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Analytical Methods · 2013 ·Vol. 5 ·期 21 ·6234-6239 · IF 1.855

A strip-based immunoassay for rapid determination of fenpropathrin

Xiujin Chen,Liqiang Liu,Hua Kuang,Shanshan Song,Chuanlai Xu

We report the generation of monoclonal antibodies against fenpropathrin, originating from a BALB/c mouse immunized with a conjugate of hapten 1 [(RS)-cyano-3-phenoxybenzyl-2,2,3,3-tetramethylcyclopropane-carboxylic acid)] and keyhole limpet hemocyanin and the establishment of a monoclonal antibody-based immunochromatographic test strip. A coating antigen (test band) and a goat anti-mouse antibody (control band) were separately immobilized on nitrocellulose membrane strips as capture reagents. The anti-fenpropathrin monoclonal antibody was labeled with gold nanoparticles as a detection probe. This test strip had a wide linear range (15.6–250 μg L−1) with a low detection limit of 62 ± 6 μg L−1 for fenpropathrin, evaluated using a strip reader, and could be read within 10 min. This novel test strip was used to test fenpropathrin in fortified samples and found to have a high recovery rate (>80%). In summary, our monoclonal antibody-based immunochromatographic strip offers a rapid screening tool for fenpropathrin detection in agricultural commodities.

研究领域: 免疫学 · 分析化学 · 食品安全 · 农药残留 · 分子诊断
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JOURNAL OF SEPARATION SCIENCE · 2019 ·Vol. 42 ·期 7 ·1432-1439 · IF 2.516

A hybrid triazine-imine core-shell magnetic covalent organic polymer for analysis of pesticides in fruit samples by ultra high performance liquid chromatography with tandem mass spectrometry

Ruiyu Liang,Yi Peng,Yuling Hu,Gongke Li

A novel hybrid triazine-imine core-shell magnetic covalent organic polymer with high adsorption capacity and excellent stability was fabricated by surface-assisted in situ growth technique. The composite possesses porous and extended π-conjugated system, and was applied as the magnetic sorbent for efficient enrichment and rapid separation of pesticides. A new analytical method for simultaneous determination of eight pesticides in fruit samples was developed by magnetic solid phase extraction combined with ultra high performance liquid chromatography and tandem mass spectrometry. The effect of extraction time, desorption time, and the type of desorption solvent on the extraction efficiency were evaluated. The established method shows good repeatability and high sensitivity. The repeatability of this method was estimated with relative standard deviations in the range of 0.7–7.0% ( n = 5) for the same batch, and 1.7–10% ( n = 3) for batch to batch. Good linearity for eight pesticides was obtained with coefficient of determination in the range of 0.9942–0.9990. Limit of detections ranged from 0.4 to 1.2 ng/L. Real sample determination showed that four and two pesticides were detected in strawberry and grape, respectively. The results demonstrated that the established method was efficient, sensitive, and convenient for trace determination of pesticides in fruit samples.

研究领域: 分析化学 · 环境科学 · 食品科学
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JOURNAL OF HAZARDOUS MATERIALS · 2025 · IF 11.3

Plasmonic microsphere lens arrays-integrated microfluidic SERS chip for mixed pesticides identification with machine learning

Zhenyong Dong,Feixiang Zheng,Hao Wang,Yukai Liu,Xiao Ren,Feng Lin,Song Zhou,Li Chen,Yan-qing Lu,Guanghui Wang

