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乙霉威
ACS Omega · 2023 · IF 4.1

Determination of the Dissipation Dynamics and Terminal Residue of Bupirimate and Its Metabolites in Cucumber by QuEChERS-Based UPLC-MS/MS

Yue Chen,Deliang Gao,Yueming Wu,Ling Wang,Weidi Fan,Yun Gao,Wenli Wang,Li Su,Beixing Li,Wei Mu,Weili Yu

Bupirimate is widely used as a highly active systemic fungicide. However, the frequent and heavy use of bupirimate has led to pesticide residues in crops that threaten human health and food safety. At present, there is limited research on the detection of ethirimol, which is the metabolite of bupirimate. This study established an ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method to simultaneously detect bupirimate and ethirimol residues based on QuEChERS pretreatment. The average recoveries of bupirimate and ethirimol in cucumber were between 95.2 and 98.7%, respectively, with relative standard deviations (RSDs) of 0.92–5.54% at fortified levels of 0.01, 0.1, and 5 mg L–1. The established method was used to determine the residues in field trials in 12 regions of China, and the final residues of bupirimate were all less than the maximum residue limit (MRL). Since the risk quotient (RQ) of bupirimate and ethirimol in cucumber was less than 1.3%, the dietary risk assessment indicated that bupirimate and ethirimol had a low long-term dietary risk to the general population in China. This study provides effective guidance on the proper use of bupirimate in cucumber fields and a reference for establishing the MRL of bupirimate in China.

CAS / MDL: 64-18-6
研究领域: 植物保护 · 食品安全 · 分析化学
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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 · 2021 ·Vol. 413 ·期 8 ·2071-2079 · IF 4.157

A low-background fluorescent aptasensor for acetamiprid detection based on DNA three-way junction-formed G-quadruplexes and graphene oxide

Zhao Yunwei,Zhang Hui,Wang Ying,Zhao Yanfang,Li Yaowei,Han Lei,Lu Lihua

A simple fluorescence detection platform has been established for acetamiprid assay based on DNA three-way junctions (TWJs), which can triple the fluorescence signal without any other amplification. It is designed with three single-stranded DNAs (ssDNA), each of which contains one-third or two-thirds of the G-quadruplex sequence at each end. Upon the addition of acetamiprid, the conformation of the aptamer-containing double-stranded DNA (dsDNA) changes from its original conformation and releases a strand of ssDNA. This ssDNA, with the other two ssDNAs, can assemble into DNA TWJs, and the three pairs of the branched ends of the DNA TWJs are adjacent to each other, allowing them to form three units of G-quadruplexes. Hence, the fluorescence of N -methyl mesoporphyrin IX (NMM) is lighted by the nascent G-quadruplexes. Graphene oxide (GO) is then added to minimize the detection background by absorbing the free NMM and non-target-induced ssDNA. The proposed strategy can assay acetamiprid in a wide linear range of 0–500 nM with a detection limit of 5.73 nM. More importantly, this assay platform demonstrates high potential for acetamiprid assay in food control and environmental monitoring.

研究领域: 生物化学 · 环境科学 · 食品科学
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SENSORS AND ACTUATORS B-CHEMICAL · 2022 · IF 9.221

Ratiometric fluorescent detection of pesticide based on split aptamer and magnetic separation

Ying Wang,Fuyan Zhu,Li Yin,Guangxu Qu,Dik-Lung Ma,Chung-Hang Leung,Lihua Lu

Pesticide residues have seriously threatened human health and affected the sustainable development of the environment. It is pivotal to establish an efficient detection platform for pesticide assays. A novel ratiometric fluorescent aptasensor for sensitive determination of pesticide has been successfully established. Carbon dots (CDs) are used as the reference emitter, while the T-rich single-stranded DNA templated copper nanoparticles (CuNPs) provide the increasing signal. More precisely, CDs/magnetic beads (MBs) combined with split aptamer are used in this detection platform to present a label-free and enzyme-free isocarbophos (ICP) detection with high sensitivity and specificity. In the presence of ICP, a sandwich-typed complex is formed which attaches a T-rich DNA. After magnetic separation and addition of Cu 2+ /ascorbic acid (AA), the CuNPs are generated and the strong red luminescent appears. Without ICP, just blue emission from CDs exits. The developed ratiometric aptasensor offers an excellent ICP detection in the linear range of 3–200 nM with a detection limit of 0.81 nM. It provides new ways for the assay of pesticides in agricultural products or environmental samples.

