Analytical Methods最新文献

{"title":"Method validation for analysis of advanced glycation end products in mouse muscle tissue using liquid chromatography-tandem mass spectrometry","authors":"Seyeon Cho, Yu Ra Lee, Sang Keun Ha, Jiyun Ahn, Hyung Joo Suh and Yoonsook Kim","doi":"10.1039/D4AY01602E","DOIUrl":"10.1039/D4AY01602E","url":null,"abstract":"<p >Advanced glycation end products (AGEs) in food and biological samples have been analyzed using several chromatographic and immunological methods, but no studies have quantitatively analyzed the major AGEs, <em>N</em><small>^ε</small>-carboxy-methyl-lysine (CML) and <em>N</em><small>^ε</small>-carboxy-ethyl-lysine (CEL), in muscle tissue. In this study, a quantitative profiling method using ultra-performance liquid chromatography-tandem mass spectrometry in mouse muscle tissue was developed and validated. For extraction, acid hydrolysis and solid-phase extraction were performed. The CML and CEL were well separated and analyzed within 5 min in multiple reaction monitoring mode. The method was validated against ICH guidelines to evaluate the linearity, limits of detection and quantification, matrix effects, recovery, accuracy, and precision, and the validated approach was applied to muscle tissue from aged mice to establish a baseline for the typical range of CML and CEL. This quantitative profiling method has the potential to be applied in the study of diseases influenced by AGEs.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 14","pages":" 2835-2840"},"PeriodicalIF":2.7,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143661617","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}

{"title":"Determination of diazepam and its active metabolites in aquatic products and aquaculture environments using modified QuEChERS-based UPLC-MS/MS†","authors":"Hao Zhou, Feng Xu, Linting Wei, Jiawei Lin, Cheng Zhao, Huiqing Mei, Qi Shan, Qing Wang, Yingchun Mu and Yi Yin","doi":"10.1039/D4AY02144D","DOIUrl":"10.1039/D4AY02144D","url":null,"abstract":"<p >In recent years, the residue of psychotropic drugs such as diazepam in aquatic products has attracted widespread attention and is one of the important hidden dangers to the quality and safety of agricultural products. This study developed a modified QuEChERS method combined with UPLC-MS/MS to determine the residues of diazepam and its active metabolites, nordiazepam, oxazepam, and temazepam, in aquatic products and aquaculture environments. The important variables of the QuEChERS procedure were screened and optimized through single-factor experiments and response surface methodology. The recoveries of analytes in five aquatic products, pond water, and sediment were 87.4–97.8%, 90.4–96.4%, and 85.2–94.7%, respectively, with relative standard deviations of less than 15%. The limits of quantification were 0.1 μg kg<small>⁻¹</small> for the four analytes in aquatic products and sediments, and 5 ng L<small>⁻¹</small> in pond water. This method has been successfully applied to the analysis of diazepam and its active metabolite residues in 28 freshwater aquaculture farms in South China. The detected concentrations of the four analytes in aquatic products, sediments and pond water were 0.18–3.03 μg kg<small>⁻¹</small>, 0.21–17.5 μg kg<small>⁻¹</small> and 5.56–391 ng L<small>⁻¹</small>, respectively. The illegal abuse of diazepam in fishing bait may be an important source of pollution in aquatic products. The risk assessment results showed that the residues of diazepam in aquaculture posed an acceptable risk to human health and a medium risk to the ecosystem. These results confirmed that the established method is suitable for the simultaneous analysis of diazepam and its active metabolites in aquatic products and aquaculture environments.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2806-2816"},"PeriodicalIF":2.7,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143655629","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}

