Analytical Methods最新文献

{"title":"A study of the effect of soil type variability on the quantitative analysis of heavy metals by XRF","authors":"Ying Wang, Tingting Gan, Nanjing Zhao, Gaofang Yin, Tanghu Li, Xingchi Li and Xiaoxuan Tan","doi":"10.1039/D5AY00249D","DOIUrl":"10.1039/D5AY00249D","url":null,"abstract":"<p >To clarify the impact of soil type variability on the quantitative analysis of heavy metals using X-ray fluorescence (XRF), the feasibility of establishing XRF quantitative analysis curves based on 15 different soil types was investigated. Pearson's correlation coefficient was employed to analyze the relationship between the XRF results and soil matrix constituents. The analysis was focused on four specific soil types: grey fluvo-aquic soil, fluvo-aquic soil, purple soil, and rice soil. The differences in the XRF quantitative analysis curves for heavy metals across these soil types were assessed by examining the overlap of the 95% confidence intervals and the cosine distances between the curves. The accuracy of heavy metal content determinations in grey fluvo-aquic soil was evaluated using the quantitative analysis curves derived from the four soil types. It was found that the linear coefficients of determination for the XRF quantitative analysis curves of heavy metals (Zn, Pb, Ni, Cu, Cr, and Cd) established from the 15 soil types were all below 0.2, indicating a poor fit and rendering them unsuitable for accurate analysis. This highlights that variability in soil types, attributed to differences in soil matrix compositions, significantly affects the accuracy of heavy metal quantification by XRF. When the quantitative analysis curves from fluvo-aquic soil, purple soil, and rice soil were applied to assess heavy metal concentrations (Cr, Ni, Cu, Zn, Pb, Cd, As, and Hg) in grey fluvo-aquic soil, significant increases in the average relative errors were noted. Specifically, these errors rose from 9.89%, 8.56%, 13.51%, 7.10%, 9.86%, 26.19%, 6.71%, and 30.97% to the following ranges: 29.74% to 34.80% (minimum 29.74%, maximum 34.80%), 59.82% to 96.34%, 41.12% to 78.33%, 25.33% to 32.64%, 16.92% to 70.36%, 24.07% to 68.79%, 48.91% to 128.98%, and 130.29% to 238.70%, increasing as much as 0.11 to 18.22 times. Such increases indicate that variability among soil types greatly impacts the accuracy of heavy metal quantitative analysis using XRF. This study establishes an important foundation for the precise quantitative detection of heavy metals <em>via</em> XRF across various soil types.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 25","pages":" 5186-5202"},"PeriodicalIF":2.7,"publicationDate":"2025-06-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144273733","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 portable optical device for quantitative detection of lithium in blood plasma†","authors":"Zitong Ye, Ziwei Huang, Jie Zhou, Haonan Li, Muyang Zhang, Qinghao He, Hao Chen, Jiahua Zhong, Huiru Zhang, Zhuoting Han, Lok Ting Chu and Weijin Guo","doi":"10.1039/D5AY00469A","DOIUrl":"10.1039/D5AY00469A","url":null,"abstract":"<p >Lithium ion (Li<small>⁺</small>) monitoring is critical for managing bipolar disorder therapy, yet conventional detection methods rely on bulky instruments and are not suitable for point-of-care diagnostics (POCD). Here, we present a portable biosensor for rapid and accurate Li<small>⁺</small> quantification in human blood plasma. The device operates based on absorbance changes at 505–525 nm induced by Li<small>⁺</small>-specific complexation with a porphyrinoid reagent. A nonlinear logistic calibration curve (<em>R</em><small>²</small> = 0.999) is established across 0–2.0 mM Li<small>⁺</small>, demonstrating high repeatability. In addition, validation using independent spiked samples (0.2–1.8 mM) shows an excellent agreement between measured and actual concentrations (<em>R</em><small>²</small> = 0.995). Moreover, specificity testing confirms robust anti-interference capability against a range of common cations. The system features automated light intensity stabilization and user-friendly operation, achieving sample-to-result within 2.0 min using 3.0 μL plasma. The device is compact and handheld, with a per-device cost of only $34.8 and a per-test cost of only $1.62. This low-cost portable device addresses the urgent need for decentralized lithium therapeutic drug monitoring, particularly in resource-limited settings.