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RSC Advances · 2014 ·Vol. 5 ·期 4 ·3039-3044 · IF 3.708

Quantum dots-based fluoroimmunoassay for the simultaneous detection of clothianidin and thiacloprid in environmental and agricultural samples

Ming Li,Ming Ma,Xiude Hua,Haiyan Shi,Qiuxia Wang,Minghua Wang

Quantum dots (QDs), luminescent semiconductor nanocrystals, have the potential to simplify the performance of multi-analyte analysis. In this work, a novel indirect competitive fluorescence-linked immunosorbent assay (FLISA) based on QDs for the detection of clothianidin and thiacloprid simultaneously in environmental and agricultural samples were performed in a single well of the microtiter plate. The QDs-labeled antibody conjugates, which consists of CdSe/ZnS core–shell QDs and polyclonal antibodies, were prepared through the 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (EDC) coupling method. Under optimal conditions, the half-maximal inhibition concentration (IC50) and the limit of detection (LOD, IC10) of the FLISA were 12.5 and 0.3 ng mL−1 for clothianidin, and 9.27 and 0.4 ng mL−1 for thiacloprid, respectively. The cross-reactivities of the FLISA with the analogues of clothianidin and thiacloprid were negligible except for dinotefuran (10.4% for clothianidin). The spiked recoveries were 73.3% to 113.1% with relative standard deviations (RSDs) of 2.7 to 13.3% for the detection of clothianidin and thiacloprid in river water, soil, cabbage, rice and tomato. Furthermore, the results of FLISA for the authentic samples correlated well with those obtained by HPLC. The proposed FLISA is a satisfactory tool for rapid, sensitive, and quantitative detection of two pesticides simultaneously in agricultural and environmental samples. This study provides a strategy for the development of QDs-based fluoroimmunoassay for the quantitative analysis of two pesticides.

研究领域: 环境科学 · 农业科学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2025 · IF 4

Hydrophobic deep eutectic solvent-based ferrofluid for the multi-residue analysis of pyrethroid insecticides in agricultural products: Facile pretreatment and MS-friendly detection

Yuxin Liu,Chenjie Ma,Mantang Chen,Jufang Hao,Wei Liu,Jingjing Yu

Pyrethroid insecticides (PYs) overuse poses ecological and health risks, leading to tightened restrictions on maximum residue limits (MRLs) by regulatory bodies like the European Union and China's National Food Safety Standards. It is important to develop multi-residue analytical methods for PYs residues. In present work, oleic acid-coated Fe 3 O 4 nanoparticles (Fe 3 O 4 -OA) were dispersed in hydrophobic deep eutectic solvents (HDES) to prepare ferrofluids (FFs), with the HDES synthesized from coumarin and thymol at a 1:2 molar ratio. And the HDES-FF was subsequently utilized as a vortex-assisted liquid-phase microextraction sorbent for the enrichment of 16 PYs, combined with GC–MS/MS analysis. HDES-FF could effectively enrich PYs within merely 3.5 min according to π-π stacking interactions and hydrophobic effects, while Fe 3 O 4 -OA nanoparticles were responsible for magnetic separation. It could successfully solve the problem of separation difficulty after liquid-liquid microextraction based on DES. Simultaneously, thermogravimetric analysis confirmed that the HDES could decompose at injection port of GC–MS/MS instrument, and mass spectrometry signals of the decomposed HDES could not be collected by adjusting the solvent delay time. Thus, it could effectively protect the ion source from contamination, making DES compatible with GC–MS methods. The detection limit (LOD) of the proposed method is 0.41–7.91 ng/mL, with the recoveries of 83.33–106.02 %. The intra-day and inter-day relative standard deviations (RSDs) are less than 4.20 % and 6.94 %, respectively. The method successfully detected 16 PYs in various real fruit and vegetable samples.

研究领域: 食品安全检测 · 农药残留分析 · 食品化学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2020 · IF 3.004

Simultaneous extraction and determination of 45 veterinary antibiotics in swine manure by liquid chromatography-tandem mass spectrometry

Suli Zhi,Jing Zhou,Haixue Liu,Huihui Wu,Zulin Zhang,Yongzhen Ding,Keqiang Zhang

A multiresidue method for identification and quantification of 45 veterinary antibiotics (VAs) belonging to 5 different drug classes has been developed, which is the first comprehensive method for pig manure. The proposed method used mixed liquor with methanol: acetonitrile: citrate buffer ratio of 1:1:2 to extract the target VAs from freeze-dried manure. The extracting solution passed through solid-phase extraction (SPE) procedure with Oasis HLB cartridges, which could isolate the target VAs and clean the samples in a single step. After blow-drying and concentrating, the samples were analyzed by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) in one single injection with a run time of 12 min. The average recovery rates for most of the VAs were in the range of 50–120% with relative standard deviations below 15%. Linearity was studied in the range between 2 and 1000 μg/kg using matrix-matched calibration and pure solvent calibration, to evaluate the matrix effects (MEs). The limits of detection (LDs) and quantification (LQs) were in the range of 0.01–1.54 μg/kg and 0.03–5.13 μg/kg respectively, except for penicillin G. Finally, the proposed method was used to quantify VA residues in real swine manure from three farms with different scales; tetracyclines, sulfonamides, quinolones and macrolides were the most frequently detected compounds.

