JOURNAL OF CHROMATOGRAPHY A
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2025
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IF 4
Jing Lin,Dan Li,Peiyuan Luo,Laisheng Li
we reported a new phenylcarbamoylethylenediureido-β-cyclodextrin CSP (PUCDP) for HPLC, which was conveniently prepared by immobilizing the addition product of diethylenetriamino-β-CD with 3,5-dichlorophenyl isocyanate onto silica gel. After structural characterization, the chromatographic performance of PUCDP was preliminarily evaluated by using common 11 triazole pesticides as probes. The results showed that PUCDP had strong chiral separation abilities for all triazoles ( R s=1.44–3.70). Especially, it could first completely separate triazoles with two chiral centers such as cyproconazole, triadimenol, metconazole, paclobutrazol and bitertanol, into four peaks, respectively. Some effects on the separation and detection were investigated, including the composition of mobile phase, pH value, column temperature, and absorption wavelength. Based on comprehensive optimization of chromatographic conditions and a homemade PUCDP column, we established a new method for the simultaneous separation and determination of twelve triazole pesticide enantiomeric residues (flutriafol, cyproconazole, tebuconazole, and metconazole) in nine kinds of fruits and vegetables (apple, banana, orange, pear, cucumber, green pepper, tomato, wax gourd, cabbage). After simple QuEChERS pretreatment, samples were analyzed under the optimized conditions of a gradient elution program with acetonitrile-water (ACN H 2 O) containing 0.5 % triethylammonium acetate (TEAA) buffer (pH=6.30) as the mobile phase at a flow rate of 0.5 mL min -1 , a photo-diode array (PDA) detector at 220 nm, column temperature at 20 °C and an injection volume of 20 μL. The method exhibited good linear relationship ( R 2 =0.9941–0.9999) in the range of 0.5–60 mg l -1 for all triazole enantiomers. The limits of detection (LODs) and limits of quantification (LOQs) ranged from 0.05 to 0.10 mg kg -1 and 0.15 to 0.30 mg kg -1 , respectively. The average recoveries of all enantiomers were 81.60 %-104.08 % with intra -day and inter -day relative standard deviations (RSDs) of 1.91 %-3.50 % ( n = 5) and 2.05 %-4.49 % ( n = 15), respectively. The determination of 54 actual samples indicated the practicality of the method. This simultaneous determination method could save analysis time, and reduce solvent consumption with high analysis efficiency. The excellent performance of PUCDP was mainly related to the rich hydrogen bonds (donors and acceptors), the large π-π stacking and the extended cavity derived from the diphenylurea groups, which was consistent with the results of AutoDock molecular docking.
研究领域:
分析化学
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色谱技术
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农药残留分析
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食品安全
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手性分离技术
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PubMed
高影响因子
MOLECULES
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2024
·Vol. 29
·期 6
·1353
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IF 4.2
Liwang Fei,Lingyun Hao
Rice blast, caused by the filamentous fungusPyricularia oryzae, has long been one of the major threats to almost all rice-growing areas worldwide. Metconazole, 5-(4-chlorobenzyl)-2, 2-dimethyl-1-(1H-1, 2, 4-triazol-1-ylmethyl) cyclopentanol, is a lipophilic, highly active triazole fungicide that has been applied in the control of various fungal pathogens of crops (cereals, barley, wheat), such as theFusariumandAlternariaspecies. However, the antifungal activity of metconazole againstP. oryzaeis unknown. In this study, metconazole exhibited broad spectrum antifungal activities against sevenP. oryzaestrains collected from rice paddy fields and the wild type strain P131. Scanning electron microscopic analysis and fluorescein diacetate staining assays revealed that metconazole treatment damaged the cell wall integrity, cell membrane permeability and even cell viability ofP. oryzae, resulting in deformed and shrunken hyphae. The supplementation of metconazole in vitro increased fungal sensitivity to different stresses, such as sodium dodecyl sulfate, congo red, sodium chloride, sorbitol and oxidative stress (H2O2). Metconazole could inhibit key virulence processes ofP. oryzae, including conidial germination, germ tube elongation and appressorium formation. Furthermore, this chemical preventedP. oryzaefrom infecting barley epidermal cells by disturbing appressorium penetration and subsequent invasive hyphae development. Pathogenicity assays indicated a reduction of over 75% in the length of blast lesions in both barley and rice leaves when 10 μg/mL of metconazole was applied. This study provides evidence to understand the antifungal effects of metconazole againstP. oryzaeand demonstrates its potential in rice blast management.
