JOURNAL OF SEPARATION SCIENCE
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2018
·Vol. 41
·期 22
·4096-4104
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IF 2.415
Nadeem Muhammad,Yun Zhang,Weixia Li,Yong-Gang Zhao,Amjad Ali,Qamar Subhani,Tariq Mahmud,Junwei Liu,Hairong Cui,Yan Zhu
A simple, cost-effective, sensitive, and quick method for the determination of nitenpyram and its metabolite 6-chloronicotinic acid in environmental samples was developed by coupling an ion chromatograph with a fluorescence detector and a post-column photochemical reactor. This developed analytical method involved a rapid sample extraction by modified and miniaturized quick, easy, cheap, effective, rugged, and safe method followed by isocratic ion chromatographic separation of nitenpyram and 6-chloronicotinic acid into an IonPac ™ AS11-HC column protected by IonPac ™ AG11A guard column by running 30 mM NaOH + 10% acetonitrile mobile phase. A homemade post-column photochemical reactor was also integrated with the ion chromatographic system for online transformation of both analytes into their respective highly fluorescent photoproduct in basic media without using an extra pump. The developed method was validated by following SANTE/11945/2015 guidelines on analytical quality control and validation procedures. The method showed a good linear response (r > 0.999), improved limit of detection (0.101–0.132 μg/L), minimum or no matrix effect, excellent recoveries (90.2–100.10%) and relative standard deviations were found to be ≤6.50%.
研究领域:
分析化学
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环境科学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
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2020
·Vol. 43
·期 20
·3921-3930
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IF 2.878
Qamar Subhani,Nadeem Muhammad,Zhouman Huang,Muhammad Asif ,Irshad Hussain,Muhammad Zahid,Cui Hairong,Yan Zhu,Dandan Guo
This study aims to introduce a simple, sensitive, and cost-effective method for the simultaneous determination of acetamiprid and its main metabolite 6-chloronicotinic acid in environmental samples by using a nonsuppressed ion chromatography hyphenated with an online postcolumn photoinduced fluorescence detection system. The fluorescence detector wavelengths λ ex /λ em = 257/382 nm was set for up to 6.0 min for acetamiprid, while λ ex /λ em = 231/370 nm programmed for 6-chloronicotinic acid for the rest of the analysis time. Both samples were treated by applying miniaturized quick, easy, cheap, effective, rugged, and safe method before the separation of analytes on an IonPac ® AS11-HC column by pumping 40 mM NaOH having minuscule content of acetonitrile (5%, v/v) as an eluent. Both intrinsically nonfluorescent analytes were turned-on by online postcolumn photoinduced derivatization, avoiding the need for complex chemical derivatization or addition of a postcolumn extra pump. The developed method was appraised for the analysis of environmental samples, exhibiting excellent linearity (0.050-10 μg/mL) with a correlation coefficient greater than 0.9993 for both analytes. Whereas, obtained limit of detection (0.025-0.0072 μg/mL), recoveries (98.02-116.00%), and inter- and intraday precision (≤3.02 %) were satisfactory for both compounds in environmental samples.
研究领域:
分析化学
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环境科学
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DOI
高影响因子
MICROCHEMICAL JOURNAL
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2025
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IF 5.1
Mengling Tu,Wen Ma,Jia Chen,Yunxiao Zhu,Yang Liu,Xiaoli Ni,Xianjiang Li
In recent years, imidacloprid, a first generation neonicotinoid pesticide, has attracted considerable attention due to its high detection rate in the environment and food, as well as its detrimental impact on human beings. The identification of structure-related impurities constitutes an essential aspect of pesticide registration and product standard development, and is of paramount importance for exposure risk and safety evaluation. In this study, the analysis of impurities in high-purity imidacloprid material was conducted using a combination of liquid chromatography-high resolution mass spectrometry (Orbitrap) and machine learning platform (SIRIUS + CSI:FingerID). The structure of IMI, as well as the feature fragments, were served as the foundation for decoding the chemical structures of the impurities, and this procedure was guided by the molecular formulas and fragment tree by SIRIUS + CSI:FingerID. Ultimately, 28 impurities were annotated and assigned confidence levels, of which 10 had CAS registry numbers, 5 had PubChem CIDs, and 4 were further verified by three dimension indexes (retention time, ultraviolet spectra and mass spectra) using standards. These impurities have been categorized into three levels (4 in level 1, 12 in level 2a and 12 in level 2b) according to their credibility. This approach was capable of providing accurate molecular formulas and possible structures of impurities, thereby greatly saving the time taken to resolve mass spectra. The elucidated impurity fingerprint can assist in the assessment of the potential health and ecological risks associated with imidacloprid and related impurities.
