Haiyue Yuan, Jiafu Wang, Jiqiang Fu, Jishi Wang, Yanwei Zhang, Yue Geng, Bei Li, Zeying He
{"title":"Determination of 523 Pesticide and Metabolite Residues in Vegetables Using Ultra-high-Performance Liquid Chromatography and Gas Chromatography Coupled to Tandem Mass Spectrometry: Method Development and Application in Monitoring Survey and Exposure Risk Assessment","authors":"Haiyue Yuan, Jiafu Wang, Jiqiang Fu, Jishi Wang, Yanwei Zhang, Yue Geng, Bei Li, Zeying He","doi":"10.1007/s12161-025-02793-z","DOIUrl":"10.1007/s12161-025-02793-z","url":null,"abstract":"<div><p>A multiresidue method for simultaneously detecting 523 pesticides and metabolites in vegetables using ultra-high-performance liquid chromatography and gas chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS and GC–MS/MS) was developed and rigorously validated for accuracy, precision, linearity, quantification limits, and matrix effects. The validated method was applied to analyze 300 vegetable samples from Shandong province, China, collected in 2023. Results showed the detection of 94 pesticides overall, with a detection rate of 31.67% and a 4.00% exceedance rate of maximum residue limits. Leafy vegetables exhibited the highest detection rate, and insecticides were commonly used in vegetable production. Thiamethoxam was the most frequently detected pesticide. Some banned and restricted pesticides were found at low levels. Celery, Chinese cabbage, tomato, cucumber, eggplant, sweet pepper, and spinach showed the highest frequency of multiple residues. In several rare cases, potential risks to adults and children were identified, highlighting the need for continuous monitoring of pesticide residues to ensure consumer safety.</p></div>","PeriodicalId":561,"journal":{"name":"Food Analytical Methods","volume":"18 7","pages":"1243 - 1254"},"PeriodicalIF":3.0,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145170808","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A Novel UPLC Method Development for Quantifying Active and Inactive Ingredients in a Commercial Energy Drink Product Using Chemometric Optimization Methodology","authors":"Nazangül Ünal, Erdal Dinç","doi":"10.1007/s12161-025-02782-2","DOIUrl":"10.1007/s12161-025-02782-2","url":null,"abstract":"<div><p>The content or matrix of commercial energy drinks, which are increasingly consumed, has been changed over time to enhance the products’ competitiveness and effectiveness. This necessitates the development of new analytical methods for quality control and routine analysis. In this regard, a novel ultra-performance liquid chromatography with photodiode array detection (UPLC-PDA) method was developed using a chemometric design and optimization methodology. The method is designed to effectively separate and quantify caffeine (CAF), the active ingredient, and potassium sorbate (PS), the inactive ingredient, in a commercial energy drink with short runtime and high resolution. A 3<sup>3</sup>-full factorial experimental design was employed, considering key factors such as column temperature (X<sub>1</sub>), phosphate buffer percentage (X<sub>2</sub>), and mobile phase flow rate (X<sub>2</sub>). The chromatograms of the 27 samples containing CAF and PS in the design matrix were recorded using a Waters Acquity® BEH C<sub>18</sub> column (100 mm × 2.1 mm i.d., 1.7 µm) with the detection at 284 nm. The ICRF values were computed from the recorded chromatograms. A quadratic second-order model was established between the design matrix (independent variables) and ICRF (dependent variable). From the model, optimal experimental conditions were identified. The optimal chromatographic conditions were found to be a column temperature of 58.9 °C, a flow rate of 0.24 mL/min, and a phosphate buffer system percentage of 59.3% (v/v) + methanol of 40.7% (v/v) with 0.4 mL triethylamine (TEA)/L, achieving the best separation and shortest analysis time. Calibration curves for CAF and PS were established within the concentration ranges of 2.0–26.0 µg/mL