Analytical Methods最新文献

{"title":"Electrochemical aptasensing strategies for emerging organic pollutants in environmental analysis","authors":"Anyou Xie, Weihong Wu and Meiqing Jin","doi":"10.1039/D5AY01084E","DOIUrl":"10.1039/D5AY01084E","url":null,"abstract":"<p >Emerging organic pollutants (EOPs), encompassing a vast array of substances like pharmaceuticals, pesticides, endocrine disruptors, and industrial chemicals, pose a significant threat to environmental integrity and human health. Traditional analytical methods for their detection, while accurate, are often laboratory-bound, costly, and time-consuming, hindering effective environmental monitoring. Electrochemical aptasensors (hereafter, ‘aptasensors’) have surfaced as a highly promising alternative, merging the high sensitivity, potential for portability, and cost-effectiveness of electrochemical transduction with the specific molecular recognition capabilities and stability of aptamers – short, synthetic nucleic acid sequences. This review comprehensively examines the fundamental principles underpinning these sensors, including aptamer selection methodologies like SELEX, particularly addressing the challenges associated with small molecule targets characteristic of many EOPs. It delves into various electrochemical transduction mechanisms such as voltammetry, impedance spectroscopy, and electrochemiluminescence, alongside critical aptamer immobilization techniques onto electrode surfaces. The significant role of diverse nanomaterials (<em>e.g.</em>, gold nanoparticles, carbon-based materials, metal oxides, and MOFs) in enhancing sensor performance through increased surface area, improved conductivity, and signal amplification is thoroughly discussed. Furthermore, this review surveys recent advancements and applications of these aptasensors for detecting key classes of EOPs in environmental matrices like water and soil, critically evaluating reported analytical performance metrics like limits of detection and selectivity.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 38","pages":" 7586-7607"},"PeriodicalIF":2.6,"publicationDate":"2025-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145129586","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-responsive colorimetric and ‘turn on’ fluorometric probes for the rapid detection of Cu2+ and F− ions: crystal structure, spectral elucidation, smartphone-based colorimetric readout, and applications in the bio-imaging of zebrafish larvae","authors":"Ramalingam Gajendhiran, Abbas Khaja Raees Ahmed, Sivaraj Mithra, Seepoo Abdul Majeed, Azeez Sait Sahul Hameed, Saravanan Jegadeeshwari, Kesavan Muthu, MohamedHanifa NizamMohideen and Aziz Kalilur Rahiman","doi":"10.1039/D5AY01091H","DOIUrl":"10.1039/D5AY01091H","url":null,"abstract":"<p >In this work, we report two dual-responsive colorimetric and ‘turn-on’ fluorometric probe molecules 1,5-bis(4-isopropylbenzylidene)carbohydrazone (S1) and 1,5-bis(4-isopropylbenzylidene)thiocarbohydrazone (S2) for the rapid detection of biologically significant inorganic ions. The molecular structure of S1 was confirmed by single crystal X-ray technique, which crystallized in the monoclinic <em>P</em>2<small>_1/<em>c</em></small> space group. The sensor molecules show dual sensing ability, which displayed highly selective optical detection toward Co<small>²⁺</small> and Cu<small>²⁺</small> cations and F<small>⁻</small> anions over other tested cations (K<small>⁺</small>, Mg<small>²⁺</small>, Ca<small>²⁺</small>, Mn<small>²⁺</small>, Fe<small>³⁺</small>, Co<small>²⁺</small>, Ni<small>²⁺</small>, Cu<small>²⁺</small> and Zn<small>²⁺</small>) and anions (F<small>⁻</small>, Cl<small>⁻</small>, Br<small>⁻</small>, I<small>⁻</small>, HSO<small>₄</small><small>⁻</small>, ClO<small>₄</small><small>⁻</small>, NO<small>₃</small><small>⁻</small> and OH<small>⁻</small>), respectively. Astonishingly, the sensor molecules exhibit ‘turn-on’ fluorometric responses for Cu<small>²⁺</small> and F<small>⁻</small> ions. The binding constant of the probes with the sensed ions was determined by the Benesi–Hildebrand equation and found to be between 2.70 × 10<small>⁵</small> and 1.89 × 10<small>⁸</small> M<small>⁻¹</small>, and the limit of detection was found to be between 0.14 and 0.27 μM in the CH<small>₃</small>CN : DMF (9 : 1, v/v) solution. Job's plot analysis showed 1 : 2 stoichiometry between the probes and the cations and 1 : 1 stoichiometry between the probes and the anion. The probe molecules have been applied for on-site quantitative colorimetric analysis using smartphone-based RGB colour values. Besides, the synthesized probes have been successfully demonstrated for the fluorescence imaging of Cu<small>²⁺</small>/F<small>⁻</small> ions in zebrafish gill cells (<em>Dr</em>G) and larvae.