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User-friendly diameter-based measurement paper sensor for chloride detection in water 基于直径的测量纸传感器,用于检测水中的氯化物,使用方便
Q3 Chemistry Pub Date : 2024-02-27 DOI: 10.1016/j.talo.2024.100305
Benjarat Tasangtong , Thanapit Pholsaptanakorn , Thanakorn Tapsawut , Nisakorn Wiwekwin , Jaruwan Mettakoonpitak , Piyaporn Na Nongkhai , Yupaporn Sameenoi

Chloride (Cl) is an anion widely distributed in nature. It is also an essential parameter to consider when assessing the water quality for ensuring drinking water safety, preventing infrastructure damage, mitigating environmental impact, identifying groundwater contamination. This work presents the first development of a diameter-based measurement paper sensor for chloride analysis using the reaction based on a Mohr's precipitation titration. The paper sensor that has a circular shape with 3-cm diameter was pre-coated with AgNO3 and CrO42− forming brown precipitates of the Ag2CrO4. The sensor was sealed using lamination films with 3-mm diameter hole-punched inlets on the top of the lamination film for sample delivery. To detect chloride, the sensor was simply immersed into the sample. The chloride solution flows into the central sample inlet and spreads radially to undergo the displacement reaction with Ag2CrO4 precipitate, forming AgCl white precipitate whose diameter proportional to the chloride that can be observed within 3 min. Concentration of AgNO3 used was found to impact the analytical figures of merit. The lower AgNO3 concentration yields lower limit of detection, narrower linear range but higher sensitivity. The sensor was applied for chloride analysis in tap water, drinking water and industrial water and the chloride concentration obtained from the developed sensors are not significant differences from those obtained from the standard titration method at 95% confidence interval (two tailed P = 0.08) indicating that the developed sensor provides accurate analysis of chloride in water samples from various sources. The developed sensor was used by the untrained staffs for on-site of analysis chloride in tap water collected at 26 locations in SaenSuk Municipality area, Chonburi, Thailand. The results showed that the chloride level in all samples is in range of 52.2–84.7 mg L−1 which is far below the acceptable range set by the Provincial Waterwork Authority of Thailand (< 250 mg L−1) indicating that the tap water used in this area is safe for consumers.

氯化物(Cl-)是一种在自然界中广泛分布的阴离子。在评估水质以确保饮用水安全、防止基础设施损坏、减轻环境影响和确定地下水污染时,它也是一个必须考虑的重要参数。这项研究首次开发了一种基于直径的测量纸传感器,利用基于莫尔沉淀滴定的反应进行氯化物分析。直径为 3 厘米的圆形纸传感器预先涂有 AgNO3 和 CrO42-,形成 Ag2CrO4 的棕色沉淀。传感器使用层压膜密封,层压膜顶部有直径为 3 毫米的打孔入口,用于样品输送。要检测氯化物,只需将传感器浸入样品中即可。氯化物溶液流入中央样品入口并向径向扩散,与 Ag2CrO4 沉淀发生置换反应,形成 AgCl 白色沉淀,其直径与氯化物成正比,可在 3 分钟内观察到。使用的 AgNO3 浓度会影响分析结果的优劣。AgNO3 浓度越低,检测限越低,线性范围越窄,但灵敏度越高。该传感器被用于分析自来水、饮用水和工业用水中的氯化物,在 95% 的置信区间(双尾 P = 0.08)内,从所开发的传感器中得到的氯化物浓度与从标准滴定法中得到的浓度差异不大,这表明所开发的传感器能准确分析各种来源水样中的氯化物。未经培训的工作人员在泰国春武里府 SaenSuk 市的 26 个地点使用开发的传感器现场分析自来水中的氯化物。结果显示,所有样本中的氯化物含量都在 52.2-84.7 毫克/升之间,远远低于泰国省级水务局规定的可接受范围(250 毫克/升),这表明该地区使用的自来水对消费者是安全的。
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引用次数: 0
3D printed cartridges for the removal of pharmaceuticals from water 用于去除水中药物的 3D 打印墨盒
Q3 Chemistry Pub Date : 2024-02-27 DOI: 10.1016/j.talo.2024.100299
Ankur Jyoti Thakuria , Purushottam Suryavanshi , Subham Banerjee

