectively, confirming its suitability for bio-analytical use. Utilizing the quality-by- design (QbD) approach adopting the two-level full factorial design allowed the optimization of the experimental conditions of the proposed method. The method’s greenness was evaluated using Analytical Eco-Scale, Green Analytical Procedure Index (GAPI), and Analytical Greenness (AGREE). Validation of the proposed method was performed in accordance with ICH and US FDA guidelines.
据报道,硝酸异山梨酯(ISDN)和柠檬酸西地那非(SIL)在临床共给药时具有潜在的药物相互作用。ISDN是长期治疗慢性稳定型心绞痛的一线治疗方法。西地那非是治疗勃起功能障碍的第一种口服药物。对于可能需要有机硝酸盐(如ISDN)的患者禁用,因为这种组合可能通过抑制5型磷酸二酯酶导致血压突然下降。此外,西地那非对继发于内皮功能障碍的心血管疾病也有效。因此,迫切需要一种灵敏、简便、选择性强的高效液相色谱(HPLC)方法在血浆样品中同时测定它们,以监测急诊病例的治疗性血药浓度水平。目前的研究介绍了第一种HPLC方法,可以在不到10分钟的时间内进行同时估计。在室温下,采用Nova-Pack®C18, 4µm色谱柱,流动相为乙腈和醋酸缓冲液(5mm, pH 5,39:61 % v/v),流速为1.1 mL/min,达到最佳分离效果。进样量为50µL,检测波长为214 nm。该方法对ISDN(0.01 ~ 10.0µg/mL)和SIL(0.025 ~ 10.0µg/mL)具有良好的线性关系,LOQ分别为0.01µg/mL和0.020µg/mL。该方法成功地用于分析加标后的人类样品,ISDN和SIL的回收率分别为104.9和105.55%,证实了其生物分析应用的适用性。采用双水平全析因设计的质量设计方法,优化了该方法的实验条件。采用分析生态尺度、绿色分析程序指数(GAPI)和分析绿色度(AGREE)对该方法的绿色度进行评价。根据ICH和FDA指南对所建议的方法进行验证。
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引用次数: 0
A review on biosensor approaches for the detection of hazardous elements in water 生物传感器在水中有害元素检测中的研究进展
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-23 DOI: 10.1016/j.talo.2025.100536
Nidhi Chauhan , Nishtha Sah , Kirti Saxena , Utkarsh Jain
Water is the basis of life on Earth, but due to increased pollution and habitat degradation, water scarcity is increasing day by day. Therefore, it is necessary to detect water pollutants to save water and aquatic diversity. Monitoring of toxic elements present in wastewater effluents is an important factor for further treatment to make it pollutant-free. While various methods have been developed for monitoring these toxic elements, biosensors can overcome the limitations of traditional methods. Biosensors are highly sensitive, selective, low in cost, and simple to use. In this review, we have provided an overview of reported biosensors for the detection of various types of toxic elements that cause water toxicity. A summary of these toxic elements has also been discussed herein. This review aims to provide an overview of advances in biosensing technology used for water monitoring.