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 39","pages":" 7920-7935"},"PeriodicalIF":2.6,"publicationDate":"2025-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145123782","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":"Assessment of the metabolic stability of avapritinib in human liver microsomes using a fast and green UPLC-MS/MS method: screening for structural alarms associated with metabolic lability and in silico toxicity","authors":"Mohamed W. Attwa, Ali S. Abdelhameed, Haitham AlRabiah and Adnan A. Kadi","doi":"10.1039/D5AY01035G","DOIUrl":"10.1039/D5AY01035G","url":null,"abstract":"<p >Avapritinib (Ayvakit™) is a highly selective inhibitor of the platelet-derived growth factor receptor alpha (PDGFRA), including D842V mutations. Avapritinib (APB) is authorized in the United States for individuals with metastatic or unresectable gastrointestinal stromal tumors (GISTs). APB is considered the exclusive therapy for adults with indolent systemic mastocytosis. This study established a rapid, validated, and environmentally friendly UPLC-MS/MS method for assessing APB in human liver microsomes (HLMs), applied to assess the APB metabolic stability. The StarDrop software, with the Metabolism and DEREK modules, was utilized to screen for alerts in the APB chemical structure and assess metabolic stability. APB and encorafenib (ECB as the internal standard) were separated using an isocratic mobile phase approach on an Agilent SB-C18 (reversed-phase) column. The APB calibration curve displayed linearity from 1 ng mL<small>⁻¹</small> to 3000 ng mL<small>⁻¹</small>. The precision and accuracy for intra- and inter-day assessments ranged from 0.53% to 5.67% and −2.18% to 10.33%, respectively. The implemented UPLC-MS/MS approach is ecologically sustainable, utilizing a diminished percentage of an organic solvent (40% acetonitrile), a short elution duration of 1 min, and a low flow rate of 0.35 mL min<small>⁻¹</small>. The metabolic stability characteristics including the intrinsic clearance and the <em>in vitro</em> half-life of APB were determined to be 22.11 mL min<small>⁻¹</small> kg<small>⁻¹</small> and 36.67 min, respectively. <em>In silico</em> analysis suggests that minor structural changes to the methyl pyrazole moiety in drug design may improve the metabolic stability and safety relative to APB.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 37","pages":" 7431-7443"},"PeriodicalIF":2.6,"publicationDate":"2025-09-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145013485","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":"Enhanced detection of N-acetylneuraminic acid using a chemiluminescence enzyme-linked immunosorbent assay","authors":"Abdurrahman Usman, Yaojun Zhu, Murtala Bindawa Isah and Xiaoying Zhang","doi":"10.1039/D5AY01350J","DOIUrl":"10.1039/D5AY01350J","url":null,"abstract":"<p > <em>N</em>-Acetylneuraminic acid (Neu5Ac) is a key sialic acid in food and food products that influences nutritional quality, glycosylation, and microbial interactions. Neu5Ac is integral to cellular recognition, immune modulation, and neural development, and it is a promising diagnostic biomarker, with applications spanning clinical diagnostics, food safety, pharmaceuticals, and targeted therapeutics. By optimizing assay parameters, we developed an improved chemiluminescence enzyme-linked immunosorbent assay (CLEIA) that significantly outperforms our previously established indirect competitive ELISA (ic-ELISA), which had limitations in precision and was prone to interference. The optimized CLEIA achieved an IC<small>₅₀</small> of 1.864 ng mL<small>⁻¹</small>, a limit of detection (LOD) of 0.272 ng mL<small>⁻¹</small>, and a limit of quantification (LOQ) of 1.321 ng mL<small>⁻¹</small>, demonstrating superior sensitivity over the ic-ELISA's LOD of 0.57 ng mL<small>⁻¹</small> and LOQ of 1.14 ng mL<small>⁻¹</small>. Spiked recovery experiments using edible bird's nest, milk, saliva, and urine confirmed the CLEIA's high stability, sensitivity, minimal matrix effects, and suitability for food quality control, safety, clinical, and biomedical applications. This advancement sets a new benchmark in analytical detection and application of Neu5Ac over traditional methods, promising to revolutionize food safety monitoring and clinical diagnostics.