The entry of pharmaceuticals into water is a key worldwide concern, with drugs being identified in all near-aqueous ecologies at often worrying concentrations. Pharmaceutical waste in environmental water has been shown to affect environmental equilibrium and pose a risk to humans adversely. In the present study, we fabricated a novel system containing 3D printed sustainable, porous Polyethylene terephthalate glycol (PETG) cartridges and RP-HPLC-DAD methodology to remove non-steroidal anti-inflammatory drugs (NSAIDs) such as diclofenac sodium (DS) and indomethacin (IND) from water samples called “Cartridges.” The device was fabricated using fused deposition modeling (FDM)-mediated 3D printing technology using indigenous hot-melt extruded filaments. To enable FDM 3D printing, the filaments were fabricated using PETG as a primary material and polyvinyl alcohol (PVA), Affnisol™, and Eudragit®EPO as water-soluble pore-forming materials. We showed that the thermoplastic, recyclable PETG composite material, which presents microporous properties after removal of PVA, Affnisol™, and Eudragit®EPO, is effective for extracting both drugs from water solution. The usefulness of the current strategy was demonstrated by the extraction of DS and IND from an aqueous solution followed by RP-HPLC analysis. The% extraction recovery was more than 80 % for both drugs, with an overall relative standard deviation of less than 3 %. The proposed approach can bring a ray of hope in extraction and sample preparation in the analytical industry due to a shift to the use of sustainable cartridges with customizable shapes, sizes, and chemical properties.

药物进入水体是全世界关注的一个重要问题,在所有近水生态环境中都发现了药物,其浓度往往令人担忧。环境水体中的药物废物已被证明会影响环境平衡,并对人类构成不利风险。在本研究中,我们制作了一种新型系统,其中包含 3D 打印的可持续多孔聚对苯二甲酸乙二酯(PETG)滤芯和 RP-HPLC-DAD 方法,用于去除水样中的非甾体抗炎药(NSAID),如双氯芬酸钠(DS)和吲哚美辛(IND),称为 "滤芯"。该装置是利用本土热熔挤出长丝,以熔融沉积建模(FDM)为媒介的三维打印技术制造的。为了实现 FDM 3D 打印,我们使用 PETG 作为主要材料,聚乙烯醇 (PVA)、Affnisol™ 和 Eudragit®EPO 作为水溶性孔隙形成材料来制造长丝。我们的研究表明,热塑性可回收 PETG 复合材料在去除 PVA、Affnisol™ 和 Eudragit®EPO 后具有微孔特性,能有效地从水溶液中提取这两种药物。通过从水溶液中萃取 DS 和 IND,然后进行 RP-HPLC 分析,证明了当前策略的实用性。两种药物的提取回收率均超过 80%,总体相对标准偏差小于 3%。由于转向使用具有可定制形状、尺寸和化学性质的可持续滤筒,所提出的方法为分析行业的萃取和样品制备带来了一线希望。
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引用次数: 0
Calibration of a passive sampling device for the determination of nitrogen dioxide in ambient air 校准用于测定环境空气中二氧化氮的被动采样装置
Q3 Chemistry Pub Date : 2024-02-27 DOI: 10.1016/j.talo.2024.100306
Thanh-Binh Huynh , Bao-Thuyen Vo-Ngoc , Trung Dang-Bao , Thi-Kieu-Anh Tran

