Analytical science advances最新文献

{"title":"A Selective Phenyl Azo Acetate Substrate for Enhanced Carbonic Anhydrase Functional Analysis.","authors":"Justinas Babinskas, Inga Matijošytė","doi":"10.1002/ansa.70091","DOIUrl":"10.1002/ansa.70091","url":null,"abstract":"<p><p>Carbon dioxide (CO₂) sequestration is a key strategy for mitigating climate change, and biocatalytic approaches offer sustainable, cost-effective alternatives to chemical and physical methods. Carbonic anhydrases (CAs) efficiently catalyse the reversible hydration of CO₂ to bicarbonate, yet their large-scale application is constrained by limited stability and the lack of robust analytical tools for activity and/or inhibition profiling. In this work, we synthesised and characterised a novel phenyl azo dye acetate to address these limitations. The substrate was optimised for spectrophotometric assays, enabling reliable kinetic and inhibition analyses of CAs. Compared with conventional substrates such as <i>p</i>-nitrophenyl acetate and indoxyl acetate, the new assay demonstrated more than 4.5-fold higher sensitivity, substantial thermal stability and wider applicability across tested hydrolases. These findings provide a more robust platform for evaluating CA activity, supporting the development of more efficient biocatalytic systems for CO₂ sequestration.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"7 1","pages":"e70091"},"PeriodicalIF":5.4,"publicationDate":"2026-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13239852/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148201551","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}

{"title":"A Robust Cost-Effective Spectrophotometric Method for Nb Determination in Refractory Nb-doped Gadolinium Zirconate: Overcoming Matrix Dissolution Challenges.","authors":"Poonam Verma, Annapurna Chandane","doi":"10.1002/ansa.70089","DOIUrl":"10.1002/ansa.70089","url":null,"abstract":"<p><p>A simple, robust and cost-effective analytical methodology was developed for the determination of niobium in highly refractory materials: Nb-doped gadolinium zirconate (Gd₂Zr₂O₇:Nb) and niobium pentoxide (Nb₂O₅). The challenge of digesting these matrices was successfully accomplished by establishing two independent dissolution procedures: (i) Fluoride-free digestion under reflux conditions and (ii) microwave-assisted digestion using a minimal volume of hydrofluoric acid (0.1 mL of 40% hydrofluoric acid). This dual digestion approach provides reliability, flexibility and robustness to the method. Subsequent to dissolution of highly refractory solid matrices, a one-step spectrophotometric method for Nb determination based on the formation of peroxoniobium complex in sulfuric acid medium was optimised and developed. The proposed method is easy and straightforward, with fewer procedural steps and requires a lower chemical inventory. The developed method has a wide linear dynamic range of 2-225 ppm Nb spanning two orders of magnitude with a regression coefficient of 0.99945 and a detection limit of 0.4 ppm. The precision obtained is 2.13% (method relative standard deviation [RSD], <i>n</i> = 5) and 0.17% (instrumental RSD, <i>n</i> = 9). The recovery of Nb from spiked samples at a 50 ppm level is greater than 98% and, thereby validating the proposed method. Furthermore, the proposed method is independently authenticated using total reflection X-ray fluorescence/energy-dispersive X-ray fluorescence techniques, with the results showing good agreement within the 95% confidence interval.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"7 ","pages":"e70089"},"PeriodicalIF":5.4,"publicationDate":"2026-05-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13176946/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147966093","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}