研究领域:
环境科学
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农药化学
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毒理学
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产品关联
DOI
高影响因子
BIODEGRADATION
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2018
·Vol. 29
·期 6
·593-603
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IF 2.41
Shi Zhoukun,Dong Weiliang,Xin Fengxue,Liu Jiawei,Zhou Xinhai,Xu Fanli,Lv Ziyao,Ma Jiangfeng,Zhang Wenming,Fang Yan,Jiang Min
Abstract An acetamiprid-degrading fungus was isolated from contaminated soil and identified as Fusarium sp. strain CS-3 based on physiological, biochemical, and molecular analyses. Strain CS-3 exploited 50 mg/L as the sole carbon source in liquid culture, removing 98% in 96 h. Strain CS-3 retained its acetamiprid degradation abilities over a wide range of pH (5.0–8.0) and temperature (20–42 °C). HPLC–MS analysis showed that N ′-[(6-chloropyridin-3-yl)methyl]- N -methylacetamide, 2-chloro-5-hydroxymethylpyridine, and 6-chloronicotinic acid were identified as the most predominant metabolites, forming the basis for a newly described acetamiprid degradation pathway. Strain CS-3 efficiently degraded 99.6% of 50 mg/kg acetamiprid in soil, indicating potential for soil remediation. Graphical abstract
研究领域:
环境科学
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微生物学
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生物修复
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2023
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IF 3
Jingwen Zhang,Junning Liu,Yuheng Wang,Yong Wang,Ruiqin Yang,Xinyang Zhou
Since neonicotinoid insecticides are now the most extensively used insecticides worldwide, there are increasing cases of neonicotinoid poisoning. A rapid and sensitive method was developed for the determination of ten neonicotinoid insecticides and a metabolite 6-chloronicotinic acid in human whole blood. The types and amounts of extraction solvent, salting-out agent, and adsorbent in the QuEChERS method were optimized by comparing the absolute recoveries of 11 analytes. The separation was performed on an Agilent EC18 column with the gradient elution with 0.1% formic acid in water and acetonitrile as the mobile phase. The quantification was achieved by Q Exactive orbitrap high-resolution mass spectrometry under parallel reaction monitoring scan mode. The 11 analytes showed good linearity with R 2 ≥ 0.9950, LODs ranging from 0.01 μg/L to 0.30 μg/L, and LOQs from 0.05 μg/L to 1.00 μg/L. The recoveries ranged from 78.3% to 119.9% at low, medium, and high spiked concentrations of blank blood, with matrix effects ranging from 80.9% to 117.8%, inter-day RSDs from 0.7% to 6.7%, and intra-day RSDs from 2.7% to 9.8%. The method was furthermore applied to a real case of neonicotinoid insecticide poisoning to demonstrate its feasibility. The proposed method is suitable for the rapid screening of neonicotinoid insecticides in poisoned human blood in the field of forensic science, as well as monitoring of neonicotinoid insecticide residues in humans in the field of environmental safety, compensating for a lack of studies on neonicotinoid insecticide determination in biological samples.
研究领域:
分析化学
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法医学
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环境科学
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毒理学
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产品关联
DOI
PubMed
高影响因子
SCIENCE OF THE TOTAL ENVIRONMENT
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2023
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IF 9.8
Dong Li,Chunran Zhou,Shuai Wang,Zhan Hu,Jia Xie,Canping Pan,Ranfeng Sun
Overusing imidacloprid (IMI) has been found to impede secondary metabolism and hinder plant growth. The impact of IMI stress on the interaction between metabolites, rhizosphere, and plant-microbe dispersion through various pathways in pepper plants has not been extensively studied. This study investigated the effects of IMI on plant signaling components, secondary metabolic pathways, and microbial communities in the rhizosphere and phyllosphere . Here, the distribution of IMI and its metabolites (6-chloronicotinic acid, IMI-desnitro, 5-hydroxy-IMI, IMI-urea, and IMI-olefin) was primarily observed in the pepper plant leaves. A rise in IMI concentration had a more significant inhibitive effect on the metabolism of pepper leaves than on pepper roots. The findings of non-target metabolomics indicated that IMI exposure primarily suppresses secondary metabolism in pepper plants, encompassing flavones, phenolic acids, and phytohormones. Notably, the IMI treatment disrupted the equilibrium between plants and microbes by decreasing the population of microorganisms such as Vicinamibacteria , Verrucomicrobiae , Gemmatimonadetes , and Gammaproteobacteria in the phyllosphere, as well as Vicinamibacteria , Gemmatimonadetes , Gammaproteobacteria , and Alphaproteobacteria in the rhizosphere of pepper plants. The study demonstrates that overexposure to IMI harms microbial composition and metabolite distribution in the rhizosphere soil and pepper seedlings, inhibiting plant growth.
研究领域:
植物学
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环境科学
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微生物学
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产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）