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 26","pages":" 5355-5361"},"PeriodicalIF":2.7,"publicationDate":"2025-06-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144473359","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 simple, sensitive, and green method for the determination of 5-fluorouracil exploiting luminol electrochemiluminescence","authors":"Barbara Rodrigues Demétrio, Dênio Emanuel Pires Souto, Saimon Moraes Silva, Flávio Santos Damos and Rita de Cássia Silva Luz","doi":"10.1039/D5AY00825E","DOIUrl":"10.1039/D5AY00825E","url":null,"abstract":"<p >This study presents a simple, sensitive, and environmentally friendly analytical method based on luminol electrochemiluminescence (ECL) for the quantification of 5-fluorouracil. The approach relies on the suppression of the luminol/hydrogen peroxide ECL signal in the presence of the analyte using a screen-printed carbon electrode (SPE). The total solution volume containing luminol, hydrogen peroxide, and the drug was only 40 μL, ensuring significant reagent savings and minimal waste generation, which qualifies it as a green analytical method. Under optimized conditions, the ECL method displayed a wide linear response range from 0.3 to 10 000 nmol L<small>⁻¹</small>. The proposed technique achieved a detection limit of 0.1 nmol L<small>⁻¹</small> and was successfully applied for the determination of 5-fluorouracil in artificial urine and plasma samples, with recovery values ranging from 95.00% to 100.18% and 97.54% to 103.74%, respectively.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 25","pages":" 5210-5220"},"PeriodicalIF":2.7,"publicationDate":"2025-06-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144273732","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 application of an ultrasensitive immunoassay for antiphospholipase A2 receptor antibodies in the differential diagnosis of membranous nephropathy†","authors":"Shang Gao, Zhenling Deng, Shangbin Kao, Danxia Zheng, Tianyu Zheng, Canlong Yan, Meichun Chen, Yuting Liu, Yuan Qin, Yao Yao, Xiumei Zhou, Jiansuo Zhou, Yue Wang and Biao Huang","doi":"10.1039/D5AY00539F","DOIUrl":"10.1039/D5AY00539F","url":null,"abstract":"<p > <em>Objective</em>: to develop an ultrasensitive time-resolved fluoroimmunoassay (TRFIA) for anti-PLA2R IgG to improve serological diagnosis of primary membranous nephropathy (PMN). The three-step indirect TRFIA uses signal cascade amplification to enhance sensitivity while maintaining specificity, aiming to increase positive detection rates in PMN patients and evaluate analytical performance and clinical utility in 65 PMN patients (including 34 patients with negative Elisa test values), disease controls, and healthy controls. <em>Results</em>: the ultrasensitive PLA2R-IgG-TRFIA had a sensitivity of 0.44 RU per mL, a wide linear range (2.3–550 RU per mL), low intra- (3.16–5.76%) and inter-assay (4.39–9.19%) CVs, and acceptable recoveries (95.48–107.54%). A cutoff of 4.28 RU per mL ensured 100% specificity. It detected anti-PLA2R IgG in 26 of the 34 ELISA-negative PMN sera, consistent with pathology. <em>Conclusion</em>: the ultrasensitive PLA2R-IgG-TRFIA method for detecting anti-PLA2R IgG achieves higher sensitivity and specificity compared to ELISA, thus increasing the positive detection rate of PMN.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 26","pages":" 5473-5479"},"PeriodicalIF":2.7,"publicationDate":"2025-06-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144473360","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":"Dual detection of hypervirulent genes of Klebsiella pneumoniae using a single CRISPR-Cas12a system modulated using entropy-driven circuits†","authors":"Wenqiao Long, Qin Li, Tingting Jin, Zhishun Lu, Fangfang Hu, Hua Zhang and Yongjie Xu","doi":"10.1039/D5AY00563A","DOIUrl":"10.1039/D5AY00563A","url":null,"abstract":"<p >A set of different CRISPR-based analyses have been extensively used to detect nucleic acids owing to their characteristics of being sensitive, specific, rapid and easy to operate. However, one of its major challenges is application to multiplex detection (https://pubmed.ncbi.nlm.nih.gov/31460243/) using a single CRISPR-Cas system because the detection relies on the indiscriminate <em>trans</em>-cleavage activity of the Cas protein. Here we developed a CRISPR-based dual gene assay system for hypervirulent <em>Klebsiella pneumoniae</em> (hv<em>Kp</em>) by integrating two parallel entropy-driven circuits (EDCs) and the <em>trans</em>-cleavage activity of the Cas12a protein towards fluorescent substrate reporters. The EDC reaction released two different fluorescent reporters and the same trigger probe according to different targets. The trigger probe activated the <em>trans</em>-cleavage activity of Cas12a towards reporter probes to achieve the purpose of the dual detection of different genes with a single CRISPR-Cas12a system in one tube. Furthermore, the assay system was designed to detect different mRNA sequences (<em>rmpA</em> and <em>peg-344</em>) of hv<em>Kp</em>, requiring no reverse transcription procedure and providing technical support for the identification of hv<em>Kp</em> and classical <em>Klebsiella pneumoniae</em> (c<em>Kp</em>). The detection limits for <em>rmpA</em> and <em>peg-344</em> were as low as 0.10 fmol L<small>⁻¹</small> and 0.17 fmol L<small>⁻¹</small>, respectively, within 25 minutes under isothermal conditions. It enabled rapid dual detection of hv<em>Kp</em> in a single tube using only a CRISPR-Cas12a system, demonstrating great potential for point-of-care testing due to its high sensitivity, low cost, and robust ability to detect various mRNA biomarkers.