and 4.0–28.0 µg/mL, respectively. Excellent linearity was observed, with high determination coefficients (<i>r</i><sup>2</sup> = 0.9996 for CAF and <i>r</i><sup>2</sup> = 0.9994 for PS). The limit of detection (LOD) and limit of quantification (LOQ) were determined as 0.18 µg/mL and 0.59 µg/mL for CAF and 0.20 µg/mL and 0.65 µg/mL for PS, respectively. The elution times were 1.29 min for CAF and 2.81 min for PS, with a total analysis runtime of 4.0 min. The results revealed that this method could serve as a new, cost-effective alternative for the quality control and routine analysis of samples containing CAF and PS. The method was validated through analysis of independent test samples, standard addition samples, and intra-day and inter-day samples, for example yielding satisfactory accuracy (percent mean recovery; 100.7 for CAF and 100.5 for PS) and precision (RSD %; 1.48 for CAF and 2.02 for PS) in applying the newly developed UPLC procedure. The ICH Q2(R1) guideline was followed for method validation to ensure compliance with international standards. This newly developed UPLC method was successfully implemented to analyze the active and inactive ingredients in a commercial energy drink product with a short runtime an","PeriodicalId":561,"journal":{"name":"Food Analytical Methods","volume":"18 7","pages":"1255 - 1268"},"PeriodicalIF":3.0,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s12161-025-02782-2.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145170809","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Highly Sensitive Cellulose Gauze Patch for the Detection of Morpholine Coating on Fruits","authors":"Balachandar Sundarrajan, Lokitha Paduvetnaya, Anusha Prabhu, Basavaraj Shettar, Harishkumar Madhyastha, Naresh Kumar Mani","doi":"10.1007/s12161-025-02791-1","DOIUrl":"10.1007/s12161-025-02791-1","url":null,"abstract":"<div><p>Morpholine, one of the chemicals that is used to achieve glazed waxy surface over fruits such as apple, possesses fungicidal properties, is pest-repellent and regulates humidity around the fruit. Despite having these advantages, it is proven to be a carcinogenic adulterant and extremely fatal for the human body, if consumed in excess above the safe dose of 0.48 µg/mL. Though the conventional methods of detecting morpholine are accurate, they are expensive, laborious, time-consuming, and require technical expertise. Hence, there is a demand for a simple, portable, and rapid device for on-site sensing of morpholine. In this present investigation, we have developed cellulose gauze patch for detecting morpholine coating on apple within 5 min by utilizing two different approaches, qualitative Simon’s based and quantitative pH-based colorimetric tests. The qualitative response is inferred by the colour change from brown to navy blue upon rubbing the cellulose gauze patch over the apple surface. The quantitative signal is deduced from the colour change from yellow to pink. In addition, there is a proportionate increase in the G-channel intensity of the pink colour obtained through the phenol red-based pH test, owing to the basic nature of morpholine and the increase in the pH value with the increase in its concentration, with a limit of detection (LOD) of 10 µg/mL.\u0000</p></div>","PeriodicalId":561,"journal":{"name":"Food Analytical Methods","volume":"18 7","pages":"1269 - 1280"},"PeriodicalIF":3.0,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s12161-025-02791-1.