CAS / MDL: 64-18-6
研究领域: 环境科学 · 分析化学
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MOLECULES · 2023 ·Vol. 28 ·期 18 ·6619 · IF 4.6

Multi-Residue Detection of Eight Glucocorticoids by Nano-Au/Fluticasone Propionate Electrochemical Immunosensor

Guozheng Zhao

Based on an indirect competitive method, a novel nano-Au/fluticasone propionate electrochemical immunosensor was successfully fabricated by combining the nanoscale effect, superior conductivity of nano-Au, stable Au−S chemical bond as well as strong interaction between glucocorticoid and the receptor, which was used to simultaneously detect eight kinds of glucocorticoids. The modified immunosensors’ electrochemical properties were explored by means of a cyclic voltammetry (CV) method and electrochemical impedance spectroscopy (EIS) measurements. Two factors (glucocorticoid receptor concentration, incubation time) were studied in order to obtain the optimal results. The immunosensor presents attractive electrochemical performance with a wide linear range (between 0.1 and 1500 ng⋅mL−1) and low detection limit (between 0.057 and 0.357 ng⋅mL−1), realizing the rapid multi-residue detection of a large class of glucocorticoids. Two glucocorticoids (hydrocortisone, triamcinolone) were detected in actual skincare samples, which obtained satisfactory detection results.

研究领域: 分析化学 · 生物医学工程 · 药物分析
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FOOD CHEMISTRY · 2018 · IF 4.946

Preparation of a chemiluminescence sensor for multi-detection of benzimidazoles in meat based on molecularly imprinted polymer

Yi Cai,Xin He,Peng Lei Cui,Jing Liu,Zhao Bin Li,Bing Jie Jia,Teng Zhang,Jian Ping Wang,Wan Zhe Yuan

In this study, a molecularly imprinted polymer capable of recognizing 8 benzimidazoles was first synthesized. The computation simulation showed that the shape and size of used template were the main factors influencing its recognition ability. Then the polymer was used as recognition reagent to prepare a chemiluminescence sensor on conventional 96-well microplate. The sample solution and a HRP-labeled hapten were added into the microplate wells to perform competitive binding, and the light signal was initiated with 4-(imidazol-1-yl)phenol enhanced luminol-H 2 O 2 system. The optimized sensor was used to determine the residues of 8 benzimidazoles in mutton and beef. Result showed that the sensor achieved ultrahigh sensitivity (limits of detection of 1.5–21 pg/mL), rapid assay process (18 min) and satisfactory recovery (65.8%–91.2%). Furthermore, this sensor could be reused for 4 times. Therefore, this sensor could be used as a rapid, simple, sensitive and durable tool for screening the residual benzimidazoles in meat.

CAS / MDL: 97-90-5
研究领域: 分析化学 · 食品科学 · 生物传感技术
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Frontiers in Chemistry · 2019 · IF 3.782

Up-Converting Nanoparticle-Based Immunochromatographic Strip for Multi-Residue Detection of Three Organophosphorus Pesticides in Food

Zou Rubing,Chang Yunyun,Zhang Tianyi,Si Fangfang,Liu Ying,Zhao Ying,Liu Yihua,Zhang Mingzhou,Yu Xiaoping,Qiao Xusheng,Zhu Guonian,Guo Yirong

Organophosphorus (OP) pesticides are widely used to control pests because of their high activity. This study described a rapid and sensitive lateral flow immunochromatographic (LFIC) assay based on up-converting nanoparticles (UCNPs) for multi-residue detection of three OP pesticides. The developed assay integrated novel fluorescent material UCNPs labeled with a broad-specific monoclonal antibody. Based on the competitive platform by immobilized antigen in the test zone, the optimized UCNPs-LFIC assay enabled sensitive detection for parathion, parathion-methyl, and fenitrothion with IC50 of 3.44, 3.98, and 12.49 ng/mL (R2 ≥ 0.9776) within 40 min. The detectable ability ranged from 0.98 to 250 ng/mL. There was no cross-reactivity with fenthion, phoxim, isocarbophos, chlorpyrifos, or triazophos, even at a high concentration of 500 ng/mL. Matrix interference from various agricultural products was also studied in food sample detection. In the spiked test, recoveries of the three OP pesticides ranged from 67 to 120% and relative standard deviations were below 19.54%. These results indicated that the proposed strip assay can be an alternative screening tool for rapid detection of the three OP pesticides in food samples.