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 26","pages":" 5362-5371"},"PeriodicalIF":2.7,"publicationDate":"2025-06-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144473361","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":"Scientific investigation of Asian lacquerware","authors":"Analytical Methods Committee, AMCTB No. 116","doi":"10.1039/D5AY90063H","DOIUrl":"10.1039/D5AY90063H","url":null,"abstract":"<p >Asian lacquerware, renowned for the durability, lustre and cultural significance of its decorative layers, often needs to be studied in terms of its composition, production techniques and degradation processes. In traditional recipes, lacquer is applied as a coating on the surface of a substrate, and is often mixed with additives such as pigments or overlaid with metal powders and inlays. As a result of this intrinsic complexity, the technical examination and scientific analysis of Asian lacquerware encompasses techniques that target both the organic matrix and the inorganic components. Although the techniques mentioned here can be and are used to analyse organic coatings in general, this Technical Brief focuses on Asian lacquerware due to its particular complexity.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 24","pages":" 5069-5073"},"PeriodicalIF":2.7,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144256843","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":"Diffusive samplers for ambient air quality monitoring","authors":"Analytical Methods Committee, AMCTB No. 117","doi":"10.1039/D5AY90067K","DOIUrl":"10.1039/D5AY90067K","url":null,"abstract":"<p >Air pollution remains a matter of concern for governments, regulators and the general public. Diffusive, or passive, samplers provide a cost-effective, versatile and spatially dense method to sample air pollution that does not require the significant investment needed to operate traditional air quality monitoring instrumentation. This Technical Brief describes the theory and operation of diffusive samplers and how their sampling rates may be calibrated. It also discusses considerations for the deployment of diffusive samplers in outdoor environments and provides examples of their practical use in sampling different air pollutants.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 24","pages":" 5074-5077"},"PeriodicalIF":2.7,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144256842","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":"Optimized BN-CQD fluorescence quenching method for rivaroxaban determination in pharmaceutical and biological samples: mechanistic insights, validation, and greenness assessment†","authors":"Reem M. Alnemari, Rami M. Alzhrani, Maram H. Abduljabbar, Farooq M. Almutairi, Muneef M. Aldhafeeri, Mohammed Almaghrabi, Yusuf S. Althobaiti, Atiah H. Almalki, Mona A. Abdel Rahman and Ahmed Serag","doi":"10.1039/D5AY00602C","DOIUrl":"10.1039/D5AY00602C","url":null,"abstract":"<p >A novel, sensitive, and selective fluorescence-based method for the determination of rivaroxaban, a critical anticoagulant drug, using boron and nitrogen co-doped carbon quantum dots (BN-CQDs) as a “turn-off” fluorescence probe was developed and validated. The morphology and optical properties of the BN-CQDs were thoroughly characterized using dynamic light scattering, transmission electron microscopy, UV-vis spectroscopy, and spectrofluorimetry. A strong blue fluorescence emission of the BN-CQDs was found to be effectively quenched in the presence of rivaroxaban, with the quenching mechanism elucidated through Stern–Volmer analysis and thermodynamic studies, indicating a static quenching process. The influential factors affecting the fluorescence quenching, including pH, BN-CQDs volume, and incubation time, were optimized using response surface methodology to achieve maximal analytical performance. A valid model was obtained with an optimal desirability of 0.903. The developed method was fully validated according to ICH guidelines, demonstrating excellent linearity in the range of 20–400 ng mL<small>⁻¹</small>, high sensitivity with a limit of detection of 6.40 ng mL<small>⁻¹</small>, and satisfactory accuracy and precision. The applicability of the method was demonstrated by successfully determining rivaroxaban in pharmaceutical dosage forms and spiked human plasma samples with high recoveries. Importantly, the greenness and analytical practicality of the developed method were assessed using the AGREE and BAGI tools, respectively, showcasing its superior environmental compatibility and enhanced analytical feasibility compared to the conventional HPLC approach reported in the literature posing a viable, greener, and more practical analytical alternative for rivaroxaban determination.