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 37","pages":" 7374-7380"},"PeriodicalIF":2.6,"publicationDate":"2025-09-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145068593","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":"Amplified electrochemical detection of sulfadiazine based on Cu-BTC-encapsulated FeNi dual-atom catalysts with improved catalytic efficiency","authors":"Shuhuai Li, Yinian Zhu, Xionghui Ma, Chaohai Pang, Rui Chen and Zongqiang Zhu","doi":"10.1039/D5AY01036E","DOIUrl":"10.1039/D5AY01036E","url":null,"abstract":"<p >The amplification of detection signals is an important method for improving the sensitivity of electrochemical detection. This study presents an efficient strategy for preparing electrochemical catalytic materials using a simple self-assembly technique to encapsulate Fe single atoms (Fe–SAs) and Ni single atoms (Ni–SAs) in the Cu-benzene-1,3,5-tricarboxylic acid (Cu-BTC) metal–organic framework to form a Cu-BTC@FeNi–SAs catalytic system. Subsequently, Cu-BTC@FeNi–SAs was modified on the surface of a gold electrode, and sulfadiazine was used as a template to prepare a molecularly imprinted polymer (MIP) on the modified electrode. After eluting sulfadiazine, an MIP was obtained for specifically recognising sulfadiazine. When sulfadiazine was adsorbed by the MIP, a differential pulse voltammetry (DPV) signal occurred in response, thus detecting sulfadiazine. The adoption of Cu-BTC-fixed FeNi–SAs significantly facilitated mass transfer during the reaction, thus improving the DPV response signal. When used to detect sulfadiazine, the sensor had a linear range from 5 × 10<small>⁻¹²</small> to 6000 × 10<small>⁻¹²</small> mol L<small>⁻¹</small> and a detection limit of 1.14 × 10<small>⁻¹²</small> mol L<small>⁻¹</small>. It also successfully detected sulfadiazine residue in seawater and fish samples with recovery rates between 91.02% and 99.20%.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 37","pages":" 7444-7451"},"PeriodicalIF":2.6,"publicationDate":"2025-09-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145013509","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":"Porous microneedle-based electrochemical sensor for potassium and glucose in skin interstitial fluid","authors":"Dake Ai, Xin Tang, Zhenlong Meng, Yang Yu, Xiuxiu Guo and Yuanpeng Wang","doi":"10.1039/D5AY00915D","DOIUrl":"10.1039/D5AY00915D","url":null,"abstract":"<p >The monitoring of biomarkers in interstitial fluid (ISF) holds significant promise for non-invasive, real-time health assessment. In this study, we present a novel porous microneedle-based electrochemical sensor (PMES) designed for the extraction and detection of key electrolytes and metabolites in ISF. The system integrates porous microneedles (PMNs) with screen-printed electrodes (SPEs) and polyethylene glycol (PEG)-loaded filter paper to facilitate efficient ISF collection and enable electrochemical detection. Both <em>in vitro</em> and <em>in vivo</em> experiments demonstrated the PMES's high biocompatibility and ability to detect potassium and glucose with reproducible, clinically relevant performance. For context, we also fabricated MN-electrode sensors (potentiometric Na<small>⁺</small>; amperometric glucose) and performed head-to-head comparisons, in which PMES exhibited superior long-term stability under identical insertion conditions. Compared with these directly functionalized MN electrodes prepared in this work, PMES maintained signal stability by decoupling ISF extraction (PMNs with PEG-assisted collection) from electrochemical transduction (external SPEs), thereby mitigating abrasion-induced coating delamination and biofouling; this comparison pertains to the architectures tested here and demonstrates the potential of PMES for minimally invasive, time-resolved health monitoring.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 37","pages":" 7541-7550"},"PeriodicalIF":2.6,"publicationDate":"2025-09-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145038884","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":"Structurally tailored Rh–Au heterodimers: plasmon-boosted oxidase mimetics for facile tea authentication via colorimetric sensing","authors":"Kai-Xin Song, Xue-Qing Sang, Yan-Ying Zheng, Jin-Fang Nie, Yun Zhang, Wen-Xin Niu and Ya-Li Yuan","doi":"10.1039/D5AY01236H","DOIUrl":"10.1039/D5AY01236H","url":null,"abstract":"<p >While nanozymes show remarkable potential in colorimetric sensing, conventional systems often suffer from compromised sensitivity and operational complexity in complex analytical scenarios. Herein, a novel heterostructured nanozyme by integrating Au nanoparticles with Rh nanocubes is