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145170801","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Construction and Performance of Nano Dual-Signal Composite Detection System for Foodborne Pathogen Detection in Meat","authors":"Yuhan Gao, Hang Ji","doi":"10.1007/s12161-025-02780-4","DOIUrl":"10.1007/s12161-025-02780-4","url":null,"abstract":"<div><p>Food safety concerns everyone, and <i>Staphylococcus aureus</i> is a common foodborne pathogen with a complex and slow detection process. To improve the detection speed and accuracy of pathogenic bacteria in fresh meat products, a dual-signal composite rapid detection system consisting of upconversion fluorescence detection and magnetic nano detection is developed. When the ratio of upconversion nanomaterials to magnetic conversion nanomaterials was 10:9, the processing time of the detection system was 20 min. When the stabilizer was added to the detection system, the detection accuracy reached more than 90%. The designed method took the shortest detection time, taking only 1 day to complete, while the traditional plate counting method took 5 days and the nano rapid detection method took 2 days. When the detection system designed for the study detects <i>Staphylococcus aureus</i>, the detection accuracy was similar to that of the traditional plate counting, with a relative standard deviation of less than 10% and could be reduced to around 3%. In this paper, a rapid detection system for dual-signal composite is developed based on upconversion fluorescence and magnetic nanomaterials. When the concentration was 1 × 10<sup>3</sup>, the detection concentration, recovery rate, and detection time of the designed method were 0.95 ± 0.02 × 10<sup>3</sup> CFU/mL, 95%, and 1 day, respectively. However, under the same conditions, the nano rapid detection method had a detection concentration, recovery rate, and detection time of 0.91 ± 0.04 × 10<sup>3</sup> CFU/mL, 91%, and 2 days, respectively. The designed method is superior to existing methods on detection concentration, recovery rate, and detection time. The <i>Staphylococcus aureus</i> detection system effectively accelerates the detection speed of fresh meat products while ensuring detection accuracy.</p></div>","PeriodicalId":561,"journal":{"name":"Food Analytical Methods","volume":"18 7","pages":"1228 - 1242"},"PeriodicalIF":3.0,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145170802","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Phytochemical Characterization of Pueraria tuberosa Root Extracts Using Microwave and Ultrasound-Assisted Extraction by LC-QTOF-MS","authors":"Poonam Patil, Pradyuman Kumar","doi":"10.1007/s12161-025-02784-0","DOIUrl":"10.1007/s12161-025-02784-0","url":null,"abstract":"<div><p>The increasing global demand for natural drugs, especially traditional medicines, has driven interest in plants like Kudzu (<i>Pueraria tuberosa</i>), renowned for its anti-inflammatory, antioxidant, antidiabetic, and anti-cancer properties. This study investigates the extraction and characterization of phytochemicals from Kudzu root, which is traditionally used in Ayurvedic and Chinese medicine. Extraction techniques, including microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE), and a combined approach (MAE + UAE), were optimized to enhance the yield of isoflavones and other phytochemicals. The high TPC (49.88 ± 0.22 mg GAE/g) and TFC (36.36 ± 0.54 mg QE/g) values are observed in the optimized sample (MAE + UAE) under extraction conditions of 100 W microwave power for 6 min with 400 W ultrasonic power for 40 min at 50 ℃. The combined MAE + UAE treatment significantly improved antioxidant activity, exhibiting the highest DPPH (76.44 ± 0.86%) and ABTS (90.76 ± 0.59%) scavenging rates with IC<sub>50</sub> value of 392.00 ± 0.39 μg/ml and 263.98 ± 0.53 μg/ml, as well as the higher FRAP value (22.77 ± 0.66 mg AAE/g). Phytochemical analysis through LC-QTOF-MS identified around 60 phytochemicals, including 10 glycosylated flavonoids, 24 isoflavonoids, five flavones and flavanols, five phenolic acids, some polyphenols, and other compounds. This study highlights the efficacy of the combined MAE + UAE method in enhancing phytochemical extraction. Furthermore, the extracts demonstrated improved functional and antioxidant activities, making them valuable for applications in functional foods and nutraceutical formulations.