研究领域: 农业化学 · 分析化学 · 食品科学
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Food Analytical Methods · 2022 ·Vol. 15 ·期 11 ·2994-3002 · IF 3.498

Selective Accelerated Solvent Extraction for Multi-residue Analysis of Organophosphate Esters in Cereal-Based Baby Food

Wu Huizhen,Zhou Min,Zheng Binyu,Song Ningying,Wei Dan,Lei Chao,Sun Nabo,Qian Mingrong

This paper reports an analytical method to simultaneously determine the level of organophosphate ester residues in different cereal-based baby foods. The samples were extracted with acidic acetonitrile and n-hexane, using mixed adsorbent (PSA:Florisil:alumina-B, 2:2:1, w/w/w) for clean-up during the extraction procedure. This method combines sample extraction and purification into one step, reducing preparation time. The target analytes were confirmed and quantified with ultra-high-performance liquid chromatography–tandem mass spectrometry. The limits of quantitation were 0.04–0.75 ng g −1 and the recovery rate was 73.2–107.0%. The proposed method was applied for the analysis of real samples obtained from domestic markets in China. It provides a new approach to detection of pollutants in complex food samples. Graphical abstract

研究领域: 食品科学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2021 · IF 4.759

Development of a modified quick, easy, cheap, effective, rugged, and safe method based on melamine sponge for multi-residue analysis of veterinary drugs in milks by ultra-performance liquid chromatography tandem mass spectrometry

Baocheng Ji,Wenhao Zhao,Xu Xu,Yu Han,Mingsha Jie,Gaigai Xu,Yanhong Bai

The purpose of this study was to develop a modified QuEChERS method based on melamine sponge for rapid determination of multi-class veterinary drugs in milks by UPLC-MS/MS. Through simple infiltration and extrusion, fast and convenient matrix purification could be achieved within several seconds, and there was no need of extra phase separation operations. Good linearity with correlation coefficient (R 2 ) ≥0.999 was obtained for all drugs in the range of 2~500 µg·kg −1 . The obtained matrix effects were within ±20% for all monitored drugs. The recoveries of all monitored drugs ranged from 60.7% to 116.0% at three spiked levels (50, 100, and 200 µg·kg −1 ), with relative standard deviations less than 7.4%. Comparatively low LODs and LOQs were obtained in the ranges of 0.1~3.8 µg·kg −1 and 0.2~6.3 µg·kg −1 , respectively. Compared with conventional purification adsorbents, melamine sponge yielded an equal or higher purification performance with matrix removal rate as high as 52.5% and acceptable recoveries in range of 60%-120% for all monitored drugs. The satisfactory results have demonstrated the good potential of melamine sponge in matrix purification for rapid determination of multiclass residues in food safety.

研究领域: 分析化学 · 食品安全 · 兽医学
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JOURNAL OF RAMAN SPECTROSCOPY · 2023 ·Vol. 54 ·期 5 ·468-476 · IF 2.5

Rapid detection and whole class control of quinolone antibiotics in pork based on surface-enhanced Raman spectroscopy

Xiao-Bing Zheng,Sheng-Hong Liu,Bao-Ying Wen,Wei Peng,Hong-Mei Li,Murugavel Kathiresan,Yue-Jiao Zhang,Shang-Zhong Jin,Jian-Feng Li

The problem of excessive quinolone antibiotic residues in pork has stimulated great attention from the international community. However, due to the diversity and structural similarity of quinolone antibiotics, it is difficult to perform multi-residue rapid detection at the same time. Currently, antibiotic multi-residue detection methods include ultra-performance liquid chromatography (UPLC) and colloidal gold immunochromatography. However, it cannot be widely used in on-site rapid detection due to its shortcomings such as the need for high cost and low sensitivity. Herein, we report the use of surface-enhanced Raman spectroscopy (SERS) technology for the study of similar structures of quinolone antibiotics. A method for whole class control and rapid quantitative detection of all quinolone antibiotics in pork was established. By using the above method, the detection limit of single standard quinolone antibiotics was 10 μg L −1 , and the detection limit of the mixed standard was 1 μg L −1 , meeting the international requirements for the detection limit of quinolone antibiotics in pork. At last, by adding a variety of quinolone antibiotics to pork, the real detection set-up was simulated. The recovery of standard addition was 86.6%–95.3%, and the whole class control method has been well applied, which is of great significance for the detection of pork quinolone antibiotics. Compared with colloidal gold immunochromatography, our method has 2.5 times the detection speed, 1/60 times the cost, and can be quantitatively detected. The method is simple, economical, and efficient and has great application value with broad application prospects in the field of rapid detection of pork antibiotics in the future.