水是地球上生命的基础,但由于污染加剧和栖息地退化,水资源短缺日益严重。因此,有必要检测水污染物,以节约用水和水生多样性。监测废水中存在的有毒元素是进一步处理以使其无公害的重要因素。虽然已经开发了各种方法来监测这些有毒元素,但生物传感器可以克服传统方法的局限性。生物传感器具有灵敏度高、选择性强、成本低、使用简单等特点。在这篇综述中,我们提供了报道的生物传感器检测引起水毒性的各种有毒元素的概述。本文还对这些有毒元素作了概述。本文综述了生物传感技术在水监测中的应用进展。
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引用次数: 0
An analytical method to quantify tetrabromobisphenol A (TBBPA) and its conjugated metabolites in rat serum or other biological samples 一种定量大鼠血清或其它生物样品中四溴双酚A (TBBPA)及其共轭代谢物的分析方法
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-23 DOI: 10.1016/j.talo.2025.100537
Mette Stub, Mikael Pedersen, Louise Ramhøj, Kit Granby, Terje Svingen, Agnieszka Anna Niklas
Brominated flame retardants (BFRs) are widely used to enhance fire resistance in consumer and commercial products, but often leach into the environment due to their surface application. Tetrabromobisphenol A (TBBPA), the most applied BFR, has been detected in human serum, urine, and breast milk. TBBPA is readily absorbed from the gastrointestinal tract, undergoing first-pass hepatic metabolism to form the two major metabolites TBBPA-sulfate and TBBPA-glucuronide. Despite evidence linking TBBPA exposure to developmental toxicity, neurobehavioral effects, uterine cancers, and endocrine disrupting potential via thyroid hormone interference, exposure assessments remain challenging. Current methods rely heavily on direct quantification of TBBPA and its metabolites using liquid chromatography-mass spectrometry (LC-MS), but a lack of commercially available TBBPA metabolites at analytical standards is a limiting factor. This study introduces a method to rapidly quantify TBBPA, and after enzymatic deconjugation, its metabolites using LC-Orbitrap. Using this method, TBBPA-glucuronide was the only metabolite detected in rat serum following oral exposure. Native TBBPA was obtained using enzymatic deconjugation of serum. The protocol simplifies exposure evaluation by offering a practical, and rapid, approach for quantifying TBBPA in biological samples.
溴化阻燃剂(BFRs)广泛用于提高消费品和商业产品的耐火性,但由于其表面应用,往往会渗入环境中。四溴双酚A (TBBPA)是应用最广泛的BFR,已在人类血清、尿液和母乳中检测到。TBBPA很容易被胃肠道吸收,经过肝脏首过代谢形成两种主要代谢物TBBPA-sulfate和TBBPA-glucuronide。尽管有证据表明TBBPA暴露与发育毒性、神经行为效应、子宫癌和通过甲状腺激素干扰内分泌的潜在干扰有关,但暴露评估仍然具有挑战性。目前的方法严重依赖于使用液相色谱-质谱(LC-MS)直接定量TBBPA及其代谢物,但缺乏市售的分析标准TBBPA代谢物是一个限制因素。本研究介绍了一种快速定量TBBPA的方法,并在酶解后使用LC-Orbitrap测定其代谢产物。采用该方法,tbbpa -葡糖苷是口服暴露后大鼠血清中唯一检测到的代谢物。用酶解血清获得天然TBBPA。该方案通过提供一种实用、快速的方法来量化生物样品中的TBBPA,从而简化了暴露评估。
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引用次数: 0
Non-invasive electrochemical sensing of toluidine blue in human saliva using silver conductive ink stabilized on paper substrate: A new platform in portable sensor technology 利用稳定在纸基上的银导电油墨对人唾液中的甲苯胺蓝进行无创电化学传感:便携式传感技术的新平台
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-23 DOI: 10.1016/j.talo.2025.100539
Rokhsareh Ebrahimi , Mohammad Hasanzadeh , Nasrin Shadjou
In this study, we developed a novel paper-based electrochemical microsensor for label-free TB detection using conducting silver nano-inks stabilized on the on the surface of photography paper. The silver ink stabilized on the surface of paper which maintained suitable conductivity and structural integrity after repeated bending, indicating excellent flexibility. In addition, the electrodes maintained stable conductivity (resistance of 5.2 Ω) and LED performance at 100 °C, indicating the thermal flexibility of the cellulose modified by ink due to the strong interaction of AgNPs with cellulose substrate. Also, exposure to moisture had minimal effect on the electrical properties, such that the brightness and LED resistance (1.7 Ω, ΔR = 2.7 Ω) remained stable, confirming the moisture resistance of the ink. The electrodes also dried immediately after drawing without requiring more time or temperatures, which was one of the advantages of our synthetic ink. The developed microscale sensor can accurately detect the concentration of salivary TB in the linear range of 10–1000 nM, with a lower limit of quantification of 10 nM, which is considered as suitable range for clinical and diagnostic applications.