</p></div>","PeriodicalId":561,"journal":{"name":"Food Analytical Methods","volume":"18 7","pages":"1213 - 1227"},"PeriodicalIF":3.0,"publicationDate":"2025-03-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145170151","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Assessing Matrix Effects in LC–MS/MS Analysis of Pesticides in Food Using Diluted QuEChERS Extracts","authors":"Abderrahim Eddahby, Abdelkarim Chahine, Lahcen Hssaini","doi":"10.1007/s12161-025-02786-y","DOIUrl":"10.1007/s12161-025-02786-y","url":null,"abstract":"<div><p>Matrix effects (MEs) in liquid chromatography-tandem mass spectrometry (LC–MS/MS) analysis of pesticide residues pose significant challenges due to signal suppression or enhancement caused by co-extracted matrix components. This study evaluates the efficacy of a 10-fold dilution strategy to mitigate MEs for 90 pesticides across 10 food matrices (tomato, bean, zucchini, potato, dates, carrot, cucumber, fennel, mint, apple). Extracts were prepared using a modified QuEChERS protocol, diluted, and analyzed via UPLC-ESI–MS/MS. MEs were quantified by comparing slopes of matrix-matched and solvent-based calibration curves. Results demonstrated that dilution significantly reduced MEs in most matrices: 97% of pesticides in tomato, 92% in zucchini, and 93% in potato exhibited acceptable ME values (± 20%). However, efficacy varied with matrix composition and pesticide properties. Hydrophilic pesticides (e.g., acephate, logP = − 0.85) showed suppression in carbohydrate-rich matrices (e.g., dates, − 14% ME), while lipophilic compounds (e.g., chlorpyrifos, logP = 4.7) displayed enhancement in lipid-dense matrices (e.g., apple, + 48.4% ME). Persistent MEs occurred in 25–27% of cases, such as fenamidone in carrot (− 15% ME) and fenpropathrin in fennel (+ 63% ME), necessitating matrix- and analyte-specific interventions. While dilution proved effective for more than 90% of cases, outliers necessitate advanced methods like isotope-labeled standards. This work validates dilution as a cost-effective strategy for routine pesticide analysis, balancing sensitivity with regulatory compliance in food.</p></div>","PeriodicalId":561,"journal":{"name":"Food Analytical Methods","volume":"18 7","pages":"1203 - 1212"},"PeriodicalIF":3.0,"publicationDate":"2025-03-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145170152","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Marjan Bazdar, Mohammad Baghery, Negin Hosseinzadeh, Vahideh Sarabi-Aghdam
{"title":"Optimization Extraction Conditions of Bioactive Compounds of Carum copticum L. Seed by Microwave Using Response Surface Methodology (RSM)","authors":"Marjan Bazdar, Mohammad Baghery, Negin Hosseinzadeh, Vahideh Sarabi-Aghdam","doi":"10.1007/s12161-025-02787-x","DOIUrl":"10.1007/s12161-025-02787-x","url":null,"abstract":"<div><p>In this study, a microwave-assisted extraction technique was utilized to extract the bioactive compounds of <i>Carum copticum</i> L. seeds. Following this extraction, response surface methodology was employed to optimize the levels of total phenolic compounds, flavonoids, and DPPH radical scavenging activity. The effect of ethanol content (0–100% v/v) and time (60–120 s) on total phenolic compounds, flavonoids, and 2,2-diphenyl-1-picrylhydrazyl (DPPH) were investigated and optimized using response surface methodology. The time range of 60 to 65 s and an ethanol concentration of 80 to 100% resulted in the highest total phenolic content. Increasing the extraction time to 60 s while reducing the ethanol concentration to 0% (100% water) significantly increased the flavonoid levels. In terms of DPPH radical scavenging activity, extending the extraction time beyond 60 s and decreasing the ethanol content to less than 95% led to an increase in IC<sub>50</sub>, thereby reducing the maximum radical scavenging activity. The optimized conditions for achieving the highest DPPH radical scavenging activity of <i>Carum copticum</i> L. seed extract, in terms of time and ethanol concentration, were determined to be 60 s and 10% ethanol (90% water), respectively. In conclusion, the optimal extraction conditions for maximizing total phenolic and flavonoid content, minimizing IC<sub>50</sub>, and achieving the highest antioxidant properties in ethanol were found to be 4.04% v/v ethanol and 60 s. Our results demonstrate the effectiveness of response surface methodology (RSM) for optimizing the extraction conditions of bioactive compounds from <i>Carum copticum</i> L. seeds and suggest its potential use as bioactive functional materials.