Nitrogen dioxide (NO2), a common air pollutant, has been widely admitted to be harmful to both the environment and human health, demanding its well-control procedure and corresponding quantification. In this study, NO2 in ambient air was collected by a passive sampling method using the Willems badge diffusive sampler, followed by a derivatization step with the Griess-Saltzman solution, and analyzed by ultraviolet-visible (UV–vis) spectroscopy at 543 nm. The device can be utilized for 168 h of continuous field sampling. The experimental sampling rate (Ke) of (4.02 ± 0.29) × 10−3 m3 h 1 with a relative standard deviation (% RSD) of 9.6 % was determined by conducting parallel experiments between an active sampling method (ISO 6768:1998) and the Willems samplers. After exposure time, samplers could be stored for two weeks in a refrigerator at 4 °C before analyzing. The studied passive diffusive sampler was simple, low-cost, easy to reuse; permitted determining the average concentration of NO2 in ambient air. The average NO2 concentrations for 2-hour to 4-hour sampling periods at different studied sampling sites in Ho Chi Minh city (Vietnam) were ranged from 11.5 to 189 μg m 3.

二氧化氮(NO2)是一种常见的空气污染物,已被广泛认为对环境和人类健康有害,因此需要对其进行良好的控制和相应的定量。在这项研究中,利用威廉斯徽章扩散采样器,采用被动采样法收集环境空气中的二氧化氮,然后用格里斯-萨尔茨曼溶液进行衍生,并用 543 纳米紫外-可见(UV-vis)光谱进行分析。该装置可连续现场采样 168 小时。通过对主动采样方法(ISO 6768:1998)和 Willems 采样器进行平行实验,确定实验采样率 (Ke) 为 (4.02 ± 0.29) × 10-3 m3 h - 1,相对标准偏差 (% RSD) 为 9.6 %。暴露时间结束后,采样器可在 4 °C 的冰箱中保存两周,然后再进行分析。所研究的被动扩散采样器简单、成本低、易于重复使用,可测定环境空气中二氧化氮的平均浓度。在胡志明市(越南)的不同研究采样点,2 小时至 4 小时采样期的二氧化氮平均浓度范围为 11.5 至 189 μg m - 3。
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引用次数: 0
Fixed combination of rivaroxaban and Aspirin: Tablet formulation and analytical method validation 利伐沙班和阿司匹林的固定复方制剂:片剂配方和分析方法验证
Q3 Chemistry Pub Date : 2024-02-26 DOI: 10.1016/j.talo.2024.100298
Hani Naseef , Mosab Afaneh , Moammal Qurt , Abdullah Rabba , Abdallah Abukhalil , Numan Malkieh , Maher Kharouf , Ramzi Moqadi

Rivaroxaban and aspirin are commonly used antithrombotic agents in combination to prevent coronary artery disease (CAD) and atherothrombotic events in adult patients after acute coronary syndrome (ACS) with elevated cardiac biomarkers, or with coronary artery disease (CAD) or symptomatic peripheral artery disease (PAD) in high-risk patients. The recommended dosage is 2.5 mg rivaroxaban twice daily in combination with 75–100 mg aspirin once daily. This study aimed to develop a fixed-dose combination tablet of rivaroxaban (2.5 mg) and aspirin (50 mg) to enhance medication adherence and decrease pill burden.

Compatibility studies were conducted on the active ingredients to develop the product formula. The formula and the manufacturing procedure were chosen based on the risk assessment for each active substance, wet granulation with both actives intragranular was found to have faster dissolution than direct mix formulae. Furthermore, a validated reverse-phase HPLC stability indicator method was developed to detect APIs and their possible degradants.