{"title":"Comprehensive Quantitative Urinary Steroid Profiling of 29 Steroids Using Liquid Chromatography-Tandem Mass Spectrometry.","authors":"Joshua T Bain, Fozia Shaheen, Alessandro Prete, Lorna C Gilligan, Angela E Taylor","doi":"10.1002/ansa.70087","DOIUrl":"10.1002/ansa.70087","url":null,"abstract":"<p><p>Steroids are critical for numerous physiological processes; disruption in their metabolism is associated with numerous endocrine disorders. Steroid quantification is essential to improve the understanding and diagnosis of these pathologies. Historically, urinary steroid profiling has been performed using low-throughput gas chromatography mass spectrometry (GC-MS), providing holistic coverage of steroid classes with low cross-reactivity. Here, we translate our previous GC-MS urinary steroid profile to a liquid chromatography tandem-MS (LC-MS/MS) platform, offering a validated, comprehensive overview of steroid metabolism with comparatively low sample preparation times and increased throughput. Urinary steroids were enzymatically hydrolysed and extracted via C₁₈ solid-phase extraction. Quantification was conducted using a triple quadrupole mass spectrometer. Chromatographic separation of 27 analytes was completed in 16 min using a C₁₈-T3 column. Due to chromatographic co-elution of tetrahydrocortisol and 5α-tetrahydrocortisol, a second injection was required on a BEH-C₁₈ column for their separation. Lower limit of quantification (LLOQ) ranged from 2 to 20 ng/mL, witha ccuracy (bias) ranging from -18.7% to 19.9%, and precision (percentage coefficient of variation [%CV]) ranging from 4.0% to 18.6%. Matrix effects remained within the ideal range <±15% for all steroids. Recovery ranged from 76% to 103%, and intra- and inter-assay imprecision (CV) ranged from 0.8% to 14.9%. In 40 healthy volunteers, most analytes were detected above the LLOQ in over 95% of samples, although tetrahydro-aldosterone (85%), 5-pregenediol (68%), and pregnanetriol-one (59%) demonstrated lower quantification rates. Diurnal and sex-based variations were observed, with excretion levels significantly higher during daytime and in males. This robust, high-throughput LC-MS/MS method facilitates the simultaneous quantification of multiple steroid classes, enhancing its utility for clinical and research applications in endocrine science.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"7 ","pages":"e70087"},"PeriodicalIF":5.4,"publicationDate":"2026-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13132653/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147824518","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}

{"title":"PANI/PTA/Fe₃O₄ Nanocomposite Coated on Stainless-Steel Towards Efficient Solid-Phase Microextraction of Tetracycline From Human Urine Samples Prior to HPLC-DAD Analysis.","authors":"Sanaz Naghinejad Orang, Hossein Salar Amoli, Mohammad Hasanzadeh","doi":"10.1002/ansa.70086","DOIUrl":"10.1002/ansa.70086","url":null,"abstract":"<p><p>Tetracycline (TC) is a commonly prescribed broad-spectrum antibiotic, and its widespread use together with its persistence in biological matrices, particularly urine, has raised serious concerns related to clinical safety, public health and the emergence of antimicrobial resistance, underscoring the need for its accurate and sensitive determination. In this work, an innovative solid-phase microextraction (SPME) strategy was developed for the efficient extraction of TC from human urine samples using polyaniline/phosphotungstic acid/Fe₃O₄ (PANI/PTA/Fe₃O₄) nanocomposite coated on stainless-steel substrate. Structural characterization of PANI/PTA/Fe₃O₄ using field-emission scanning electron microscopy with energy-dispersive, x-ray diffraction (XRD) and Fourier-transform infrared spectroscopy confirmed the successful incorporation of phosphotungstic acid (PTA) and Fe₃O₄ within the PANI framework. The resulting polymeric coating exhibited a rough and porous morphology, providing numerous active sites for efficient TC adsorption. Key extraction variables, including coating composition, film thickness, solution pH, ionic strength, extraction duration and desorption conditions, were systematically optimized. Under the optimized conditions, the PANI/PTA/Fe₃O₄ nanocomposite exhibited excellent analytical performance, with a limit of detection of 0.97 ng mL^-1, a limit of quantification of 3.24 ng mL^-1 and good linearity (<i>R</i> ² > 0.99) over a wide concentration range. The nanocomposite also exhibited strong reproducibility (intra-day relative standard deviation [RSD] 2.6%-3.9%; inter-day RSD 4.8%-5.0%) and high recoveries in spiked urine samples (99.5%-100.5%). The enhanced sorption performance was attributed to the combined effects of PANI (providing conductivity and π-π/π/hydrogen-bonding interactions), PTA (contributing electrostatic and hydrogen-bonding affinity) and Fe₃O₄ (imparting magnetic stability and surface activity). Overall, the PANI/PTA/Fe₃O₄ nanocomposite represents a robust and efficient SPME coating with strong potential for the determination of TC in complex biological matrices. The proposed SPME-high-performance liquid chromatography (HPLC) methodology may be further adapted for the analysis of other structurally analogous antibiotics and pharmaceutical analytes in complex biological matrices by rational tailoring of the coating composition.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"7 ","pages":"e70086"},"PeriodicalIF":5.4,"publicationDate":"2026-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13132652/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147824562","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}