engineered to address this challenge. By precisely constructing cubic-spherical Rh–Au heterodimers (dimers) with controlled interfacial geometry, a 2.5-fold enhancement in oxidase-mimetic activity compared to the monometallic counterpart is achieved along with a (54 ± 5)% decrease in the activation energy (<em>E</em><small>_a</small>) for the oxidation of 3,3′,5,5′-tetramethylbenzidine (TMB), using the absorbance of oxidized TMB (oxTMB) as the signal. This result arises from the localized surface plasmon resonance (LSPR) effect, which catalyzes the increased production of reactive oxygen species (ROS). Taking the absorbance of oxTMB as the signal, a multi-channel colorimetric sensing system for tea polyphenol discrimination and tea authentication is developed based on Rh–Au dimers, eliminating the conventional requirement for hydrogen peroxide in the detection process. The experimental data were systematically analyzed through principal component analysis (PCA) and hierarchical cluster analysis (HCA), enabling effective classification of seven polyphenols down to 1 μM. Besides, polyphenol mixtures of 7 components as the real sample mimics, together with diverse tea samples of different storage times, brands and types, are successfully differentiated. The developed colorimetric sensing platform establishes a robust analytical framework for polyphenol evaluation in complex tea samples, showing great potential in the field of food quality monitoring.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 39","pages":" 7994-8004"},"PeriodicalIF":2.6,"publicationDate":"2025-09-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145147330","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":"Liquid-phase microextraction method for the separation of hexavalent and total chromium in environmental water samples with spectrophotometric detection","authors":"Zekeriyya Bahadır and Demet Tasmacıoğlu","doi":"10.1039/D5AY01075F","DOIUrl":"10.1039/D5AY01075F","url":null,"abstract":"<p >Metal pollution, particularly chromium, in water and food samples is a critical issue due to its transfer to the human body through the food chain and its threat to human health. Among the chromium species that can be found in water samples, chromates are classified as toxic by scientific authorities. Spectroscopic instruments have limitations in metal speciation analysis, and there is a need for suitable methods that allow chromium speciation. In this work, a simple microextraction method was presented to extract Cr(<small>VI</small>) into an extraction solvent after it was complexed with a cationic reagent named benzyldimethyltetradecylammonium chloride, followed by measurement using ultraviolet-visible spectrometry. Total chromium was obtained after the oxidation of Cr(<small>III</small>) to Cr(<small>VI</small>) using a sulfuric acid/potassium permanganate/potassium oxalate combination. The method allows for a calibration curve (0.015–0.35 mg L<small>⁻¹</small>) and a low detection limit (1.8 μg L<small>⁻¹</small>) for the quantification of Cr(<small>VI</small>) and total Cr in seawater and wastewater samples. The accuracy of the proposed method was evaluated by the spiking-recovery method, with recoveries in the range of 91–103% for real water samples, and a certified reference material (LGC6026) was analyzed using the method for the determination of chromium content. In this work, benzyldimethyltetradecylammonium chloride (also known as the zephiramine ion, a disinfectant and antimicrobial agent commonly used in medical treatments) is used for the first time in a microextraction method for complexing with Cr(<small>VI</small>). The combination of microextraction with ultraviolet-visible spectrometry also makes this method low-cost and easy to apply in general chemistry laboratories. In addition, the presented method provides a more convenient oxidation procedure from Cr(<small>III</small>) to Cr(<small>VI</small>) in acidic media, using potassium oxalate instead of sodium azide to remove excess potassium permanganate.