利伐沙班和阿司匹林是常用的联合抗血栓药物,用于预防急性冠状动脉综合征(ACS)后心脏生物标志物升高的成年患者、冠状动脉疾病(CAD)或无症状外周动脉疾病(PAD)高危患者的冠状动脉疾病(CAD)和动脉粥样硬化血栓事件。推荐剂量为 2.5 毫克利伐沙班,每天两次,联合 75-100 毫克阿司匹林,每天一次。本研究旨在开发一种利伐沙班(2.5 毫克)和阿司匹林(50 毫克)的固定剂量复方片剂,以提高服药依从性并减少药片负担。根据对每种活性物质的风险评估结果,选择了配方和生产程序,发现将两种活性物质粒内湿法制粒比直接混合配方溶解更快。此外,还开发了一种经过验证的反相高效液相色谱稳定性指标法,用于检测原料药及其可能的降解剂。
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引用次数: 0
Method development for an untargeted HS-SPME-GC–MS analysis of terpenes and cannabinoids for the geographical sourcing of Marijuana 针对大麻地理来源的萜烯和大麻素的非目标 HS-SPME-GC-MS 分析方法开发
Q3 Chemistry Pub Date : 2024-02-24 DOI: 10.1016/j.talo.2024.100300
Janet Crespo Cajigas, Vidia A. Gokool , Howard K. Holness, Kenneth G. Furton, Lauryn E. DeGreeff

Despite growing decriminalization of Cannabis sativa (i.e., marijuana) possession throughout the United States of America, there remains to be an ongoing interest in the detection of unlawfully possessed and transported marijuana. This issue has resulted in an increasing interest regarding the generalization and specification related to the canine detection of marijuana. More specifically, canine trainers have expressed concerns on whether canines can generalize on the odor of marijuana regardless of the origin of their training materials. This research aims to differentiate multiple marijuana headspace samples from three regions in the USA based solely on the volatile organic compounds (VOCs) found in their odor profiles. In this study, a heated headspace solid phase micro-extraction (SPME) technique was optimized and implemented for the collection of both volatile terpenes and cannabinoids from marijuana. The headspace samples were analyzed using two full-scan, untargeted, optimized methods on a gas chromatograph coupled to a mass spectrometer (GC–MS), and a variety of chemometric tools were applied to the data to enable differentiation and potential classification between sample populations. Principal component analysis and sparse partial least squares discriminant analysis (sPLS-DA) employed in this study have demonstrated a disparity between marijuana varieties based on geography using the VOCs extracted from their odor profiles. With this research, it is intended to determine some fundamental differences between Cannabis of different geographical origins and set a foundation for the development and advancement of instrumental applications for other non-contact marijuana detection techniques in support of the improvement of illicit substance detection technology.

尽管美国各地越来越多地将持有大麻(即大麻)非刑罪化,但人们对检测非法持有和运输大麻的兴趣依然不减。因此,人们对警犬侦测大麻的通用性和规范性越来越感兴趣。更具体地说,警犬训导员对警犬是否能对大麻气味进行归纳表示担忧,无论其训练材料的来源如何。本研究旨在仅根据气味特征中发现的挥发性有机化合物 (VOC) 来区分来自美国三个地区的多种大麻顶空样品。在这项研究中,对加热顶空固相微萃取 (SPME) 技术进行了优化和实施,以收集大麻中的挥发性萜烯和大麻素。顶空样品通过与质谱仪(GC-MS)耦合的气相色谱仪上的两种全扫描、非目标优化方法进行分析,并将多种化学计量学工具应用于数据,以实现样品群之间的区分和潜在分类。本研究采用的主成分分析和稀疏偏最小二乘判别分析(sPLS-DA)利用从大麻气味特征中提取的挥发性有机化合物,证明了不同地理位置的大麻品种之间存在差异。这项研究旨在确定不同地理产地大麻之间的一些基本差异,并为开发和推进其他非接触式大麻检测技术的仪器应用奠定基础,从而支持非法物质检测技术的改进。
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引用次数: 0
Radiation evaluation assay using a human three-dimensional oral cancer model for clinical radiation therapy. 使用人体三维口腔癌模型进行临床放射治疗的放射评估测定。
Q3 Chemistry Pub Date : 2024-02-16 DOI: 10.1016/j.talo.2024.100297
Lucie Sercombe , Kazuyo Igawa , Kenji Izumi