{"title":"Rapid Analysis of Sports Prohibited Substances in Black Market Pharmaceutical Products Using Atmospheric Solids Analysis Probe-Mass Spectrometry.","authors":"Alisha Henderson, Oliver Krug, Ashley Sage, David Douce, Scott J Campbell, John Moncur, Mario Thevis, Liam M Heaney","doi":"10.1002/ansa.70088","DOIUrl":"10.1002/ansa.70088","url":null,"abstract":"<p><p>Misuse of performance-enhancing substances in sport remains a persistent threat to the values of fair competition, with estimated doping prevalence far exceeding adverse analytical findings in routine testing. This highlights the need for improved surveillance tools capable of rapid and simple, on-site screening methods. This proof-of-concept study evaluated atmospheric solids analysis probe-mass spectrometry (ASAP-MS) as a minimally complex, high-throughput, and potentially deployable approach for detecting prohibited substances in black market products. Sixteen pharmaceutical products previously confirmed to contain prohibited substances were blind-analysed using ASAP-MS, alongside eleven third-party batch-tested sports supplements. Resultant multi-channel spectra were interrogated manually for the presence of known precursor and product ions. In addition, a compound library was developed and applied using software-driven matching. At least one prohibited substance was detected in all products without generating false positives in certified supplements. Manual spectral review identified only 68% of individual substances correctly. Initial issues with false positive detection of trenbolone in testosterone ester products using the software-driven approach were iteratively optimised through alteration of match score thresholds. This achieved 96% correct substance identification and 100% detection for an adverse finding. Moreover, investigation of diagnostic precursor ions via heatmaps offered a complementary and additional reporting tool to reduce false negatives. This work demonstrated that ASAP-MS, with tailored software-driven analysis, provides reliable near-real-time qualitative screening of prohibited substances. More broadly, this supports the potential for portable, rapid mass spectrometry-based screening platforms to strengthen forensic intelligence, accelerate anti-doping investigations, and enhance athlete protection by complementing laboratory-based confirmatory testing in sport.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"7 ","pages":"e70088"},"PeriodicalIF":5.4,"publicationDate":"2026-04-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13124081/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147791720","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}

{"title":"Method Development and Validation for the Simultaneous Analysis of Miconazole Nitrate, Hydrocortisone and Chlorocresol in a Pharmaceutical Topical Cream by Reverse Phase Liquid Chromatography.","authors":"Netai Mukaratirwa-Muchanyereyi, Pretty Chihiya, Stephen Nyoni","doi":"10.1002/ansa.70085","DOIUrl":"10.1002/ansa.70085","url":null,"abstract":"<p><p>Miconazole/Hydrocortisone (HCA) cream is a pharmaceutical formulation developed as a combination of three major components (HCA, miconazole nitrate [MCN] and chlorocresol [CHL]). In some instances, reference monographs used for referencing the quantification of pharmaceutical molecules focus on individual analysis of molecules. Therefore, there is need to develop, optimize and validate methods that simultaneously separate constituents of a combined formulation. In this study, a method for the separation of HCA, MCN and CHL in miconazole/HCA cream was developed by investigating the effect of mobile phase, stationary phase, wavelength and gradient program on the separation of HCA, MCN and CHL in miconazole/HCA cream. A 10 mM ammonium acetate (AAC) buffer pH 5.0 was used. Acetonitrile was used as the organic modifier. An injection volume of 10 µL was used on a C18, 15 cm × 4.6 mm Zorbax. The optimum conditions for reverse phase liquid chromatography were obtained as follows: injection volume (10 µL), column temperature (30°C), flow rate (1 mL/min), gradient elution program: 0 min, 60AAC:40ACN; 4 min, 60AAC:40ACN; 9 min, 5AAC:95ACN; 13 min, 5AAC:95ACN using a C18 stationary phase, UV detector, 5 µm stationary phase pore size and post run of 3 min.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"7 ","pages":"e70085"},"PeriodicalIF":5.4,"publicationDate":"2026-04-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13112079/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147791706","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}

