Analytical Methods最新文献_第4页

A rapid isocratic LC-MS/MS method for the quantification of busulfan in human plasma and its clinical application in pediatric bone marrow transplantation. 快速等容LC-MS/MS法定量人血浆中布苏凡及其在小儿骨髓移植中的临床应用。

IF 3 3区化学

Analytical Methods Pub Date : 2026-10-15 DOI: 10.1039/d6ay01474g

Ying Xia, Yong Zhang, Feng Chen

{"title":"A rapid isocratic LC-MS/MS method for the quantification of busulfan in human plasma and its clinical application in pediatric bone marrow transplantation.","authors":"Ying Xia, Yong Zhang, Feng Chen","doi":"10.1039/d6ay01474g","DOIUrl":"10.1039/d6ay01474g","url":null,"abstract":"A rapid isocratic LC-MS/MS method for quantifying busulfan in human plasma was developed and validated. Plasma samples were processed by protein precipitation with acetonitrile using busulfan-d8 as the internal standard. Separation was performed on a Kinetex C18 column (2.1 × 50 mm, 5 µm; Phenomenex) with isocratic elution (water : acetonitrile = 70 : 30, v/v, containing 1 mM formic acid and 1 mM ammonium acetate) at 0.5 mL min-1, with a total run time of 1 min. Detection was conducted using positive electrospray ionization in multiple reaction monitoring mode (m/z 264.1 → 151.1 for busulfan; m/z 272.1 → 159.1 for busulfan-d8). The assay was linear over the concentration range of 0.100-10.0 µg mL-1 (r = 0.9998). Intra- and inter-batch RSD values were <5.5% and bias ranged from -3.6% to 5.0%. Recovery and matrix effect values were 100.1-101.3% and 101.4-101.8%, respectively. The method was successfully applied to 85 pediatric patients undergoing bone marrow transplantation. AUC0-∞ could be reliably estimated in 70 of the 85 patients (82.4%). Of these, 61.4% achieved the target AUC0-∞ (900-1500 µmol min L-1) after the first dose, while 18.6% fell below and 20.0% exceeded the target range, highlighting the substantial pharmacokinetic variability and the inadequacy of weight-based dosing in pediatric patients. This simple, rapid (1 min per sample) method is suitable for busulfan therapeutic drug monitoring in pediatric patients.","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"9119-9127"},"PeriodicalIF":3.0,"publicationDate":"2026-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148943988","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

A machine learning-assisted colorimetric platform based on a Cu-doped carbon dot nanozyme for sensitive detection of N-acetylcysteine in serum. 基于cu掺杂碳点纳米酶的机器学习辅助比色平台灵敏检测血清中n -乙酰半胱氨酸。

IF 3 3区化学

Analytical Methods Pub Date : 2026-10-15 DOI: 10.1039/d6ay01708h

Shanshan Wei, Feifei Wang, Boyang Bai, Yufeng An, Guoying Sun

{"title":"A machine learning-assisted colorimetric platform based on a Cu-doped carbon dot nanozyme for sensitive detection of N-acetylcysteine in serum.","authors":"Shanshan Wei, Feifei Wang, Boyang Bai, Yufeng An, Guoying Sun","doi":"10.1039/d6ay01708h","DOIUrl":"10.1039/d6ay01708h","url":null,"abstract":"N-Acetylcysteine (NAC), a thiol-containing mucolytic agent for COPD, exhibits significant pharmacokinetic variability among patients, motivating the need for convenient therapeutic monitoring. Herein, a colorimetric platform based on copper-doped chiral carbon dots (Cu-D-CDs) was synthesized via a one-pot hydrothermal route using D-histidine and CuCl2 as precursors. The Cu-D-CDs displayed enhanced peroxidase-like activity, catalyzing H2O2-mediated oxidation of TMB to blue oxTMB (λmax = 652 nm). Upon NAC introduction, oxTMB was reduced via a thiol-disulfide redox reaction, producing an absorbance decrease proportional to NAC concentration. Under optimized conditions, the assay exhibited a linear dynamic range of 10-90 µM, a detection limit of 3.74 µM (LOD = 3σ/S), and recoveries of 96.00-106.60% (RSD < 4%) in mouse serum, demonstrating its feasibility for NAC quantification in serum samples. Beyond the single-wavelength readout at 652 nm, the full-spectral data were further processed by an LSTM network, which significantly improved prediction accuracy (R2 > 0.9998) compared with single-wavelength calibration (R2 = 0.9979), effectively mitigating matrix interference. This integrated colorimetric-LSTM strategy shows promise for COPD therapeutic drug monitoring and pharmaceutical quality control.","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"8939-8949"},"PeriodicalIF":3.0,"publicationDate":"2026-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148878583","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