The use of multiple pesticides in agriculture has caused mixed residues, complicating food safety testing. Surface-enhanced Raman scattering (SERS) offers high sensitivity and fingerprinting capabilities for pesticide detection; however,its application is limited by spot size, uneven sample distribution, spectral analysis challenges in mixed samples, and the lack of integrated automated systems for sample preparation, detection, and analysis. Hence, we developed a SERS microfluidic chip integrated with plasmonic microsphere lens arrays, which integrates optical field-modulated microspheres and plasmonic nanostructures to realise the transition of SERS detection from point-hotspots to uniform area-hotspots, achieving high-sensitivity, high-stability Raman detection under wide-field laser excitation. Moreover, a comprehensive a sample-to-answer total analysis system was established with this chip as the core, incorporating the micro-QuEChERS pretreatment module for efficient extraction of pesticides in complex matrices and the random forest-dual annealing spectral parsing algorithm for mixed spectral analysis. The results indicate that the limits of detection for 2,4-dichlorophenoxyacetic acid, acetamiprid, and thiabendazole were 1.15 nM, 0.63 nM, and 0.69 nM, respectively. The linear ranges were 10⁻⁴–10⁻⁹ M, with R² values of 0.9982, 0.9989, and 0.9996, respectively. Average recoveries ranged from 90.8 % -104.66 %, 89.1 %-107.89 %, and 89.73 %-108.4 %, respectively, with relative standard deviations below 8 %. The algorithm quantified mixed pesticides with mean absolute percentage errors of 4.96 %, 5.35 %, and 7.72 %, respectively. The system showed 3 s detection response and 15-minute analysis time. Thus, the method provides a rapid, on-site solution for detecting mixed pesticides in complex matrices by exceptional optical performance and automated processing functionality.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY A · 2025 · IF 4

A Simple, Efficient, and Rapid Pipette Tip-Integrated Silanized Melamine Sponge Device for UPLC-MS/MS Analysis of Multi-Pesticide Residue in Cowpea

Xu Xu,Shiping Zhao,Ziling Zhang,Lanrui Yang,Wenhao Zhao,Baocheng Ji,Yanhong Bai

In this study, a facile and efficient pipette tip-integrated silanized melamine sponge device was developed for the rapid quantification of multi-pesticide residues in cowpea by ultra-performance liquid chromatography-tandem mass spectrometry. By embedding silanized melamine sponges within a pipette tip architecture, the device facilitates efficient matrix cleanup through simple aspiration-dispensing maneuvers, substantially simplifying sample pretreatment workflows. Comparative evaluations against conventional commercial adsorbents revealed that the proposed system exhibits comparable or enhanced purification performance. Method validation demonstrated that target analytes achieved recoveries spanning 81.0%-115.4% across three spiking concentrations, with intra- and inter-day precisions both below 15%. Additionally, excellent linearity (R²≥0.9985), negligible matrix effects (-18.3% to 19.8%), and low limits of detection (0.025-2.40 μg·kg⁻¹) and quantification (0.05-5.00 μg·kg⁻¹) were attained. These findings underscore the considerable potential of the developed purification device for pesticide multi-residue analysis in complex food matrices.

研究领域: 分析化学 · 食品安全 · 环境监测 · 农药分析
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FOOD CHEMISTRY · 2025 · IF 9.8

Singly capped cucurbit[7]uril-mediated magnetic solid phase extraction coupled with HPLC-MS/MS for the multiresidue analysis of 20 pesticides in vegetables

Huiyu He,Rui Wang,Rongbin Nie,Nan Dong

Pretreatment technology suffers from drawbacks such as tedious operation, low efficiency, and poor selectivity. Hence, we presented a singly capped cucurbit[7]uril-mediated magnetic solid phase extraction (Q[7]-MagSPE) combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for multiresidue analysis of 20 pesticides. The Q[7]-MagSPE was constructed by assembling Q[7] onto the gold magnetic nanoparticles (GoldMag) via the reaction between one of the electron-rich carbonyl portals of Q[7] and gold. The host-guest interaction activity of supramolecules, the high dispersibility and easy separability of GoldMag were integrated in the Q[7]-MagSPE. The detection limits for 20 pesticides were lower than 10.3 ng/kg, and the recoveries were 71.55 – 110. 6 % . Moreover, the reusability of the Q[7]-GoldMag and effect of washing times on the pesticide residue were evaluated to be satisfactory. Therefore, the Q[7]-MagSPE provides a rapid and robust pretreatment method for the multiresidue determination of pesticides in vegetables, which is of great significance for food safety.