{"title":"Dry Deposition Strategies for MALDI-MS Imaging: Principles, Advances and Emerging Applications.","authors":"Toufik Mahamdi, Oscar Yanes","doi":"10.1002/ansa.70082","DOIUrl":"10.1002/ansa.70082","url":null,"abstract":"<p><p>Matrix-assisted laser desorption/ionisation mass spectrometry imaging (MALDI-MSI) has become a pivotal tool in biomedical research, enabling untargeted, spatially resolved analysis of molecular species in complex biological tissues. Among the critical steps in MALDI-MSI workflows, matrix deposition significantly influences sensitivity, spatial resolution and reproducibility by affecting crystal morphology and analyte extraction efficiency. While wet deposition techniques, such as manual spray-coating, electrospray deposition and automated systems, have been widely adopted, they often suffer from limitations related to solvent-induced analyte delocalisation. These challenges have driven increasing interest in dry matrix deposition methods, which aim to eliminate or minimise solvent use to enhance spatial fidelity and image quality. This review summarises the main dry deposition strategies used in MALDI-MSI, covering their principles, instrumentation, benefits and limitations. It also discusses recent comparative studies (2023-2025) between wet and dry approaches, examining their impact on analytical performance and the increasing importance of dry deposition in high-resolution spatial omics.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"7 ","pages":"e70082"},"PeriodicalIF":5.4,"publicationDate":"2026-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13102396/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147791679","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}

{"title":"","authors":"","doi":"","DOIUrl":"","url":null,"abstract":"","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"7 1","pages":""},"PeriodicalIF":4.1,"publicationDate":"2026-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148077861","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"","authors":"","doi":"","DOIUrl":"","url":null,"abstract":"","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"7 1","pages":""},"PeriodicalIF":4.1,"publicationDate":"2026-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148111155","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Extraction of Sulfachloropyridazine from Food Samples Using Cellulose: Application of Central Composite Design Approach","authors":"Mbuyelo Shikweni,&nbsp;Nikita Tawanda Tavengwa,&nbsp;Rabelani Mudzielwana,&nbsp;Dakalo Ndou,&nbsp;Tebogo Mokgehle","doi":"10.1002/ansa.70084","DOIUrl":"10.1002/ansa.70084","url":null,"abstract":"<p>Sulfonamide antibiotics are among the most widely used veterinary drugs in livestock and often end up contaminating milk, which is subsequently consumed by humans. To mitigate this health hazard, cellulose and its functionalized derivatives were investigated for their ability to extract sulfonamides from milk and honey. The approach used a biodegradable sorbent (cellulose modified with oxalic and adipic acids) and a green solvent system (ATPE, which reduces the usage of harmful organic solvents) to improve sorbent-analyte interactions and extraction efficiency. In comparison to traditional extraction procedures, the suggested method provided a simpler, more cost-effective, and environmentally friendly method for analysing sulfonamides in complex food matrices. To improve adsorption, cellulose was functionalized with oxalic and adipic acids. The resulting sorbents were then characterised using Fourier-transform infrared, Brunauer–Emmett–Teller and scanning electron microscope techniques. Batch adsorption experiments using a central composite design approach were conducted using sulfachloropyridazine to evaluate the adsorption efficiency of cellulose and its functionalized derivatives at varying temperature, time and mass of sorbent. The optimal conditions for the adsorption of sulfachloropyridazine using cellulose, adipic acid functionalized cellulose (cell@AA) and oxalic acid functionalized cellulose (cell@OA) yielded 53%, 57% and 52% extraction, respectively. The optimal conditions for the adsorption of sulfachloropyridazine for temperature, time and mass were 75°C, 180 min and 50 mg for cellulose, 60°C, 180 min and 5 mg for cell@OA, and 75°C, 30 min and 5 mg for cell@AA, respectively. Application studies revealed that the extraction percentages of sulfachloropyridazine from milk using cellulose, cell@OA and cell@AA were 57%, 86% and 68%, respectively. Therefore, the functionalization of cellulose with adipic and oxalic acids proved to influence the adsorption of Sulfachloropyridazine when compared to cellulose.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"7 1","pages":""},"PeriodicalIF":4.1,"publicationDate":"2026-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13081797/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147700964","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}