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":561,"journal":{"name":"Food Analytical Methods","volume":"18 6","pages":"1189 - 1202"},"PeriodicalIF":3.0,"publicationDate":"2025-03-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145169047","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yan Qi, Fengyang Wang, Yanjun Jiang, Lei Ji, Xiaohui Xiong, Yuanjian Liu
{"title":"A Bipolar Electrode-Electrochemiluminescence Sensor for Sensitive Detection of Escherichia coli O157:H7 Based on Loop-Mediated Isothermal Amplification","authors":"Yan Qi, Fengyang Wang, Yanjun Jiang, Lei Ji, Xiaohui Xiong, Yuanjian Liu","doi":"10.1007/s12161-025-02795-x","DOIUrl":"10.1007/s12161-025-02795-x","url":null,"abstract":"<div><p><i>Escherichia coli</i> O157:H7 (<i>E. coli</i> O157:H7) is a foodborne pathogen with high pathogenicity and lethality, capable of producing substantial amounts of Vero toxin (VT), posing a significant threat to human health. Consequently, a platform based on the bipolar electrode-electrochemiluminescence (BPE-ECL) and loop-mediated isothermal amplification (LAMP) was constructed for the detection of <i>E. coli</i> O157:H7. Firstly, LAMP technology is utilized to efficiently obtain the amplified product (double-stranded DNA, dsDNA) of <i>E. coli</i> O157:H7. On the one hand, SYBR Green was added to the amplified product to detect <i>E. coli</i> O157:H7 by colorimetric determination. The concentration of 10 CFU mL<sup>−1</sup> <i>E. coli</i> O157:H7 can only obtain qualitative analysis, to determine the presence of the target bacteria. On the other hand, methylene blue (MB) molecules were embedded in the dsDNA through electrostatic interactions. Then, by dropwise adding the mixture onto the cathode of the BPE, the ECL signal of Ru(bpy)<sub>3</sub><sup>2+</sup> onto the anode was generated. Specifically, the BPE-ECL sensor displayed superior sensitivity for <i>E. coli</i> O157:H7 with a detection limit of 10 CFU mL<sup>−1</sup> and a wide linear concentration range of 10<sup>1</sup>–10<sup>6</sup> CFU mL<sup>−1</sup>. In summary, this sensor can effectively enhance the sensitivity and reliability of detection when compared to traditional colorimetric methods, and achieve qualitative and quantitative detection of <i>E. coli</i> O157:H7 by measuring the anode ECL signal of Ru(bpy)<sub>3</sub><sup>2+</sup>.</p></div>","PeriodicalId":561,"journal":{"name":"Food Analytical Methods","volume":"18 6","pages":"1180 - 1188"},"PeriodicalIF":3.0,"publicationDate":"2025-03-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145169046","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Katrin Reichenberger, Sabine Lutz-Wahl, Lucas Kettner, Lutz Fischer
{"title":"An Extremely Sensitive Amylase Activity Assay and its Application for the Determination of the Residual Amylase Activity in Bread","authors":"Katrin Reichenberger, Sabine Lutz-Wahl, Lucas Kettner, Lutz Fischer","doi":"10.1007/s12161-025-02781-3","DOIUrl":"10.1007/s12161-025-02781-3","url":null,"abstract":"<div><p>An extremely sensitive amylase activity assay was developed using the natural substrate starch and two ancillary enzymes: a glucose oxidase (GOD) and a peroxidase, to measure the residual activity of the <i>α</i>-amylase from <i>Bacillus subtilis</i> in white bread. Firstly, the concentrations of the assay components: electron acceptor DA-67 (50 μM), horseradish peroxidase (681 nkat mL<sup>−1</sup>), a GOD from <i>Aspergillus niger</i> (1550 nkat mL<sup>−1</sup>) and the natural substrate starch (0.01% (w/v)), were optimized to achieve high sensitivity. The linearity of the assay