With the development of various radiation-based cancer therapies, radiobiological evaluation methods instead of traditional clonogenic assays with monolayer single cell culture are required to bridge gaps in clinical data. Heterogeneity within cancer tissues is the reason for bridging the gap between basic and clinical research in cancer radiotherapy. To solve this problem, we investigated an evaluation assay using a three-dimensional (3D) model of cancer tissue. In this study, a 3D model consisting of tumor and stromal layers was used to compare and verify radiobiological effects with conventional two-dimensional (2D) methods. A significant difference in the response to radiation was observed between the 2D and 3D models. The relative number of cancer cells decreased with X-ray dose escalations in the 2D and 3D models. In contrast, the relative number of normal cells was quite different between the 2D and 3D models. Considering the ability of cells to recover from radiation-induced damage, the histological results of the 3D model were reflected in the clinical data. Histopathological analysis using a 3D model is a potential method for evaluating radiobiological effects on the tumor and tumor margins.

随着各种基于辐射的癌症疗法的发展,需要用放射生物学评估方法取代传统的单层单细胞培养克隆生成试验,以弥补临床数据的不足。癌症组织内部的异质性是弥合癌症放射治疗基础研究与临床研究之间差距的原因。为了解决这个问题,我们研究了一种使用癌症组织三维(3D)模型的评估检测方法。在这项研究中,我们使用由肿瘤层和基质层组成的三维模型来比较和验证传统二维(2D)方法的放射生物学效应。二维模型和三维模型对辐射的反应存在明显差异。在二维和三维模型中,癌细胞的相对数量随着 X 射线剂量的增加而减少。相比之下,二维和三维模型中正常细胞的相对数量则大不相同。考虑到细胞从辐射损伤中恢复的能力,三维模型的组织学结果反映在临床数据中。使用三维模型进行组织病理学分析是评估放射生物学对肿瘤和肿瘤边缘影响的一种潜在方法。
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引用次数: 0
Forensic analysis of counterfeit psychotropic drugs 假冒精神药物的法医分析
Q3 Chemistry Pub Date : 2024-02-10 DOI: 10.1016/j.talo.2024.100295
Klara Dégardin, Aurélie Guillemain, Alexandra Feng, Christian Saladin, Stéphanie Paratte, Raphaël Zurbach, Tobias Mohn

Medicine counterfeiting is a worldwide problem affecting all therapeutic areas. The analysis of such products is sometimes a scientific challenge, since their chemical composition is unknown and might be very different from the one of the original product. While some counterfeited drug products are quite easy to detect, others are close in composition with the genuine products. The health consequences of counterfeit medicines are appalling since these products can contain the =rong chemical composition, impurities or toxic compounds, and be manufactured and stored in dreadful conditions that do not even respect the basic hygienic conditions. Providing reliable analytical tools is therefore necessary for an efficient fight against the phenomenon. In this study, the analysis of counterfeits of psychotropic drugs presenting a rare closeness in composition to the genuine drugs will be described. It will be exposed how the choice of reliable analytical strategy and tools is decisive for the correct authentication of such pharmaceuticals. The results of classical methods like High-Performance Liquid Chromatography (HPLC) will be presented. Then the contribution of vibrational spectroscopy and imaging tools, including spectral imaging and Near infrared (NIR) spectroscopy, and spectral imaging, will be described, as well as Gas Chromatography coupled with Mass Spectrometry (GC–MS), 1H Nuclear Magnetic Resonance (NMR), 3D microscopy as support for the physical analysis, and finally X-ray fluorescence spectroscopy (XRF) as an elemental analysis technology. The results of the forensic analysis will also reveal analytical links between the counterfeit cases, providing useful information for law enforcement investigations.