Uracil-DNA glycosylase-engineered recombinase polymerase amplification for single-nucleotide polymorphism discrimination and genotyping. 尿嘧啶- dna糖基化酶工程重组酶扩增用于单核苷酸多态性鉴别和基因分型。

IF 3 3区化学

Analytical Methods Pub Date : 2026-10-15 DOI: 10.1039/d6ay01745b

Min Zhu, Xiyue Wu, Yangming Zhang, Yuedong Zhu, Mengting Xu, Feng Li, Yanyan Yu

引用次数: 0

Fluorescent aptamer sensing of clenbuterol and salbutamol in artificial urine and construction of a proof-of-concept screening model. 人造尿液中盐酸克仑特罗和沙丁胺醇的荧光适体检测及概念验证筛选模型的构建。

IF 3 3区化学

Analytical Methods Pub Date : 2026-10-15 DOI: 10.1039/d6ay01912a

Qinfeng Dong

{"title":"Fluorescent aptamer sensing of clenbuterol and salbutamol in artificial urine and construction of a proof-of-concept screening model.","authors":"Qinfeng Dong","doi":"10.1039/d6ay01912a","DOIUrl":"https://doi.org/10.1039/d6ay01912a","url":null,"abstract":"A proof-of-concept differential dual-modal aptamer array was developed for clenbuterol (CLB) and salbutamol (SAL) screening in artificial urine. A CLB-selective aptamer and AP-Ago, a broad β2-agonist aptamer, were coupled to graphene-oxide fluorescence resonance energy transfer and to methylene-blue/ferrocene-labelled gold electrodes. Their four responses formed an analyte fingerprint by combining CLB-selective recognition with the broader response of AP-Ago. Seventy-two blind-coded samples represented six matrices, four screening classes and three independent preparation batches. Batches 1-2 (n = 48) supported model development, whereas batch 3 (n = 24; six samples per class) was locked for external assessment. Weighted calibration gave provisional procedural limits of detection of 0.083 ng mL-1 for CLB and 0.164 ng mL-1 for SAL. Mean external prediction-to-reference ratios were approximately 96% for CLB and 81% for SAL, distinct from controlled spike recoveries; intraday precision was 3.7% and interbatch precision was 5.8%. Against isotope-dilution LC-MS/MS, concordance correlation coefficients were 0.939 for CLB and 0.793 for SAL. A regularized multinomial logistic model achieved external balanced accuracy of 0.833, macro-F1 of 0.836 and Matthews correlation coefficient of 0.791. The reported bootstrap 95% confidence interval for balanced accuracy was 0.656-0.969, reflecting the small external set. The results support a candidate front-end triage strategy within the tested artificial matrices: differential signals identify presumptive CLB, SAL-associated high-response and mixed patterns, while any presumptive positive is referred for confirmatory LC-MS/MS rather than used for an anti-doping adjudication.","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":""},"PeriodicalIF":3.0,"publicationDate":"2026-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149177933","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

Comparative evaluation of conventional acid digestion and a calcination-assisted sample preparation for titanium dioxide determination in paints by UV-vis spectrophotometry. 紫外-可见分光光度法测定涂料中二氧化钛的常规酸消解和煅烧辅助样品制备的比较评价。