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 25","pages":" 5259-5268"},"PeriodicalIF":2.7,"publicationDate":"2025-06-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144289360","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":"Determining tolfenpyrad in oat samples using solid–liquid extraction with low-temperature purification and analysis by gas chromatography coupled with mass spectrometry†","authors":"Karine Rocha Teófilo, Lucélio Marques Alves Costa, Gustavo Rodrigues Amarante Figueiredo, Lázaro Chaves Sicupira and Flaviano Oliveira Silvério","doi":"10.1039/D5AY00287G","DOIUrl":"10.1039/D5AY00287G","url":null,"abstract":"<p >Tolfenpyrad is an insecticide classified as highly toxic to humans, and was recently approved for use in oat cultivation in Brazil. This approval has raised concerns about potential food safety risks in the country. Thus, the present study aims to optimize and validate solid–liquid extraction with low-temperature purification followed by analysis by gas chromatography coupled with mass spectrometry to quantify tolfenpyrad in oats to facilitate monitoring and inspection for tolfenpyrad use in oat samples. The method consisted of adding 4 g of oats, 4 mL of water, and 8 mL of pure acetonitrile to a bottle with a cap. The mixture was shaken, centrifuged, and refrigerated at −20 °C for 1 h. The supernatant obtained was then transferred to a Falcon tube with 500 mg of Na<small>₂</small>SO<small>₄</small> and 150 mg of C18 sorbent. The mixture was again shaken and centrifuged, and the supernatant was subsequently removed for chromatographic analysis. Under optimized conditions, the method showed selectivity, accuracy, and precision with a recovery of 99.25% and a relative standard deviation of 2.70%. The validated linear range was 3.0 to 150 μg kg<small>⁻¹</small>, with detection and quantification limits of 0.5 and 3.0 μg kg<small>⁻¹</small>, respectively. The calculated matrix effect was 89.23%. The optimized and validated technique was applied to 19 real samples and three samples presented tolfenpyrad at concentrations of 11 to 45 μg kg<small>⁻¹</small>. These results demonstrate the method's potential as a practical tool for routine monitoring of pesticide residues, contributing to strengthening food safety control.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 24","pages":" 5018-5026"},"PeriodicalIF":2.7,"publicationDate":"2025-06-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144245279","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":"Key-enabled molecular rotation modulates intramolecular hydrogen bonding toward a turn-on trace-level N2H4 sensor†","authors":"Dagang Shen, Chang Song, Liqin Liu, Huabao Li, Yingying Ju, Weiwen Jing and Huanhuan Wang","doi":"10.1039/D5AY00676G","DOIUrl":"10.1039/D5AY00676G","url":null,"abstract":"<p >Hydrazine (N<small>₂</small>H<small>₄</small>) is a highly toxic and versatile chemical raw material that has been widely used in industrial production and agricultural applications, but it has also caused environmental pollution. In this research, a fluorescent probe <strong>SDG-2</strong> was designed and synthesized for hydrazine detection through esterification functionalization of pyridinium acylion. Hydrazine induces the hydrolysis of the ester group in <strong>SDG-2</strong> to a hydroxyl group, thereby creating an intramolecular hydrogen bond donor that results in fluorescence enhancement, characteristic of sensitive N<small>₂</small>H<small>₄</small> monitoring. Analytical results demonstrate that <strong>SDG-2</strong> achieves an exceptional detection limit of 0.43 μM with a linear response spanning 20–250 μM. The probe exhibits remarkable selectivity and resistance to interference from competing analytes, accompanied by recovery rates ranging from 92.40 to 106.27% in practical sample analysis. This work establishes a robust molecular platform with significant potential for environmental hydrazine assessment, featuring both operational convenience and analytical reliability. The mechanistic insights into IMHB-mediated sensing provide valuable guidelines for developing advanced fluorogenic probes for environmental chemistry applications.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 29","pages":" 6061-6072"},"PeriodicalIF":2.7,"publicationDate":"2025-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144598940","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}