药品造假是一个影响所有治疗领域的世界性问题。对这类产品进行分析有时是一项科学挑战,因为它们的化学成分未知,可能与正品大相径庭。有些假药很容易被发现,但有些假药的成分却与正品很接近。假药对健康造成的后果令人震惊,因为这些产品可能含有错误的化学成分、杂质或有毒化合物,而且生产和储存条件恶劣,甚至不符合基本的卫生条件。因此,提供可靠的分析工具是有效打击这一现象的必要条件。在本研究中,将介绍对成分罕见地接近真药的精神药物假货的分析。研究将揭示选择可靠的分析策略和工具对于正确鉴定此类药品的决定性作用。将介绍高效液相色谱法(HPLC)等经典方法的结果。然后将介绍振动光谱学和成像工具(包括光谱成像和近红外(NIR)光谱学和光谱成像)的贡献,以及气相色谱-质谱联用仪(GC-MS)、1H 核磁共振(NMR)、作为物理分析支持的三维显微镜,最后是作为元素分析技术的 X 射线荧光光谱学(XRF)。法医分析的结果还将揭示假冒案件之间的分析联系,为执法调查提供有用信息。
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引用次数: 0
An equation for fitting distance-based measurements with analyte concentrations: From discrete segments simulation to closed-form solution 基于距离的测量与分析物浓度的拟合方程:从离散片段模拟到闭式求解
Q3 Chemistry Pub Date : 2024-02-07 DOI: 10.1016/j.talo.2024.100296
Prapin Wilairat

In this study, an equation for fitting the band lengths in µPADs to the concentrations/amount of analyte added to the µPAD sample area is derived. A simulation of the band formation is carried out using a discrete segment model. The detector channel is divided into equal segments with the same amount of reagent R in each segment. The sample moves into the channel in steps corresponding to segments of the same size as the detector segment. Each sample segment contains analyte A at C mole ratio to reagent R. Assuming a stoichiometric ratio of 1:1 for reaction between A and R, there will be formation of only one product band in each detector segment. By examining the number of bands (n) formed after N steps, a set of linear algebraic equations is derived to determine the number of bands (n) for any integer values of N and C. By extrapolating this result to real positive numbers, we obtain the equation L=a.CA/(b + CA), where L represents the band length, and CA represents the concentration/amount of analyte. The equation represents a rectangular hyperbola.

在本研究中,得出了一个用于拟合 µPAD 中的带长与添加到 µPAD 样品区域的分析物浓度/数量的方程式。使用离散段模型对谱带的形成进行了模拟。检测器通道被分成相等的区段,每个区段中的试剂 R 量相同。样品以与检测器段相同大小的段为单位进入通道。假设 A 和 R 之间的反应化学计量比为 1:1,则在每个检测器段中只会形成一条产物带。通过检查 N 个步骤后形成的条带数量(n),可以得出一组线性代数方程,从而确定 N 和 C 的任意整数值下的条带数量(n)。将这一结果推断为实数正数,可以得出方程 L=a.CA/(b + CA),其中 L 代表条带长度,CA 代表分析物的浓度/数量。该方程表示一个矩形双曲线。
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引用次数: 0
Validated spectrophotometric approach for the estimation of an antiepileptic drug: retigabine in pure form and pharmaceutical formulations utilizing N-Bromosuccinimide as an oxidant 利用 N-溴代琥珀酰亚胺作为氧化剂,采用经过验证的分光光度法估算纯品和药物制剂中的抗癫痫药物:瑞替加滨
Q3 Chemistry Pub Date : 2024-02-04 DOI: 10.1016/j.talo.2024.100294
Mohannad M. Garoub , Ragaa El Sheikh , Sara G. Mohamed , Moataz S. Mahmoud , Ahmed F. Abdel Allem , Ahmed El Sayed , Ahmed A. Ghazy , Nessma M. Gomaa , Sameh Abdalla , Osama M.A. Salem , Ayman A. Gouda