IF 3 3区化学

Analytical Methods Pub Date : 2026-10-15 DOI: 10.1039/d6ay00744a

Antonio Carlos Magalhães Nichele, João Henrique Zimnoch Dos Santos

{"title":"Comparative evaluation of conventional acid digestion and a calcination-assisted sample preparation for titanium dioxide determination in paints by UV-vis spectrophotometry.","authors":"Antonio Carlos Magalhães Nichele, João Henrique Zimnoch Dos Santos","doi":"10.1039/d6ay00744a","DOIUrl":"10.1039/d6ay00744a","url":null,"abstract":"Titanium dioxide (TiO2) is a critical functional component in paint formulations, providing essential properties such as opacity, whiteness, UV resistance, high cleaning power and durability. Given that TiO2 is among the most expensive raw materials in the industry, accurate quantification is vital for both quality control and cost-benefit optimization. This study aimed to optimize a routine analytical method for TiO2 determination by focusing on the sample preparation stage-the most resource-intensive phase of the process. A comparative analysis was conducted between the traditional direct acid digestion method and a proposed alternative incorporating a calcination step. The performance was evaluated using UV-vis molecular spectroscopy based on validation criteria including analysis time, reagent consumption, and sample throughput. The optimized method demonstrated high linearity (R2 > 0.99) with a Limit of Detection (LOD) and Limit of Quantification (LOQ) of 4.35 and 5.76 mg L-1, respectively. The process proved precise and accurate, with a Coefficient of Variation (CV) below 5.0% and recoveries exceeding 95% across all concentration levels. While statistical differences between analysts were noted for two solvent-based samples (t-test > t-critical of 12.7), the calcination step demonstrated significant advantages for routine operations. Implementation resulted in a 50% reduction in total analysis time, a 25% decrease in acid consumption, and a 75% reduction in energy expenditure. Furthermore, evaluation via the AGREEprep tool confirmed that the proposed method significantly enhances analyst safety and aligns with green analytical chemistry principles.","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"9141-9149"},"PeriodicalIF":3.0,"publicationDate":"2026-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148962669","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

Development of a rapid colorimetric method for detection of synthetic corticosteroids in food and dietary supplements. 一种快速比色法检测食品和膳食补充剂中合成皮质类固醇的方法。

IF 3 3区化学

Analytical Methods Pub Date : 2026-10-15 DOI: 10.1039/d6ay00915h

Shubhangi Pandey, Nishita Pradhan, Pawankumar Rai, Sandeep K Sharma

{"title":"Development of a rapid colorimetric method for detection of synthetic corticosteroids in food and dietary supplements.","authors":"Shubhangi Pandey, Nishita Pradhan, Pawankumar Rai, Sandeep K Sharma","doi":"10.1039/d6ay00915h","DOIUrl":"10.1039/d6ay00915h","url":null,"abstract":"Synthetic corticosteroids such as dexamethasone and prednisolone are widely used for the treatment of various conditions including tumors and skin disorders. Chronic exposure to synthetic corticosteroids leads to adverse health effects such as osteoporosis, hyperglycemia and hypertension. Several dietary and health supplements have recently been reported to be adulterated with synthetic corticosteroids. Conventional analytical techniques such as high-performance liquid chromatography (HPLC), thin-layer chromatography (TLC) and immunochromatography used for detection of these corticosteroids are time-consuming and require trained personnel, necessitating the development of rapid and cost-effective screening methods to ensure food safety. Here, a rapid and cost-effective colorimetric recognition chemistry has been developed for detection of synthetic corticosteroids in dietary supplements. The method employs spectrophotometric quantification of the chromogenic end product at 410 nm, which was further assessed using RGB-based image analysis. Selectivity and interference studies showed no significant matrix interference from the tested structurally similar steroids and common dietary supplement samples. The assay demonstrated a limit of detection (LOD) of 0.04 ± 0.008% (w/v) and a limit of quantification (LOQ) of 0.12 ± 0.027% (w/v) for prednisolone. The developed method is suitable for on-site detection of synthetic corticosteroids, and can be used by regulatory agencies and industries to ensure food safety and human health.","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"9059-9066"},"PeriodicalIF":3.0,"publicationDate":"2026-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148904712","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