在这项研究中,我们开发了一种新型的纸基电化学微传感器,用于无标签结核病检测,该传感器使用的是稳定在相纸表面的导电银纳米油墨。银墨稳定在纸张表面,纸张经多次弯曲后仍保持适当的导电性和结构完整性,显示出优异的柔韧性。此外,电极在100°C下保持稳定的电导率(电阻为5.2 Ω)和LED性能,这表明由于AgNPs与纤维素基质的强相互作用,油墨修饰的纤维素具有热柔韧性。此外,暴露在湿气中对电性能的影响最小,因此亮度和LED电阻(1.7 Ω, ΔR = 2.7 Ω)保持稳定,证实了油墨的防潮性。电极也在绘制后立即干燥,而不需要更多的时间或温度,这是我们的合成墨水的优点之一。所研制的微尺度传感器可在10 ~ 1000 nM的线性范围内准确检测唾液TB浓度,定量下限为10 nM,适合临床和诊断应用。
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引用次数: 0
Portable electrochemiluminescent detection system with 3D printed materials and mobile phone detection 便携式电化学发光检测系统,具有3D打印材料和手机检测
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-22 DOI: 10.1016/j.talo.2025.100535
Patrick J. Herchenbach , Ethan Gomez , Dale Mee , Charles S. Henry , Erin M. Gross
3D printing offers advantages and novel opportunities for the analytical chemistry laboratory. The method presented here used 3D printed materials as the substrates for electrochemiluminescent sensors and used 3D printing to construct a portable housing for the sensors that not only aligns the sensor to the detector but provides a light-tight environment for the luminescence measurement. This work evaluated four different 3D-printed plastics as substrate materials for sensors fabricated from stencil-printed carbon-ink electrodes (SPCE’s). SPCE chips were fabricated that incorporated an electrochemical cell onto three different plastics printed via fused deposition modeling and a plastic printed using stereolithography printing. The chips were used to develop an ECL detection method with the luminophore tris(2,2′-bipyridyl)ruthenium(II) [Ru(bpy)32+] and 2-(dibutylamino)ethanol (DBAE). The ECL reaction between Ru(bpy)32+ and DBAE was used to optimize a chip-based ECL detection method for amine-containing species. The limits of detection (S/N = 3) for DBAE on the four different substrates were similar, ranging from 3 – 4 μM. The method was applied to the detection of the biogenic amine spermidine. The method had a detection limit of ∼130 μM for spermidine. With goals of accessibility and portability, the method also utilized a mobile phone detector, and portability was demonstrated with the use of a USB power supply to generate the voltage for the ECL reaction.
3D打印为分析化学实验室提供了优势和新的机会。本文提出的方法使用3D打印材料作为电化学发光传感器的衬底,并使用3D打印为传感器构建便携式外壳,不仅使传感器与检测器对齐,而且为发光测量提供了一个不透光的环境。这项工作评估了四种不同的3d打印塑料作为由模板打印碳墨水电极(SPCE)制造的传感器的基板材料。SPCE芯片将电化学电池集成到三种不同的塑料上,通过熔融沉积建模印刷,并使用立体光刻印刷。利用芯片建立了发光基团三(2,2′-联吡啶基)钌(II) [Ru(bpy)32+]和2-(二丁基氨基)乙醇(DBAE)的ECL检测方法。利用Ru(bpy)32+与DBAE之间的ECL反应优化了基于芯片的含胺物种ECL检测方法。四种不同底物对DBAE的检出限(S/N = 3)相似,范围为3 ~ 4 μM。该方法适用于生物胺亚精胺的检测。该方法对亚精胺的检出限为~ 130 μM。为了便于使用和携带,该方法还使用了移动电话检测器,并通过使用USB电源来产生ECL反应的电压来证明便携性。
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引用次数: 0
3D-printed carbon black-based electrode for simultaneous determination of ascorbic acid and kojic acid in dermo-cosmetic products 同时测定皮肤化妆品中抗坏血酸和曲酸的3d打印炭黑基电极
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-20 DOI: 10.1016/j.talo.2025.100532