{"title":"Development and validation of a novel UV-TOF MS method for real-time exhaled propofol analysis in Beagles†","authors":"Pan Chang, Xiaoxiao Li, Xing Liu, Yi Kang, Deying Gong, Wenwen Li, Zhongjun Zhao, Tao Zhu, Jin Liu and Wen-sheng Zhang","doi":"10.1039/D4AY02131B","DOIUrl":"10.1039/D4AY02131B","url":null,"abstract":"<p >Propofol, a fast-acting anesthetic, requires precise titration to minimize adverse effects. While plasma-based monitoring is slow, exhaled propofol offers a real-time, non-invasive alternative, though its clinical application remains limited. This study evaluates ultraviolet time-of-flight mass spectrometry (UV-TOF MS) for real-time monitoring, presenting its calibration and validation in Beagle dogs. Calibration showed excellent linearity (<em>R</em><small>²</small> = 0.9939) over 3.23–46.13 ppbv. The intra-day imprecision at propofol concentrations of 4.61 and 23.06 ppbv was below 5.83% and 7.75%, respectively, while the inter-day imprecision was 9.69% and 9.75%, respectively. Carry-over effects were minimal, with signal recovery within 40–60 s, measuring 8.7%, 9.1%, and 4.7% at 4.61, 9.30, and 23.06 ppbv, respectively. In Beagle dogs, <em>C</em><small>_exhaled</small> exhibited a moderately strong linear correlation with <em>C</em><small>_plasma</small> (<em>R</em><small>²</small> = 0.7950) and a moderate correlation with sedative effects, as indicated by the bispectral index (<em>R</em><small>²</small> = 0.5501) after a single bolus injection. Pharmacokinetic (PK) analysis revealed a delay in peak concentration (<em>T</em><small>_max</small>) for <em>C</em><small>_exhaled</small> (2.00 ± 0.21 min) compared to <em>C</em><small>_plasma</small> (1.00 ± 0.00 min). While AUC values were not directly comparable, both exhibited R_AUC &gt; 80%, indicating reliable drug kinetic reflection. Mean residence time (MRT) and elimination rate constants (<em>λ</em><small>_z</small>) showed no significant differences. These results suggest that exhaled breath analysis provides pharmacokinetic insights comparable to plasma, with a slight delay in peak concentration. UV-TOF MS proved to be an efficient method for detecting exhaled propofol, offering potential for real-time anesthesia monitoring in clinical settings.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 11","pages":" 2467-2476"},"PeriodicalIF":2.7,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ay/d4ay02131b?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143539423","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Classification of roasted coffee bean products using laser-induced breakdown spectroscopy: a novel variable selection approach for multiclass modeling","authors":"Yujin Oh, Heesu Chae, Hyemin Jung, Sandeep Kumar, Sang-Ho Nam and Yonghoon Lee","doi":"10.1039/D5AY00124B","DOIUrl":"10.1039/D5AY00124B","url":null,"abstract":"<p >The classification of coffee beans by species, origin, and quality is essential in the coffee industry to ensure authenticity and consistency. While existing methods like spectroscopic and chromatographic techniques offer valuable insights, some require complex sample preparation, while others, such as near-infrared (NIR) and visible/near-infrared (VIS/NIR), rely on molecular information that is labile during coffee roasting. Laser-induced breakdown spectroscopy (LIBS), a fast and minimally invasive elemental analysis technique, shows promise for food authentication. In this study, we evaluated the feasibility of combining LIBS with the <em>k</em>-nearest neighbors (<em>k</em>-NN) algorithm to classify 12 roasted coffee bean products available in South Korean markets. LIBS spectra revealed emission peaks for elements such as Li, Na, K, Rb, Mg, Ca, C, H, and O, along with molecular emission bands of CN and C<small>₂</small>. Using the newly developed statistical concept of the ‘inter-to-intraclass variation ratio,’ the emission intensities of Li, Na, and Rb were identified as key discriminatory variables for the classification model. The <em>k</em>-NN model achieved a classification accuracy of 96.0% with <em>k</em> = 1, which improved to 98.5% with standard deviation-based scaling and <em>k</em> = 3. It should be emphasized that the model based on the Li, Na, and Rb composition is not expected to be labile during the coffee bean roasting process. These findings underscore the potential of LIBS, combined with a simple machine-learning algorithm, as a practical and efficient tool for authenticating coffee products, leveraging its high sensitivity to alkali metal elements for rapid and accurate classification.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 11","pages":" 2437-2445"},"PeriodicalIF":2.7,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143539420","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}

{"title":"Chemometric-assisted electrochemical sensor for simultaneous determination of neonicotinoids imidacloprid and thiamethoxam in honey samples†","authors":"Matias Alberto Cardenas, Macarena Vignati, Gastón Darío Pierini, Sebastián Noel Robledo, Marcela Beatriz Moressi and Fabiana D'Eramo","doi":"10.1039/D4AY02247E","DOIUrl":"10.1039/D4AY02247E","url":null,"abstract":"<p >Neonicotinoids are systemic insecticides used in agriculture. In particular, imidacloprid (IM) and thiamethoxam (TM) have selective toxicity to insects, and they have been implicated in the steep decline of the global honeybee population, specifically in colony collapse disorder (CCD). Some scientific reports have shown that a significant amount of honey worldwide contains traces of neonicotinoids, at levels strong enough to cause damage to bees. Therefore, the development of portable and low-cost sensor devices to permit rapid detection of these neonicotinoids in the field (<em>in situ</em>) is of great importance. The main goal of this work was the development of an electrochemical method, for the first time, to simultaneously determine IM and TM, which can occur in honey samples from Argentina. The electrochemical sensor was based on a pretreated glassy carbon electrode (GCE) using square wave voltammetry (SWV) as the analytical technique. All parameters involved in the response were optimized using a central composite design. The SWV response was modeled using the artificial neural network (ANN) algorithm. Recovery experiments were performed with spiked honey samples, yielding recovery values from 90% to 107% without pretreatment of the samples. The proposed method is presented as a very good and simple alternative for determining IM and TM in Argentina honeys samples.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 13","pages":" 2686-2696"},"PeriodicalIF":2.7,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143612704","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}