A spectrophotometric method that is sensitive, easy, accurate, exact, reproducible, and verified has been developed for quantifying a new antiepileptic medication called retigabine in both its pure form and pharmaceutical formulations. The techniques employ N-bromosuccinimide (NBS) as an oxidizing agent and three dyes, namely amaranth, methylene blue, and indigo carmine. The three methods rely on the oxidation reaction of retigabine with an excess of N-bromosuccinimide (NBS) in an acidic environment. The unreacted NBS is then quantified by reacting it with fixed amounts of dyes, specifically amaranth, methylene blue, and indigo carmine. The absorbance at 520 nm, 664 nm, and 610 nm is measured for each respective dye. Linear relationships with high correlation coefficients (0.9992-0.9997) were observed under optimal conditions across concentration ranges of 0.5-12, 0.5-16, and 0.5–10 µg/ml. The limit of detection (LOD) for amaranth, methylene blue, and indigo carmine methods were determined to be 0.15, 0.15, and 0.14 µg/ml, respectively. The accuracy and precision of the approaches have been assessed for both intra-day and inter-day measurements. There was no observable interference caused by the typical tablet excipients. The proposed methodologies were verified in compliance with ICH recommendations and effectively utilized for the analysis of retigabine in pharmaceutical formulations. The reliability of the approaches was confirmed by conducting recovery studies employing the usual addition method. The findings produced by the proposed methods were statistically compared to those of the described approach using the student's t-test and F-test, which showed a significant level of agreement.

本研究开发了一种灵敏、简便、准确、精确、可重复和可验证的分光光度法,用于定量检测一种名为瑞替加滨的新型抗癫痫药物的纯品和药物制剂。该技术采用 N-溴琥珀酰亚胺(NBS)作为氧化剂,并使用三种染料,即苋菜红、亚甲基蓝和靛胭脂红。这三种方法都是利用过量的 N-溴代琥珀酰亚胺(NBS)在酸性环境中对瑞替加滨进行氧化反应。然后将未反应的 NBS 与固定量的染料(特别是苋菜红、亚甲基蓝和靛胭脂红)反应,对其进行定量。测量每种染料在 520 纳米、664 纳米和 610 纳米波长处的吸光度。在最佳条件下,在 0.5-12、0.5-16 和 0.5-10 µg/ml 的浓度范围内观察到线性关系,相关系数较高(0.9992-0.9997)。苋菜、亚甲蓝和靛胭脂红方法的检测限(LOD)分别为 0.15、0.15 和 0.14 µg/ml。对日内和日间测量的准确度和精密度进行了评估。没有观察到典型片剂辅料的干扰。经过验证,所提出的方法符合 ICH 建议,可有效用于分析药物制剂中的瑞替加滨。通过采用通常的添加方法进行回收研究,证实了这些方法的可靠性。使用学生 t 检验和 F 检验对所提出的方法和所描述的方法得出的结果进行了统计比较,结果显示两者具有显著的一致性。
{"title":"Validated spectrophotometric approach for the estimation of an antiepileptic drug: retigabine in pure form and pharmaceutical formulations utilizing N-Bromosuccinimide as an oxidant","authors":"Mohannad M. Garoub ,&nbsp;Ragaa El Sheikh ,&nbsp;Sara G. Mohamed ,&nbsp;Moataz S. Mahmoud ,&nbsp;Ahmed F. Abdel Allem ,&nbsp;Ahmed El Sayed ,&nbsp;Ahmed A. Ghazy ,&nbsp;Nessma M. Gomaa ,&nbsp;Sameh Abdalla ,&nbsp;Osama M.A. Salem ,&nbsp;Ayman A. Gouda","doi":"10.1016/j.talo.2024.100294","DOIUrl":"https://doi.org/10.1016/j.talo.2024.100294","url":null,"abstract":"<div><p>A spectrophotometric method that is sensitive, easy, accurate, exact, reproducible, and verified has been developed for quantifying a new antiepileptic medication called retigabine in both its pure form and pharmaceutical formulations. The techniques employ N-bromosuccinimide (NBS) as an oxidizing agent and three dyes, namely amaranth, methylene blue, and indigo carmine. The three methods rely on the oxidation reaction of retigabine with an excess of N-bromosuccinimide (NBS) in an acidic environment. The unreacted NBS is then quantified by reacting it with fixed amounts of dyes, specifically amaranth, methylene blue, and indigo carmine. The absorbance at 520 nm, 664 nm, and 610 nm is measured for each respective dye. Linear relationships with high correlation coefficients (0.9992-0.9997) were observed under optimal conditions across concentration ranges of 0.5-12, 0.5-16, and 0.5–10 µg/ml. The limit of detection (LOD) for amaranth, methylene blue, and indigo carmine methods were determined to be 0.15, 0.15, and 0.14 µg/ml, respectively. The accuracy and precision of the approaches have been assessed for both intra-day and inter-day measurements. There was no observable interference caused by the typical tablet excipients. The proposed methodologies were verified in compliance with ICH recommendations and effectively utilized for the analysis of retigabine in pharmaceutical formulations. The reliability of the approaches was confirmed by conducting recovery studies employing the usual addition method. The findings produced by the proposed methods were statistically compared to those of the described approach using the student's t-test and F-test, which showed a significant level of agreement.</p></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-02-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666831924000080/pdfft?md5=1f0d4ecf4534f34969eb9ce600700d4b&pid=1-s2.0-S2666831924000080-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139737167","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
Effect of modified Triethanolamine on grinding efficiency and performance of cementitious materials 改性三乙醇胺对水泥基材料研磨效率和性能的影响
Q3 Chemistry Pub Date : 2024-02-04 DOI: 10.1016/j.talo.2024.100293
Yahya Kaya , Veysel Kobya , Ali Mardani , Joseph J. Assaad