Larissa Gil Lucas , Eduardo Constante Martins , Pãmyla Layene dos Santos , João Paulo Winiarski , Edson Roberto Santana , Iolanda Cruz Vieira , Almir Spinelli
A miniaturized and disposable poly(lactic acid)-carbon black-based working electrode (3D CB-PLA) was developed using 3D printing technology through fused filament fabrication to be applied to the simultaneous analysis of the antioxidant compounds ascorbic acid (vitamin C) and kojic acid. A previous chemical/electrochemical activation of the 3D CB-PLA electrode was carried out in 1.0 mol L−1 NaOH, applying a fixed potential of +1.0 V vs. Ag/AgCl, KCl(sat) for 1800 s. This procedure was necessary to remove a smooth layer of PLA polymer on the electrode surface and to allow the carbon black conductive sites to be exposed. Morphological and spectroscopic characterizations performed before and after activation revealed a rougher surface with an increased presence of oxygenated functional groups, attributed to both the activation process and the enhanced exposure of carbon black. Using cyclic voltammetry in 0.1 mol L−1 Britton-Robinson buffer (pH 7.0), the irreversible oxidation reactions of ascorbic and kojic acids were observed at +0.30 and +0.87 V vs. Ag/AgCl, KCl(sat), respectively. With the experimental conditions optimized, calibration curves were constructed for both analytes by square wave voltammetry, with detection limits of 4.80 and 5.40 µmol L−1 for ascorbic acid and kojic acid, respectively. The activated 3D CB-PLA electrode enabled accurate and precise simultaneous quantification of both antioxidant compounds in facial whitening creams, demonstrating its effectiveness and analytical potential.
利用3D打印技术,通过熔丝制作技术,研制了一种小型化的一次性聚乳酸-炭黑工作电极(3D CB-PLA),用于抗氧化剂抗坏血酸(维生素C)和曲酸的同时分析。在1.0 mol L−1 NaOH溶液中,施加+1.0 V vs. Ag/AgCl, KCl(sat)固定电位1800 s,对3D CB-PLA电极进行化学/电化学活化。这一过程是必要的,以去除电极表面的光滑层PLA聚合物,并允许炭黑导电部位暴露出来。在活化前后进行的形态学和光谱表征显示,由于活化过程和炭黑暴露增强,氧化官能团的存在增加,表面更粗糙。采用循环伏安法,在0.1 mol L−1 briton - robinson缓冲液(pH 7.0)中,在+0.30和+0.87 V (Ag/AgCl, KCl)下,观察了抗坏血酸和曲酸的不可逆氧化反应。在优化实验条件的基础上,建立了抗坏血酸和曲酸的方波伏安法校准曲线,检测限分别为4.80和5.40µmol L−1。激活的3D CB-PLA电极能够准确和精确地同时定量面部美白霜中的两种抗氧化化合物,证明了其有效性和分析潜力。
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引用次数: 0
Sustainable upcycling of watermelon peels into a nanosensor for the selective detection of mefenamic acid, a nonsteroidal anti-inflammatory drug with antioxidant properties, in biofluids and pharmaceutical formulations 西瓜皮的可持续升级回收成为一种纳米传感器,用于选择性检测生物流体和药物配方中的甲氧胺酸,甲氧胺酸是一种具有抗氧化特性的非甾体抗炎药
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-20 DOI: 10.1016/j.talo.2025.100533
Ahmed A. Shokeer, Nora A. Abdallah, Fawzia A. Ibrahim