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 36","pages":" 7313-7319"},"PeriodicalIF":2.6,"publicationDate":"2025-09-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144999224","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 of a smartphone-based colorimetric chemosensor for on-site detection of indium ions in environmental water samples: solution and solid-state analysis","authors":"Savikriti Saini, Selva Kumar Ramasamy and Vetriarasu Venkatesan","doi":"10.1039/D5AY01214G","DOIUrl":"10.1039/D5AY01214G","url":null,"abstract":"<p >A novel diaminomaleonitrile-based colorimetric probe, 2-amino-3-[(8-hydroxy-2-quinolinyl)methylene]amino]-2-butenedinitrile (<strong>HQ-DAMN</strong>), was successfully synthesized and extensively characterized using a range of spectroscopic techniques. The sensing ability of <strong>HQ-DAMN</strong> towards multiple cations was investigated using colorimetric analysis, paper strips, an RGB model, alginate beads, and a UV-Vis spectrophotometer method in ACN: H<small>₂</small>O (4 : 6, v/v, pH 6.5). Upon interaction with the In<small>³⁺</small> ion, the colorless solution of <strong>HQ-DAMN</strong> immediately transforms into orange, while no visible color change was observed with other metal ions. UV-Vis spectrophotometric studies revealed that <strong>HQ-DAMN</strong> exhibits a strong absorption peak at 374 nm and a weak absorption peak at 266 nm, attributed to intramolecular charge transfer (ICT) and ligand-to-ligand charge transfer (LLCT), respectively. Upon binding with the In<small>³⁺</small> ion, new peaks emerge at 472 nm, indicative of ligand-to-metal charge transfer (LMCT). The <strong>HQ-DAMN</strong>–In<small>³⁺</small> complex exhibited a 2 : 1 binding stoichiometry, with a binding constant of 7.70 × 10<small>³</small> M<small>⁻²</small>, as determined using Job's plot and Benesi–Hildebrand (B–H) plot analysis. <strong>HQ-DAMN</strong> was found to be stable in a pH range of 4.0–7.0, retaining its high selectivity in the presence of competing ions. Moreover, it achieved excellent sensitivity, with detection limits as low as 66.7 nM using spectrophotometric methods and 0.68 μM with the RGB model. The interaction between <strong>HQ-DAMN</strong> and In<small>³⁺</small> ions was thoroughly investigated using <small>¹</small>H NMR spectra, ESI mass spectrometry, and FT-IR spectroscopy, supported by theoretical computational studies. These findings affirm the potential of <strong>HQ-DAMN</strong> as a colorimetric and smartphone RGB sensor for In<small>³⁺</small> ion detection.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 39","pages":" 8042-8052"},"PeriodicalIF":2.6,"publicationDate":"2025-09-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145184288","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 modified QuEChERS method for simultaneous determination of 73 pesticides, 23 PCBs and 16 PAHs in wheat by GC-MS/MS","authors":"Mengmeng Yan, Yujie Xie, Mengjie Shi, Xingqiang Wu, Kaixuan Tong, Qiaoying Chang and Hui Chen","doi":"10.1039/D5AY00950B","DOIUrl":"10.1039/D5AY00950B","url":null,"abstract":"<p >In this study, a modified QuEChERS method for the simultaneous determination of 73 pesticides, 23 PCBs and 16 PAHs in wheat was developed by gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). The sample was first hydrated with 4 mL of ultrapure water, extracted with 10 mL of acetone–hexane (1 : 1, V:V), and then cleaned up with a mixture of 50 mg of PSA, 150 mg of C18, and 400 mg of anhydrous MgSO<small>₄</small>. Under the optimized conditions, the samples were analyzed by GC-MS/MS for quantitative analysis using the matrix-matched external standard method. As a result, 112 compounds showed good linearity in their linear ranges with correlation coefficients (<em>R</em><small>²</small>) greater than 0.995, and the limits of detection (LODs) of the method were in the range of 0.15–3 μg kg<small>⁻¹</small>, and the limits of quantification (LOQs) were between 0.5 and 10 μg kg<small>⁻¹</small>. The recoveries ranged from 71.2% to 112.1%, with relative standard deviations (RSD, <em>n</em> = 6) below 20% at the three spiked levels (LOQ, 2× LOQ, and 10× LOQ). The intra-day precision and inter-day precision were within 0.5–11.6% and 2.4–18.9%, respectively. The proposed method was applied to 40 batches of wheat samples, and neither PCBs nor PAHs were detected. Five pesticides were detected: epoxiconazole, difenoconazole, flutriafol, bifenthrin, and simazine. Among them, simazine was detected in 10 batches of samples, with concentrations ranging from 10.01 to 48.31 μg kg<small>⁻¹</small>, which exceeded the MRL prescribed by the EU. The results demonstrate that the method is characterized by simple pretreatment, rapidity, and sensitivity, and is suitable for the simultaneous determination of pesticide residues and environmental pollutants in wheat.</p>","PeriodicalId":64,"journal":{"name":"Analytical Methods","volume":" 36","pages":" 7301-7312"},"PeriodicalIF":2.6,"publicationDate":"2025-09-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144991025","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}