CAS / MDL: 107-22-2 57-13-6
研究领域: 分析化学 · 食品安全 · 纳米技术 · 农药分析 · 超分子化学
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TALANTA · 2018 · IF 4.244

Fabrication of gold nanorods for SERS detection of thiabendazole in apple

Gendi Fu,Da-Wen Sun,Hongbin Pu,Qingyi Wei

Thiabendazole (TBZ) is a kind of pesticide that is widely used in agriculture, and its residue may pose a threat to human health. In order to measure TBZ residues in food samples, a surface-enhanced Raman spectroscopy (SERS) method combined with a homogeneous and reusable gold nanorods (GNR) array substrate was proposed. GNR with a high uniformity was synthesized and then applied to the self-assembly of a GNR vertically aligned array. The relative standard deviation (RSD) of the array for SERS could reach 15.4%, and the array could be reused for more than seven times through the treatment of plasma etching. A logarithmic correlation between TBZ concentration and Raman intensity was obtained, with the best determination coefficient (R 2 ) and the corresponding limit of detection (LOD) of 0.991 and 0.037 mg/L in methanol solution, and 0.980 and 0.06 ppm in apple samples, respectively. The recoveries of TBZ in apple samples ranged from 76% to 107%. This study provided a rapid and sensitive approach for detecting TBZ in apples based on SERS coupled with GNR array substrate, showing great potential for analyzing other trace contaminants in food matrices.

研究领域: 分析化学 · 纳米技术 · 食品安全 · 农药分析
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MICROCHIMICA ACTA · 2019 ·Vol. 186 ·期 6 ·1-10 · IF 5.479

Magnetic nanoparticles modified with hyperbranched polyamidoamine for the extraction of benzoylurea insecticides prior to their quantitation by HPLC

Liu Zikai,Lin Xiwen,Liu Xinya,Li Jing,Zhou Wenfeng,Gao Haixiang,Zhang Sanbing,Lu Runhua

A magnetic sorbent was fabricated by covalently grafting hyperbranched polyamidoamine onto the surface of Fe 3 O 4 nanoparticles. The sorbent was used in the magnetic solid-phase extraction (MSPE) of benzoylurea insecticides (BUs) from environmental water samples. It is perceived that hydrogen bonding interactions and hydrophobic interactions are the main mechanisms for the adsorption of BUs. The sorbent was characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, elemental analysis, Brunauer-Emmett-Teller measurement, X-ray photoelectron spectroscopy, vibrating sample magnetometry and X-ray diffraction. Various experimental parameters affecting the MSPE were optimized. Following elution with acetonitrile, the BUs were quantified by HPLC with diode array detection. The method based has a wide linear response range (2.5–500.0 ng mL −1 ), satisfactory coefficient of determination (0.9922–0.9976), high enrichment factors (62.8–74.4), acceptable limits of quantitation (2.5 ng mL −1 ) and low limits of detection (0.39–0.72 ng mL −1 ). The intra-day precision at concentration levels of 5.0, 50.0 and 250.0 ng mL −1 ranged from 2.3–6.4% and the inter-day precision was between 1.0 and 5.5%. The sorbent can be re-used at least 15 times. It was applied to the extraction of BUs from genuine water samples where it showed satisfactory relative recoveries (75.1–111.4%) and precision (1.0–9.1%). Schematic presentation of magnetic nanoparticles modified with hyperbranched polyamidoamine and their application for extraction of benzoylurea insecticides.