{"title":"A supramolecular polypseudorotaxane material based on novel pillar[5]arene for ultrasensitive Fe3+ reaction†","authors":"Wen-Bo Zhu, Xiao-Wei Zhang, Zhi-Jun Li, Li-Yuan Liu, Yu-Quan Zhang, Liang Zhang and Hui Wen","doi":"10.1039/D4AY00832D","DOIUrl":"10.1039/D4AY00832D","url":null,"abstract":"<p >In this study, a novel linear supramolecular polypseudorotaxane was synthesized using a pillar[5]arene derivative (<strong>CP5</strong>) as the host and bis-bromohexyl pillar[5]arene (<strong>DP5</strong>) as the guest, facilitated by host–guest interactions. Subsequently, these components self-assembled to create an <strong>AIE</strong>-active material (<strong>CPDP-G</strong>) through C–H⋯π interactions involving the pillar[5]arene groups. Notably, the <strong>CPDP-G</strong> fluorescence material exhibits an exceptionally sensitive response to Fe<small>³⁺</small>, with a detection limit of 0.543 nM. The fabricated <strong>CPDP-G</strong> film serves as a rudimentary kit for Fe<small>³⁺</small> detection. Moreover, <strong>CPDP-G</strong> demonstrates robust stability under diverse conditions, including variations in temperature, exposure to KClO<small>₄</small>, AcOH, and tetrabutylammonium hydroxide, and ultrasonic treatment. Consequently, the innovative supramolecular polypseudorotaxane material <strong>CPDP-G</strong> holds promising potential for the ultrasensitive detection of Fe<small>³⁺</small> ions.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 12","pages":" 2586-2590"},"PeriodicalIF":2.7,"publicationDate":"2025-02-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143595790","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}

{"title":"Enhancing gel electromembrane extraction using glycine-doped agarose to mitigate electroendosmosis flow: application to tramadol extraction from biological specimens","authors":"Mehdi Navaser, Ardeshir Shokrollahi, Fereshteh Zarghampour and Fatemeh Saeidi","doi":"10.1039/D4AY01939C","DOIUrl":"10.1039/D4AY01939C","url":null,"abstract":"<p >This study involves incorporating glycine into agarose to effectively eliminate electroendosmosis (EEO) effects in gel electromembrane extraction (G-EME) of tramadol (TMD) from biological samples. The development of a glycine-modified agarose membrane for EEO-free tramadol extraction represents a significant advancement in analytical chemistry with far-reaching societal implications. By eliminating the confounding effects of electroendosmosis and eschewing the use of harmful organic solvents typically employed in electromembrane procedures, this environmentally friendly method enhances the accuracy and precision of tramadol quantification in biological matrices. The operational procedure consists of the extraction tramadol, from 10 mL aqueous sample solution (pH 6.0), as the donor phase (DP), transferring it into membrane (pH 5.0); as the final step, it enters into an acceptor phase (AP, 700 μL, pH 4.0). The optimization of critical parameters, including the (w/v) percentage of agarose and glycine, the gel thickness, and the pH levels of the acceptor phase, gel, and donor phase, was conducted utilizing the one-factor-at-a-time methodology, while voltage, time, and stirring rate were optimized employing the design of experiment approach. Remarkably, under the optimized conditions, a satisfactory linear relationship was established within the range of 0.05–6 μg mL<small>⁻¹</small> (<em>R</em><small>²</small> = 0.9925), accompanied by a commendable limit of detection (LOD) amounting to 0.015 μg mL<small>⁻¹</small>, with an extraction recovery rate of 94%. Finally, the proposed method was successfully applied to the determination of TMD in urine, plasma, and tablet samples.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 11","pages":" 2398-2408"},"PeriodicalIF":2.7,"publicationDate":"2025-02-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143514204","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}

