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A fast, reproducible and sensitive human-plasma HPLC-fluorescence method to quantify Carvedilol and the error function 一种快速、重复性好、灵敏的人血浆hplc -荧光定量卡维地洛及其误差函数的方法
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-29 DOI: 10.1016/j.talo.2025.100544
Antonio J. Braza, Montserrat Viñas-Bastart, Maria Sureda-Rosich, Cecilia F. Lastra, Eduardo L. Mariño, Pilar Modamio
A robust and sensitive bioanalytical method was developed and fully validated using reverse-phase High-Performance Liquid Chromatography (HPLC) with fluorometric detection for the quantitative analysis of carvedilol in a complex matrix (human plasma). The method demonstrated satisfactory performance within the therapeutic concentration range (3.91–125 ng/mL), showing good linearity (coefficient of variation, CV: 12.05 %), accuracy (relative error, RE: 11.51 %), and precision—both intra-day (CV: 8.31 %) and inter-day (CV: 10.84 %)—as well as a recovery rate of 89.3 %. The lower limit of quantification (LLOQ) and the limit of detection (LOD) were 1.95 ng/mL and 0.98 ng/mL, respectively. Sample stability was confirmed for up to 24 h under autosampler conditions. The method yielded a short retention time of 3.15 minutes, enabling high-throughput analysis. Once validated, an analytical error function, expressed as a standard deviation (SD), was calculated to determine the most appropriate data-weighting approach across the calibration range. The best-fitting function was linear: SD (ng/mL) = 0.322 + 0.086C. An Analytical GREEnness Metric Approach (AGREE) of the method obtained a score of 0.67, indicating a moderately green profile. Due to its simplicity, cost-effectiveness, and rapid turnaround, the method is well suited for routine clinical use and may serve as a practical tool for monitoring medication adherence in healthcare settings, including hospitals.
建立了一种可靠、灵敏的生物分析方法,并充分验证了反相高效液相色谱(HPLC)与荧光检测对复杂基质(人血浆)中卡维地洛的定量分析。该方法在治疗浓度范围(3.91 ~ 125 ng/mL)内具有良好的线性(变异系数:12.05%)、准确度(相对误差:11.51%)、精密度(日内(CV: 8.31%)和日间(CV: 10.84%),回收率为89.3%。定量下限和检出限分别为1.95 ng/mL和0.98 ng/mL。在自动进样器条件下,样品稳定性可达24小时。该方法保留时间短,为3.15分钟,可实现高通量分析。验证后,计算以标准差(SD)表示的分析误差函数,以确定整个校准范围内最合适的数据加权方法。最佳拟合函数为线性:SD (ng/mL) = 0.322 + 0.086C。该方法的分析绿色度量方法(AGREE)得分为0.67,表明适度绿色。由于其简单,成本效益和快速周转,该方法非常适合常规临床使用,并可作为监测医疗机构(包括医院)药物依从性的实用工具。
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引用次数: 0
Application of BSA-modified silica for solid phase extraction of progesterone from river water samples bsa改性二氧化硅固相萃取河水中黄体酮的应用
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-29 DOI: 10.1016/j.talo.2025.100545
Mladen M. Đurđević , Miloš P. Pešić , Tatjana Ž. Verbić
This study reports the development and application of bovine serum albumin (BSA)-modified silica gels as selective and durable sorbents for the solid-phase extraction (SPE) of progesterone from river water samples. One of the sorbents was used for SPE preconcentration followed by progesterone quantification in a sample collected from the Danube River. The standard addition method followed by high-performance liquid chromatography (HPLC-DAD) detection enabled the quantification of progesterone at a concentration of 143.0 ± 4.0 ng/L. At elevated progesterone concentrations (1.0 to 2.0 × 10-7 M), recoveries approached 100 %, demonstrating the high efficiency of the developed extraction sorbents. The overall method recovery ranged from 91.4 to 101.0 %, confirming the method’s accuracy and robustness. Furthermore, under optimized SPE conditions, developed sorbents were highly selective towards progesterone compared to other reproductive hormones. The sorbents exhibited excellent long-term stability, with no significant change in binding efficiency observed over a four-year period (variation lower than 3 %), maintaining consistent recoveries of 94–96 %. Newly developed BSA-modified silica sorbents represent a promising tool for trace analysis of steroid hormones, as well as for their routine environmental monitoring.