研究领域: 分析化学 · 环境科学 · 纳米技术 · 农药分析
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JOURNAL OF CHROMATOGRAPHY A · 2019 · IF 3.858

Solid phase extraction of carbamate pesticides with porous organic polymer as adsorbent followed by high performance liquid chromatography-diode array detection

Xiaolan Wang,Xufeng Meng,Qiuhua Wu,Chun Wang,Zhi Wang

A solid phase extraction (SPE) method with a porous organic polymer as adsorbent was established for the extraction of five carbamate pesticides (metolcarb, carbaryl, isoprocarb, bassa and diethofencarb) from milk, white wine and juice samples prior to high performance liquid chromatography-diode array detection. The main factors affecting the SPE were optimized, including sample volume, sample loading rate, sample solution pH, desorption conditions and cartridge reusability. Under the optimal conditions, a good linearity existed in the range from 1.0 to 320.0 ng mL −1 for milk and white wine samples and from 0.5 to 160.0 ng mL −1 for juice sample with the correlation coefficients between 0.9956 and 0.9998. The method recoveries of the carbamates were 82.0%–110.0%. The limits of detection were 0.12-0.40 ng mL -1 for milk and white wine samples, and 0.06-0.20 ng mL −1 for juice sample. The adsorption mechanism of the adsorbent was investigated by the extraction of different types of organic compounds (carbamates, benzoylurea insecticides, endocrine disrupting chemicals and polycyclic aromatic hydrocarbons) with the adsorbent. The results showed that the existence of the hydrogen-bonding between the adsorbent and the analytes is favorable for the adsorption and strong hydrophobicity seems to have an adverse effect.

研究领域: 分析化学 · 环境科学 · 食品科学 · 农药分析
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2022 ·Vol. 414 ·期 24 ·7277-7289 · IF 4.478

Homogeneous photoelectrochemical biosensor for sensitive detection of omethoate via ALP-mediated pesticide assay and Bi2S3@Bi2Sn2O7 heterojunction as photoactive material

Wang Min,Hou Li,Chen Xiaoyu,Lin Tianran

A simple homogeneous photoelectrochemical (PEC) sensing platform based on an alkaline phosphatase (ALP)–mediated pesticide assay was established for the sensitive detection of omethoate (OM). The Bi 2 S 3 @Bi 2 Sn 2 O 7 heterojunction was used as a photoactive material to provide stable background photocurrent signals. The inhibition of OM on ALP and PEC determination was carried out in the homogeneous system. In the absence of OM, dephosphorylation of L-ascorbic acid 2-phosphate trisodium salt (AAP) was catalyzed by ALP to produce the enzyme-catalyzed product (L-ascorbic acid, AA). AA, as an electron donor, could capture photogenerated holes on the Bi 2 S 3 @Bi 2 Sn 2 O 7 heterojunction, thus inhibiting the recombination of electron holes to achieve an increase of the photocurrent signal. When the OM was introduced, the enzyme activity of ALP was reduced due to the organophosphorus pesticides (OPs)–based enzyme inhibition, and the AA produced by catalytic hydrolysis was also reduced, thus reducing the photocurrent signal. Compared with the traditional PEC sensor for OPs, this homogeneous PEC sensor avoided immobilization procedures, covalent labeling, separation, and the steric hindrance effect caused by immobilized biomolecules, which achieved high recognition efficiency and caused a reduction in analysis time. Additionally, an ALP-mediated pesticide assay for the determination of OPs with a simplified experimental process further improved the stability and reproducibility of the PEC sensor. The PEC sensor showed high sensitivity to the target OM within a dynamic range of 0.05 ~ 500 ng mL −1 , and the detection limit was 0.0146 ng mL −1 . Additionally, the PEC biosensing system showed good selectivity and anti-interference ability, and exhibited a satisfactory result in spinach and mustard samples. Graphical abstract A homogeneous PEC biosensor based on ALP inhibition strategy was constructed for OM detection in vegetable samples via Bi 2 S 3 @Bi 2 Sn 2 O 7 heterojunction as the photoactive substrate material

研究领域: 分析化学 · 环境科学 · 材料科学 · 生物传感器 · 农药分析
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