研究领域: 食品安全 · 分析化学 · 光谱学
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Frontiers in Chemistry · 2020 · IF 3.693

Functional Up-Conversion Nanoparticle-Based Immunochromatography Assay for Simultaneous and Sensitive Detection of Residues of Four Tetracycline Antibiotics in Milk

Xu Ying,Ma Biao,Chen Erjing,Yu Xiaoping,Sun Chuanxin,Zhang Mingzhou

An ultrahigh-sensitivity lateral flow immunochromatography (LFIC) assay based on up-converting nanoparticles (UCNPs) was developed to carry out a multi-residue detection of tetracycline in milk. The sensitivity of the immunoassay was greatly improved by the use of a broad-spectrum monoclonal antibody attached to UCNPs to form a signal probe. Under the optimal conditions, the UCNP-LFIC assay enabled sensitive detection of tetracycline (TC) as well as of oxytetracycline (OTC), chlortetracycline (CTC), and doxycycline (DOX) within 10 min, with IC50 values of 0.32, 0.32, 0.26, 0.22 ng/mL, respectively. There was no cross-reactivity with ten other antibiotics. Similarly, we evaluated the experimental results for matrix effects. Experiments involving spiking showed the four tetracycline antibiotics displaying mean recoveries ranging from 93.95 to 111.90% with relative standard deviations (RSDs) of < 9.95%. The detection results of actual samples using the developed method showed a good correlation (R2 ≥ 0.98) with the results using high-performance liquid chromatography (HPLC). Thus, the assay can achieve an ultrahighly sensitive detection of antibiotics in milk, and can hence promote human health and provides promising applications in the bio-detection field.

CAS / MDL: 9005-64-5
研究领域: 分析化学 · 食品安全 · 生物技术 · 兽医学
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FOOD CHEMISTRY · 2021 · IF 7.514

Detection of organophosphorus pesticides by nanogold/mercaptomethamidophos multi-residue electrochemical biosensor

Guozheng Zhao,Binhua Zhou,Xiuwen Wang,Jian Shen,Bo Zhao

Based on the successful synthesis of mercaptomethamidophos as a substrate, a novel nanogold/mercaptomethamidophos multi-residue electrochemical biosensor was designed and fabricated by combining nanoscale effect, strong Au–S bonds as well as interaction between acetylcholinesterase (AChE) and mercaptomethamidophos, which can simultaneously detect 11 kinds of organophosphorus pesticides (OPPs) and total amount of OPPs using indirect competitive method. Electrochemical behavior of the modified electrode was characterized by differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS). The AChE concentration and incubation time were optimized at 37.4 °C to achieve the best detection effect. This biosensor exhibits excellent electrochemical properties with a wider linear range of 0.1 ~ 1500 ng·mL −1 , lower detection limit of 0.019 ~ 0.077 ng·mL −1 , better stability and repeatability, which realizes the rapid detection of total amount of OPPs, and can simultaneously detect a large class of OPPs rather than one kind of OPP. Two OPPs (trichlorfon, dichlorvos) were detected in actual samples of apple and cabbage and achieved satisfactory test results.

研究领域: 分析化学 · 环境科学 · 农业科学
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Analytical Methods · 2015 ·Vol. 8 ·期 3 ·666-672 · IF 1.821

Simultaneous determination of seven insecticides in soft drinks and fruit juices using ultraperformance liquid chromatography tandem mass spectrometry with product ion confirmation scan mode

L. Chen,Y. Qin,X. Yang,C. Liu

An analytical method for the simultaneous determination of seven insecticides, including six neonicotinoids and one pyridine-azomethine, in drinks by LC-MS/MS using the Product Ion Confirmation Scan (PICS) mode was developed and validated. The compounds were extracted by modified QuEChERS and purified by d-SPE. The separation of all compounds was achieved in less than 3 minutes using a BEH C18 reverse-phase column and a mobile phase composed of 0.01% formic acid in water and methanol in the gradient elution mode at 0.4 mL min−1. Except for the two transitions and retention time demanded by EU/2002, identification was further carried out by matching the mass spectrum between the reference and sample produced by PICS if necessary. The LODs and LOQs for all compounds were lower than 0.014 μg L−1 and 0.05 μg L−1, respectively. The calibration curves were ranging from the LOQ to 0.02 mg L−1 with r2 higher than 0.9917 and reasonable recoveries were between 81.19% and 105.79% with RSD <15.0%. This work illustrates the advantages of using the PICS mode to build MRM acquisition methods in the application field of pesticide multi-residue analysis. It is very effective when only one MRM transition is obtained or the confirmation ion transition is too weak. It is proved that this is a rapid and reliable analytical method.

CAS / MDL: 64-19-7 64-18-6
研究领域: 食品科学 · 分析化学
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