{"title":"A microfluidic DNA sensor array for real-time screening of early-stage lung cancer by simultaneous detection of multiple miRNAs†","authors":"Jian Zhang, Wen Yao, Xuanjiao Mao, Xinyu Hu, Li Lv and Haochen Qi","doi":"10.1039/D5AY00109A","DOIUrl":"10.1039/D5AY00109A","url":null,"abstract":"<p >We present a DNA sensor array for simultaneous detection of four targeted miRNAs in serum for early-stage lung cancer screening. Owing to effective microfluidic enrichment coupled with ultrasensitive solid–liquid capacitive sensing, the detection limit is as low as 12.84–24.69 aM, with a dynamic range of 0.1 fM to 10 pM. The response time for each miRNA detection is only 30 s, and the total detection time is 120 s. The selectivity reaches above 10 000 : 1. The miRNA concentrations in the patients with early-stage lung cancer are determined to be 6.5–263 times higher than those in healthy individuals, demonstrating the excellent feasibility of this sensor array for clinical applications for real-time screening of early-stage lung cancer.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 11","pages":" 2376-2379"},"PeriodicalIF":2.7,"publicationDate":"2025-02-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143539397","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}

{"title":"An easily synthesizable naphthalene-based sensing platform for Al3+ and Zn2+ ions: theoretical insights and live cells imaging†","authors":"Jolly Kaushal, Sain Singh, Heena, Saakshi Saini and Partha Roy","doi":"10.1039/D5AY00044K","DOIUrl":"10.1039/D5AY00044K","url":null,"abstract":"<p >A new naphthalene-derived Schiff base probe, 1-((2-(diphenylphosphino)ethylimino)methyl)naphthalen-2-ol (<strong>HL</strong>), has been demonstrated for fluorometric detection of Al<small>³⁺</small> and Zn<small>²⁺</small> ions. <strong>HL</strong> was characterized by elemental analysis, FT-IR, NMR, UV-Vis, fluorescence, and ESI-MS analyses. It exhibited high sensitivity and selectivity toward Al<small>³⁺</small> and Zn<small>²⁺</small> ions in a semi-aqueous medium (CH<small>₃</small>CN–H<small>₂</small>O; 4 : 1, v/v), remaining unaffected by other competing metal ions. As a ‘turn-on’ fluorogenic probe, <strong>HL</strong> displayed strong emission enhancements at 430 nm and 450 nm (<em>λ</em><small>_ex</small> 300 nm) upon the addition of Al<small>³⁺</small> and Zn<small>²⁺</small> ions, respectively, with detection limits of 0.62 μM for Al<small>³⁺</small> and 0.54 μM for Zn<small>²⁺</small>. The addition of Al<small>³⁺</small> caused <em>ca.</em> 20 nm blue-shift in emission and absorption maxima of <strong>HL</strong> due to strong complex formation. The calculated binding constant values were found to be 1.39 × 10<small>³</small> M<small>⁻¹</small> and 4.78 × 10<small>³</small> M<small>⁻¹</small>, respectively, for Al<small>³⁺</small> and Zn<small>²⁺</small> ions. Job's plot, NMR, ESI-MS, and density functional theory (DFT) studies supported the metal ion binding mechanism with 1 : 1 stoichiometry. Fluorescence imaging experiments further revealed <strong>HL</strong>'s ability to detect intracellular Al<small>³⁺</small> in live cells with very low cytotoxicity, highlighting its potential as a selective chemosensory probe.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 12","pages":" 2541-2549"},"PeriodicalIF":2.7,"publicationDate":"2025-02-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143583965","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}

{"title":"A high-density 4-vinylpyridine membrane for rapid purification of antibodies†","authors":"Qingrong Wu, Bin Wang and LiYun Zhang","doi":"10.1039/D4AY02100B","DOIUrl":"10.1039/D4AY02100B","url":null,"abstract":"<p >In order to further investigate the mechanism of action of rituximab in humans and its biotransformation, it is essential to obtain high purity rituximab while maintaining its structural and functional integrity. In this study, we proposed and fabricated a small-molecule 4-vinylpyridine-modified high-density membrane material (P4VP@M) using the surface-initiated atom transfer radical polymerization (SI-ATRP) method. This approach can overcome the limitations of conventional enrichment materials, such as long incubation time and low adsorption capacity. P4VP@M incorporates high-density HEMA polymer brushes to prevent non-specific protein adsorption and 4-vinylpyridine polymer brushes for high-performance rituximab enrichment under mild conditions. In addition, P4VP@M has high permeability, hydrophilicity and mechanical strength. Compared to previous methods, this novel material showed excellent rituximab binding capacity (100.3 mg g<small>⁻¹</small>), shorter processing time (only 15 min), and lower cost (only $2). Notably, P4VP@M was able to purify rituximab rapidly and efficiently from the mixture samples and exhibited good selectivity, recovery (&gt;92.6%) and purity (&gt;94.8%). Thus, this proposed purification strategy using P4VP@M has great potential in enriching target proteins from complex samples, as well as contributing to the in-depth study of their biological functions.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 12","pages":" 2577-2585"},"PeriodicalIF":2.7,"publicationDate":"2025-02-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143583953","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}