was then tested with both an endo- (<i>α</i>-amylase from <i>B. subtilis</i>) and exo-acting amylase (maltogenic amylase from <i>Geobacillus stearothermophilus</i>), and the effect of the incubation time on the assay sensitivity was investigated and optimized. The optimized assay was capable of determining a minimal amylase activity of 0.33 pkat mL<sup>−1</sup> for both amylases tested with an assay run time of 7.5 h. This new DA-67 amylase assay demonstrated 4.7- and 4.2-times higher sensitivity, respectively, compared to optimized versions of the commercial Ceralpha (determination of endo-amylase activities) and Betamyl3 (determination of exo-amylase activities) assays. The new DA-67 amylase assay was used to determine the residual activity of <i>α</i>-amylase from <i>B. subtilis</i> in white bread. A consistent residual activity of 2.26 ± 0.15% was reliably determined. </p></div>","PeriodicalId":561,"journal":{"name":"Food Analytical Methods","volume":"18 6","pages":"1149 - 1161"},"PeriodicalIF":3.0,"publicationDate":"2025-03-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s12161-025-02781-3.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145168382","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pâmela Caires de Oliveira, Liriana Mara Roveda, Lucimara Ramires Pereira Ruis, Paula Mantovani dos Santos, César Ricardo Teixeira Tarley, Adriana Evaristo de Carvalho, Daiane Roman, Marcela Zanetti Corazza
{"title":"Modified Magnetic Nanocomposites with 2-Aminobenzothiazole as a Selective Adsorbent for Dispersive Magnetic Micro-solid Phase Extraction of Ultra-trace Amounts of Cadmium in Environmental and Food Samples by Thermospray Flame Furnace Atomic Absorption Spectrometry","authors":"Pâmela Caires de Oliveira, Liriana Mara Roveda, Lucimara Ramires Pereira Ruis, Paula Mantovani dos Santos, César Ricardo Teixeira Tarley, Adriana Evaristo de Carvalho, Daiane Roman, Marcela Zanetti Corazza","doi":"10.1007/s12161-025-02790-2","DOIUrl":"10.1007/s12161-025-02790-2","url":null,"abstract":"<div><p>This study reports for the first time the synthesis and analytical performance of two novel magnetic nanocomposites-based silica-coated and carbon nanotubes thiol (2-aminobenzothiazole – ABT) functionalized as adsorbents for preconcentration of cadmium ions in water, cigarette and food samples by dispersive magnetic micro-solid phase extraction <i>(DM-µ-SPE)</i> and determination by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS). The synthesized materials were characterized by Fourier infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), nitrogen adsorption–desorption, and thermogravimetric analysis (TGA). The pH was investigated univariately while other parameters that influence the <i>DM-µ-SPE</i> were investigated using a two-level (2<sup>4</sup>) full factorial design. As optimized conditions, pH 7.0 and 6.0; 20 mg of nanoparticles; HNO<sub>3</sub> 1.5 M as eluent and 2 min and 8 min as elution time, were found to m-SiO<sub>2</sub>-ABT and MMWCNT-ABT, respectively. The method also showed good linearity in the range of 1.0 to 10.0 µg L<sup>−1</sup> (r<sup>2</sup> ≥ 0.99) and of 2.0 to 20.0 µg L<sup>−1</sup> (r<sup>2</sup> ≥ 0.99), and low limits of detection (0.02 and 0.11 µg L<sup>−1</sup>) to m-SiO<sub>2</sub>-ABT and MMWCNT-ABT, respectively. The nanocomposites, m-SiO<sub>2</sub>-ABT and MMWCNT-ABT, can be regenerated without significant adsorption capacity loss for ten cycles, yielding recovery percentages of analytical signal of 93.04% and of 103.2%, respectively. The analysis of different water samples (tap water and mineral water), tobacco, green tea, and rice was carried out without matrix interference, yielding recovery values ranging from 88 to 104%.\u0000</p></div>","PeriodicalId":561,"journal":{"name":"Food Analytical Methods","volume":"18 6","pages":"1162 - 1179"},"PeriodicalIF":3.0,"publicationDate":"2025-03-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145168735","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}