This paper seeks to improve through esterification the efficiency of triethanolamine (TEA) molecules used in the cement grinding industry. The unmodified and modified-TEAs are tested at 0.025 % to 0.1 % rates to determine their effect on clinker grindability and cement properties including fineness, flow, zeta potential, morphology, rheology, setting, and compressive strength. Test results showed that the esterification reactions performed to modify the TEA hydroxyl groups can remarkably increase their adsorption potentials onto the clinker grains, which reduces the agglomeration phenomenon and grinding energy consumption by 6 % to 13 %. The TEA modified using medium hydrocarbon chain lengths (4–8 carbons) of mono-carboxylic acid compounds performed better than the one containing short hydrocarbon chain lengths (1–3 carbons). The pastes and mortars prepared using the modified-TEA cements exhibited significantly higher fluidity, better compatibility with polycarboxylate-based superplasticizer, and increased strengths than the equivalent mixtures made using cement ground using the unmodified TEA molecules.

本文旨在通过酯化提高水泥粉磨工业中使用的三乙醇胺(TEA)分子的效率。以 0.025% 至 0.1% 的比率对未改性和改性三乙醇胺进行了测试,以确定它们对熟料可磨性和水泥性能(包括细度、流动性、ZETA 电位、形态、流变学、凝结和抗压强度)的影响。试验结果表明,对三乙醇胺羟基进行改性的酯化反应可显著提高其在熟料颗粒上的吸附潜力,从而减少结块现象,并将粉磨能耗降低 6% 至 13%。使用中等碳氢链长度(4-8 个碳)的单羧酸化合物改性的三乙醇胺比含有短碳氢链长度(1-3 个碳)的三乙醇胺性能更好。与使用未改性三乙醇胺分子研磨的水泥制成的同等混合物相比,使用改性三乙醇胺水泥制备的浆料和砂浆具有明显更高的流动性,与聚羧酸基超塑化剂的相容性更好,强度更高。
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引用次数: 0
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Talanta Open
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