本研究报道了牛血清白蛋白(BSA)修饰硅胶作为固相萃取(SPE)河水中黄体酮的选择性和耐用吸附剂的开发和应用。其中一种吸附剂用于多瑙河样品的固相萃取预富集和黄体酮定量。采用标准加入-高效液相色谱法(HPLC-DAD)检测,测定黄体酮浓度为143.0±4.0 ng/L。当黄体酮浓度升高(1.0 ~ 2.0 × 10-7 M)时,回收率接近100%,表明所开发的萃取吸附剂具有较高的效率。总回收率为91.4% ~ 101.0%,证实了该方法的准确性和稳健性。此外,在优化的固相萃取条件下,制备的吸附剂对黄体酮的选择性高于其他生殖激素。吸附剂表现出优异的长期稳定性,在四年的时间内,结合效率没有显著变化(变化低于3%),回收率保持在94 - 96%之间。新开发的bsa改性二氧化硅吸附剂是一种很有前途的工具,用于类固醇激素的痕量分析,以及它们的常规环境监测。
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引用次数: 0
Fabrication of patterned paper-based sensors for highly efficient formaldehyde detection 用于高效甲醛检测的图案纸传感器的制造
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-28 DOI: 10.1016/j.talo.2025.100541
Taeuk Ji , Gwangbeom Nam , Shinwon Hwang, Minju Park, Jung Hwal Shin
Paper-based sensors are widely used in formaldehyde (FA) sensing in various studies. The development of paper-based sensors with high accuracy and rapid response is important for FA detection. In this study, paper-based FA sensors (PFASs) were developed using a commercial inkjet printer, with filter paper as a substrate. The substrate was coated with a reactive solution containing two pH indicators: thymol blue (TB) and bromophenol blue (BPB), and hydroxylamine sulfate. To evaluate the performance of PFASs, the intensity of the color change caused by FA vapor was detected via colorimetry and optimized with respect to the TB:BPB ratio of the solution and the pattern formation during printing. The optimum TB:BPB ratio was 10:1. The response time decreased as the pattern line width decreased and the pore size increased, and check patterns showed a faster response than those of regularly spaced lines. The sensor was tested in an environment with a relative humidity of 50 ± 5 % at room temperature to ensure consistent experimental conditions, minimizing any potential interference from external factors. The color change of the sensor was visibly noticeable for FA concentrations above 1 ppm. Thus, the proposed technique shows great promise for rapid, high-precision FA detection.
纸基传感器广泛应用于甲醛(FA)的检测中。开发高精度、快速响应的纸基传感器对FA检测具有重要意义。在本研究中,利用商用喷墨打印机,以滤纸为基材,开发了基于纸张的FA传感器(PFASs)。底物包被含有两种pH指示剂的反应溶液:百里酚蓝(TB)和溴酚蓝(BPB),以及硫酸羟胺。为了评价PFASs的性能,通过比色法检测FA蒸气引起的颜色变化强度,并根据溶液的TB:BPB比和印刷过程中的图案形成进行优化。最佳TB:BPB比为10:1。随着纹线宽度的减小和孔径的增大,响应时间减小,且格子纹的响应速度快于规则间距纹的响应速度。为了保证实验条件的一致性,最大限度地减少外部因素的潜在干扰,传感器在室温下的相对湿度为50±5%的环境中进行测试。当FA浓度高于1ppm时,传感器的颜色变化明显。因此,该技术对快速、高精度的FA检测具有很大的前景。
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引用次数: 0
Green rapid HPLC method for testing retinol and tocopherol in ophthalmic gels 绿色快速高效液相色谱法测定眼用凝胶中视黄醇和生育酚
IF 3.7 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-08-28 DOI: 10.1016/j.talo.2025.100538
Xiao-Chen Huang , Ahmed Sobhy Darwish , Wageh Sobhy Darwish , Ri-Meng Chen , Jin-Kui Ma
In addition to providing immediate comfort for dry and irritated eyes, vitamin A (retinol) and E (tocopherol) drops strengthen the eyes' defenses. Optic gels, which are compatible with contact lenses, use vitamins A and E to improve vision, soothe and hydrate dry and sensitive eyes, and provide immediate comfort. It is now feasible to determine the amounts of vitamin A and vitamin E in ocular gels thanks to the development and validation of a thorough, rapid, simple, and eco-friendly stability-indicating LC approach. In compliance with ICH guidelines, the two medications underwent a series of assessments. Vitamin A palmitate, vitamin E acetate, and related degradants were successfully resolved via isocratic separation. Utilizing the octadecylsilyl phase at ambient temperature (25° C ± 5°C), both drugs were quantified and qualified. Constant ratios of filtered water (neutral purified water at pH range 5 to 7) to ethanol comprise the isocratic mobile phase, which has a flow rate of 2.0 mL/min. During the 290 nm detection, the concentrations of vitamin A palmitate and vitamin E acetate varied from 5 to 200 IU/mL and 25 to 1000 μg/mL, respectively. The LC technique's ecological benefits are demonstrated by its overall AES grade of 79, AGREE grade of 0.64, MoGAPI grade of 76, BAGI grade of 80, and final whiteness of 95.8. According to research, the suggested method is accurate, reliable, long-lasting, eco-friendly, and distinctive.
除了为干燥和受刺激的眼睛提供即时的舒适外,维生素A(视黄醇)和E(生育酚)滴剂还能增强眼睛的防御能力。光学凝胶,与隐形眼镜兼容,含有维生素A和E,改善视力,舒缓和滋润干燥和敏感的眼睛,并提供即时的舒适。由于开发和验证了一种彻底、快速、简单、环保的稳定性指示LC方法,现在可以测定眼凝胶中维生素A和维生素E的含量。根据ICH指南,对这两种药物进行了一系列评估。维生素A棕榈酸酯、维生素E醋酸酯和相关的降解物通过等温分离成功地分离出来。在室温(25°C±5°C)下,利用十八烷基硅基相对两种药物进行定量鉴定。过滤水(pH值范围为5至7的中性纯净水)与乙醇的恒定比例组成等密度流动相,其流速为2.0 mL/min。在290 nm检测过程中,维生素A棕榈酸酯和维生素E醋酸酯的浓度分别在5 ~ 200 IU/mL和25 ~ 1000 μg/mL之间变化。LC技术的总体AES等级为79,AGREE等级为0.64,MoGAPI等级为76,BAGI等级为80,最终白度为95.8,证明了LC技术的生态效益。研究表明,该方法准确、可靠、持久、环保、独特。
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引用次数: 0
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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