Mefenamic acid has recently been identified to possess antioxidant properties, expanding its potential applications beyond traditional pain relief. Emerging studies suggest its possible role in the prevention or management of Alzheimer’s disease through its anti-inflammatory and oxidative stress-reducing effects. This study represents an innovative, highly green eco-friendly method for determination of mefenamic acid in plasma, urine and in its pharmaceutical forms. It involves the transformation of waste watermelon peels into a highly fluorescent switch off nanosensor. For the first time, carbon quantum dots were synthesized from watermelon peel in one step via in situ microwave-assisted carbonization process, completed within 17.0 min without the addition of any external chemicals. The synthesized carbon quantum dots were found to have good fluorescence (λex/em 330.0/420.0 nm), high water solubility and good stability. The synthesized carbon dots were characterized using fluorescence spectroscopy, UV–Visible Spectroscopy, X-ray photoelectron spectroscopy, Zeta potential analysis; Transmission electron microscopy and Fourier transform infrared. The formed Carbon dots appeared to have average particle size of 3.69 - 6.19 nm and their shape was spherical. Mefenamic acid, a nonsteroidal anti-inflammatory anthranilic acid derivative with antioxidant properties, was determined using the synthesized carbon quantum dots by inner filter effect (IFE) and static fluorescence quenching mechanism. The quenching effect on the produced carbon quantum dots was utilized for determination of mefenamic acid over the range of (0.50 – 20.0 µg/mL). The % recovery of the developed method was found to be 100.03 ± 0.776 in pure form, 99.973 ± 0.713 in capsule, 99.70 ± 3.740 in plasma and 99.968 ± 4.005 in urine. Determination of mefenamic acid in the presence of different species indicated high selectivity of the suggested method. The validity of the proposed method was assessed according to the ICH recommendations. Different greenness assessment tools were used for evaluation of the proposed method sustainability. By using watermelon peel, typically regarded as waste, this method offers a green and sustainable route for synthesizing carbon quantum dots from natural sources. Also, using water as solvent without using any other organic solvents; it gives a great advantage to our work as it does not produce any chemical or harmful waste, which makes it safe for the analyst and earth.
甲氧胺酸最近被确定具有抗氧化特性,扩大其潜在的应用超出传统的疼痛缓解。新出现的研究表明,它可能通过抗炎和减少氧化应激的作用,在预防或控制阿尔茨海默病方面发挥作用。这项研究代表了一种创新的、高度绿色环保的方法,用于测定血浆、尿液和其药物形式中的甲氧胺酸。它包括将废弃的西瓜皮转化为高荧光开关纳米传感器。首次以西瓜皮为原料,在不添加任何外部化学物质的情况下,采用原位微波辅助碳化工艺一步合成了碳量子点,在17.0 min内完成。合成的碳量子点具有良好的荧光(λex/em 330.0/420.0 nm)、高水溶性和良好的稳定性。采用荧光光谱、紫外-可见光谱、x射线光电子能谱、Zeta电位分析对合成的碳点进行了表征;透射电子显微镜和傅里叶变换红外。形成的碳点平均粒径为3.69 ~ 6.19 nm,形状为球形。甲氧胺酸是一种具有抗氧化性能的非甾体抗炎邻氨基苯酸衍生物,利用合成的碳量子点通过内滤效应(IFE)和静态荧光猝灭机制对其进行了测定。利用对碳量子点的猝灭效应,在(0.50 ~ 20.0µg/mL)范围内测定甲氧胺酸。方法的回收率分别为:纯品(100.03±0.776)、胶囊(99.973±0.713)、血浆(99.70±3.740)、尿液(99.968±4.005)。对不同种类甲芬那酸的测定结果表明,该方法具有较高的选择性。根据ICH的建议评估了所建议方法的有效性。采用不同的绿色评价工具对所提出方法的可持续性进行了评价。通过使用通常被视为废物的西瓜皮,该方法为从天然来源合成碳量子点提供了一条绿色和可持续的途径。同时,以水为溶剂,不使用任何其他有机溶剂;它给我们的工作带来了很大的优势,因为它不会产生任何化学物质或有害废物,这使得它对分析人员和地球都是安全的。
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