研究领域: 分析化学 · 环境科学 · 纳米技术 · 生物技术
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TALANTA · 2018 · IF 4.244

Label-free and enzyme-free fluorescent isocarbophos aptasensor based on MWCNTs and G-quadruplex

Xiaotong Li,Xiaomin Tang,Xiaojie Chen,Baohan Qu,Lihua Lu

A novel label-free and enzyme-free detection strategy has been developed for the fluorescent detection of isocarbophos (ICP) using multi-walled carbon nanotubes (MWCNTs) and G-quadruplex as the signal transducers. In this work, the split ICP aptamer were attached to a G-quadruplex motif at their respective terminals. In the presence of ICP, the split aptamers could undergo conformational change into a sandwiched-like ternary complex, which prevent them from adsorbing to the MWCNTs due to the increased steric hindrance . As a result, the fluorescence signal of the G-quadruplex probes N-methyl mesoporphyrin IX (NMM) was enhanced significantly. In the absence of ICP, the split aptamer only existed in the form of single-stranded DNA, which could be easily adsorbed by MWCNTs and resulted in a quenched fluorescence signal of NMM. The proposed strategy could selectively and sensitively detect ICP with a detection limit of 10 nM. Furthermore, we have also demonstrated the capability of this strategy in the detection of ICP in real samples from vegetable extract, indicating the potential application of this strategy in food safety issues.

研究领域: 分析化学 · 食品安全 · 生物传感技术
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JOURNAL OF CHROMATOGRAPHY A · 2017 · IF 3.981

Barley husk carbon as the fiber coating for the solid-phase microextraction of twelve pesticides in vegetables prior to gas chromatography–mass spectrometric detection

Weiqian Liang,Juntao Wang,Xiaohuan Zang,Wenhuan Dong,Chun Wang,Zhi Wang

In this work, a barley husk biomaterial was successfully carbonized by hydrothermal method. The carbon had a high specific surface area and good stability. It was coated onto a stainless steel wire through sol-gel technique to prepare a solid-phase microextraction fiber for the extraction of trace levels of twelve pesticides (tsumacide, fenobucarb, indoxacarb, diethofencarb, thimet, terbufos, malathion, thiamethoxam, imidacloprid, buprofezin, acetamiprid, thiamethoxam) from vegetable samples prior to gas chromatography–mass spectrometric (GC–MS) detection. The main experimental parameters that could influence the extraction efficiency such as extraction time, extraction temperature, sample pH, sample salinity, stirring rate, desorption temperature and desorption time, were investigated. Under the optimized conditions, the linearity was observed in the range of 0.2–75.0   μg   kg −1 for tomato samples, and 0.3–60.0   μg   kg −1 for cucumber samples, with the correlation coefficients ( r ) ranging from 0.9959 to 0.9983. The limits of detection of the method were 0.01–0.05   μg   kg −1 for tomato samples, and 0.03–0.10   μg   kg −1 for cucumber samples. The recoveries of the analytes for the method from spiked samples were in the range of 76%–104%, and the precision, expressed as the relative standard deviations, was less than 12%.

研究领域: 分析化学 · 环境科学
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Food Analytical Methods · 2019 ·Vol. 13 ·期 3 ·690-698 · IF 2.413

A Graphene Oxide–Based Composite for Solid-Phase Extraction of Carbamate Pesticides from Vegetables