Smartphone-assisted dual-mode cyanide ion sensing in environmental and biological matrices using a triphenylamine-quinoline-conjugated chromogenic receptor. 使用三苯胺-喹啉偶联显色受体的智能手机辅助环境和生物基质双模氰化物离子传感。

IF 3 3区化学

Analytical Methods Pub Date : 2026-10-15 DOI: 10.1039/d6ay01475e

Karuppaiyan Kaviya, S Ajay Kumar, Ramar Rajamanikandan, Tsai-Xuan Lin, Shu-Pao Wu, Krishnamoorthy Shanmugaraj, Palanisamy Rajkumar, Kailasam Saravana Mani

{"title":"Smartphone-assisted dual-mode cyanide ion sensing in environmental and biological matrices using a triphenylamine-quinoline-conjugated chromogenic receptor.","authors":"Karuppaiyan Kaviya, S Ajay Kumar, Ramar Rajamanikandan, Tsai-Xuan Lin, Shu-Pao Wu, Krishnamoorthy Shanmugaraj, Palanisamy Rajkumar, Kailasam Saravana Mani","doi":"10.1039/d6ay01475e","DOIUrl":"10.1039/d6ay01475e","url":null,"abstract":"This work presents the efficient recognition of the hazardous chemical cyanide ions (CN- ions) using a newly designed organic molecule-based fluorescent receptor, (E)-4-(4-(diphenylamino)styryl)-1-propylquinolin-1-ium (TAME). CN- ion detection occurs via nucleophilic addition to the styryl group, inducing distinct electronic perturbations as well as blocking of the intramolecular charge transfer (ICT) process. Absorption spectral titration studies reveal a notable blue shift (517-507 nm) in the presence of CN- ions, while steady-state fluorescence measurements demonstrate significant fluorescence quenching (∼82%) with a strong red shift from 553 nm to 576 nm following the interaction of CN- ions with the receptor TAME. The lowest limit of detection (LOD) for this fluorescence-based sensing strategy was calculated to be 1.48 nM, which is much lower than the WHO-permissible limit for cyanide in drinking water. Furthermore, the probe was successfully employed as a paper strip, enabling the portable and effective recognition of CN- ions. Additionally, this sensing system illustrates a notable colour-changing behaviour, which was further exploited for CN- ion detection through a smartphone-based RGB color variation analysis technique. The real-world utility of the receptor TAME was established through its ability for the effective quantification of hazardous CN- ions in various real water and food samples.","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"8905-8916"},"PeriodicalIF":3.0,"publicationDate":"2026-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148904757","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

Automated sample preparation microfluidic platform for immuno-LAMP detection: application to troponin I quantification. 用于免疫lamp检测的自动样品制备微流控平台：在肌钙蛋白I定量中的应用。

IF 3 3区化学

Analytical Methods Pub Date : 2026-10-15 DOI: 10.1039/d6ay00864j

Valentin Tardieux, Mathilde Aubret, Charlotte Parent, Yves Fouillet, Patricia Laurent, Christine Saint-Pierre, François Boizot, Ishaq Gherbi, Leslie Gudimard, Arnaud Buhot, Myriam Cubizolles