Gao Tian,Wang Juntao,Wu Qiuhua,Wang Chun,Wang Zhi

In this work, a graphene oxide-based composite (DABP-GO) was prepared by aminating graphene oxide (GO) with the diazonium salt of 4,4′-diaminobiphenyl (DABP). The DABP-GO composite was characterized by scanning electron microscopy, infrared spectroscopy, and nitrogen adsorption-desorption. The DABP-GO showed to be an effective solid-phase extraction (SPE) adsorbent for carbamate pesticides. A SPE method with the DABP-GO as the adsorbent combined with high-performance liquid chromatography with ultraviolet detection was established to determine trace carbamate residues in vegetable samples (benincasahispida and pakchoi). Under the optimal conditions, the linear range was from 1.0 to 40.0 ng g −1 . The limits of detection and limits of quantitation of the six carbamates (metolcarb, arprocarb, carbaryl, isoprocarb, fenobcarb, and diethofencarb) were 0.3–0.5 ng g −1 and 0.9–1.5 ng g −1 for benincasahispida sample and 0.5–1.0 ng g −1 and 1.5–3.0 ng g −1 for pakchoi sample, respectively. The relative standard deviations (RSDs) for the intra-day precision at the analyte concentration of 40 ng g −1 are from 2.3 to 8.2% ( n  = 5) and the inter-day RSDs ( n  = 5) are from 4.5 to 9.2%.

研究领域: 分析化学 · 环境科学 · 食品安全
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MICROCHIMICA ACTA · 2020 ·Vol. 187 ·期 4 ·1-11 · IF 6.232

Layered porous organic frameworks as a novel adsorbent for the solid phase extraction of chlorophenols prior to their determination by HPLC-DAD

Wang Qianqian,Li Gaigai,Wang Chun,Wu Qiuhua,Wang Zhi

A layered porous organic framework (L-POF) with high surface area and porous volume was used as a novel adsorbent for adsorption of chlorophenols (CPs). The L-POF showed much higher adsorption capacity for four CPs (2-CP, 3-CP, 2,3-CP, 2,4-CP) compared with corresponding amorphous POF and some commercial adsorbents. Then, an L-POF-based solid-phase extraction method combined with high-performance liquid chromatography for analyzing CPs at the wavelength of 280 nm in water and honey samples was established. Under the optimum conditions, four CPs exhibited good linearity in the range 0.10–80.0 ng mL −1 for water and 2–400 ng g −1 for honey samples with determination coefficient r 2  > 0.996. The method has low limits of detection of 0.03–0.10 ng mL −1 for water and 0.5–1.0 ng g −1 for honey samples. The method presented satisfactory precision and accuracy with relative standard deviations ≤ 7.8% and recoveries of 80–115%. High enrichment factors of 123–190 for water and 63–97 for honey were obtained. The validated method was successfully used to determine CPs in water and honey samples. The L-POF also displayed prominent adsorption performance for many other dyes and organic contaminants. This suggests that it can be an ideal candidate as adsorbent for wide application in separation and analysis. Graphical Abstract

研究领域: 分析化学 · 环境科学
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MICROCHIMICA ACTA · 2020 ·Vol. 187 ·期 9 ·1-10 · IF 6.232

Graphene intercalated with carbon nanosphere: a novel solid-phase extraction sorbent for five carbamate pesticides

Guo Liying,Wu Jingyu,Xing Fei,Liu Weihua,Hao Lin,Wang Chun,Wu Qiuhua,Wang Zhi

Graphene-carbon nanosphere composite (G@CNS) was prepared via a simple hydrothermal method. The G@CNS nanocomposite was characterized by X-ray diffraction, scanning electron microscope, surface area, and porosity analysis. The G@CNS was applied as a new sorbent for solid-phase extraction of five carbamate pesticides (tsumacide, carbaryl, isoprocarb, bassa, diethofencarb) prior to quantitative determination by high-performance liquid chromatography with ultraviolet detection at 208 nm. Some experimental parameters including desorption conditions, sample pH, sample volume, and loading rate were studied carefully. Under the optimized condition, the method provided good linearity ranging from 0.3 to 100.0 ng mL −1 with low limits of detection of 0.10–0.20 ng mL −1 for grape juice, 0.10–0.30 ng mL −1 for blend fruit juice, and 0.10–0.20 ng mL −1 for water sample. Good method recoveries (80.2–110%) with relative standard deviations less than 7.2% and high enrichment factors (167–293) were achieved. Results demonstrated that this novel G@CNS can serve as a promising alternative sorbent for more applications. In this work, a graphene-carbon nanosphere (G@CNS) composite was synthesized via a simple hydrothermal method. Then, the G@CNS was served as a novel sorbent for solid-phase extraction of five carbamate pesticides (tsumacide, carbaryl, isoprocarb, bassa, diethofencarb) in juice and environmental water samples, followed by their quantitative analysis with high-performance liquid chromatography-ultraviolet detection.

研究领域: 材料科学 · 分析化学 · 环境科学
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