{"title":"Automated sample preparation microfluidic platform for immuno-LAMP detection: application to troponin I quantification.","authors":"Valentin Tardieux, Mathilde Aubret, Charlotte Parent, Yves Fouillet, Patricia Laurent, Christine Saint-Pierre, François Boizot, Ishaq Gherbi, Leslie Gudimard, Arnaud Buhot, Myriam Cubizolles","doi":"10.1039/d6ay00864j","DOIUrl":"10.1039/d6ay00864j","url":null,"abstract":"Easy-to-use, highly-sensitive, and quantitative assays over a large dynamic range are needed to improve patient care and disease monitoring. These factors are challenging to address simultaneously using classical methods. The laboratory ELISA assay is relevant for complex matrices over a linear quantification range, whereas immunoassay implementation in commercial lateral flow assays (LFA) remains mostly qualitative. In the case of myocardial infarction (MI), the cardiac biomarker troponin I (cTnI) is present at low levels in the blood of a healthy patient but increases by several orders of magnitude at the onset of symptoms. Here, we aim to detect cTnI as a proof of concept for developing a sample preparation microfluidic system for the immuno loop-mediated isothermal amplification (immuno-LAMP) method. Immuno-LAMP combines the sensitivity and selectivity of antibody recognition with the wide dynamic range allowed through nucleic acid amplifications. cTnI immuno-LAMP assays are firstly validated in a well-plate, and then optimized and integrated into microfluidic cartridges to improve reliability and enable automation. A network of valves and chambers controls a sample preparation module that handles magnetic beads coupled to capture antibodies. Detection antibodies coupled to short oligonucleotides, used to form the immuno-complex, hybridize with an oligonucleotide structure called a dumbbell. This structure is isothermally amplified in tubes to allow the quantification of cTnI. Our work has demonstrated the ability of our automated sample preparation platform to quantify cTnI spiked in human blood plasma at sub-picomolar concentrations. This prototype opens perspectives for integrating the whole immuno-LAMP method from human plasma samples in a microfluidic device including the LAMP amplification and detection.","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"8876-8887"},"PeriodicalIF":3.0,"publicationDate":"2026-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148962701","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

Application of robotic sheath-flow probe electrospray ionization (sfPESI) to wet and dry agricultural products and insecticides. 机器人鞘流探针电喷雾电离（sfPESI）在干湿农产品和杀虫剂中的应用。

IF 3 3区化学

Analytical Methods Pub Date : 2026-10-15 DOI: 10.1039/d6ay01499b

Stephanie Rankin-Turner, Satoshi Ninomiya, Osamu Ariyada, Kenzo Hiraoka

引用次数: 0

Quantification of tadalafil in HLMs using an ultrafast UPLC-MS/MS method to assess metabolic stability, including in silico analysis of metabolic lability, DEREK alerts, and ADME characteristics. 使用超快速UPLC-MS/MS方法定量他达拉非在HLMs中的代谢稳定性评估，包括代谢不稳定性，DEREK警报和ADME特征的硅分析。

IF 3 3区化学

Analytical Methods Pub Date : 2026-10-15 DOI: 10.1039/d6ay01110a

Mohamed W Attwa, Haitham AlRabiah, Obaid S Alruqi, Adnan A Kadi

{"title":"Quantification of tadalafil in HLMs using an ultrafast UPLC-MS/MS method to assess metabolic stability, including in silico analysis of metabolic lability, DEREK alerts, and ADME characteristics.","authors":"Mohamed W Attwa, Haitham AlRabiah, Obaid S Alruqi, Adnan A Kadi","doi":"10.1039/d6ay01110a","DOIUrl":"10.1039/d6ay01110a","url":null,"abstract":"Tadalafil (Cialis) is an FDA-approved oral drug used for benign prostatic hyperplasia, pulmonary arterial hypertension, and erectile dysfunction. A fast, environmentally friendly, and reliable UPLC-MS/MS method was established to quantify tadalafil (TDF) in human liver microsomes (HLMs) and assess its in vitro metabolic stability. Unlike previously reported TDF assays, which target plasma or other biological fluids, the present method uniquely couples HLM-based metabolic-stability assessment with in silico metabolic soft-spot, toxicity, and ADME prediction and dual greenness evaluation in a single workflow. The method is linear over 1 to 4000 ng mL-1, provides detection within 1 min, and maintains high precision and repeatability regardless of the presence of HLMs. TDF and baricitinib (internal standard) were separated using an Eclipse Plus 1.8 µm C18 column (reversed-phase; 50 mm × 2.1 mm), with a mobile phase of 0.1% HCOOH in water (45%) and in acetonitrile (55%). The approach's accuracy and precision ranged from -4.35% to 7.33% (intra-day) and -5.02% to 12.0% (inter-day). TDF's in vitro half-life was 59.65 min, with a slow intrinsic clearance (Clint) of 13.59 mL min-1 kg-1. In silico results reveal that minor modifications at C28 of the 1,3-benzodioxole ring (95%) could enhance the safety and stability of the new derivatives relative to TDF.","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" ","pages":"9016-9032"},"PeriodicalIF":3.0,"publicationDate":"2026-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148899724","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