研究领域:
植物病理学
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农学
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DOI
PubMed
高影响因子
TALANTA
·
2025
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IF 6.1
Yuanyuan Zheng,Manyi Wang,Mengyuan Lv,Yu Huang,Bingyu Wang,Chenqi Niu,Di Chen
This study presents a novel liquid-filled stick microextraction (LFSME) method for the efficient extraction of hydrophobic compounds from aqueous samples. The LFSME device, inspired by a single-use swab, consists of a hollow plastic stick pre-filled with a hydrophobic deep eutectic solvent (DES), and wrapped with polypropylene fabric at the end. Upon activation, the DES is released and absorbed by the polypropylene fabric, enabling direct immersion into the sample solution for efficient extraction. The extracted analytes are subsequently desorbed with acetonitrile and analyzed by liquid chromatography-ultraviolet detection. The method demonstrated excellent analytical performance, including high enrichment factors (34–90), good linearity (R 2 > 0.99), and low limits of detection (LODs: 0.99–2.61 ng/mL) for the five target triazole pesticides. The disposable and portable nature of the LFSME device eliminates the need for complex sample handling, providing a cost-effective and user-friendly solution for routine monitoring of pesticide residues and other contaminants in complex matrices.
研究领域:
分析化学
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食品科学
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PubMed
高影响因子
Food Chemistry-X
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2025
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IF 8.2
Yuxin Wang,Jin Liu,Suzhen Li,Jizhen Fu,Xiaowen Wang,Li Li,Xu Jing
The widespread use of triazole fungicides has raised concerns over residual. This study presents an automated, environmentally friendly, simple, and efficient method for detecting triazole fungicides in food samples, utilizing high-throughput liquid processing, dispersive liquid-liquid microextraction, and ultra-high-performance liquid chromatography-tandem mass spectrometry. The automated liquid handling workstation was employed to automate the whole sample pre-treatment process. Fatty acid, bio-based solvent, and saturated sodium chloride solution were used as the extractant, dispersant, and demulsifier, respectively. The whole operation process obviated the use of toxic reagents and eliminated the need for time-consuming centrifugation. The linear ranged from 0.01 to 1 μg L −1 with limits of detection and quantification of 0.003 μg L −1 and 0.01 μg L −1 , respectively. Ten triazole fungicides were successfully detected in food samples with recoveries of 70.1 %–105.7 %. The automation of dispersive liquid-liquid microextraction demonstrates huge potential for broad applicability within the field of food safety testing.
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PubMed
高影响因子
ACS Applied Materials & Interfaces
·
2025
·
IF 8.2
Haonan Zhang,Donglai Zhang,Bin Yu,Qiuyu Xiong,Yun Fang,Zifeng Yang,Zerui Li,Jingli Cheng,Jinhao Zhao
The design of intelligent pesticide delivery systems based on the characteristics of soil-borne diseases is of great significance for improving pesticide utilization efficiency and achieving long-lasting disease control. Herein, a cost-effective and degradable functional poly(butylene oxalate) (PBO) material was constructed and applied for the encapsulation of metconazole (MEZ) to develop a sustained-release pesticide delivery system (MEZ@PBO). The optimized MEZ@PBO was mainly distributed within the 200–300 nm range, with a fungicide-loading capacity reaching 55.7%. Release experiments confirmed the regulatory effect of the PBO molecular weight on the release rate, with higher molecular weight resulting in a longer sustained release period, thereby prolonging the duration of efficacy. MEZ@PBO significantly enhances the photostability of the fungicide while preventing pesticide loss caused by leaching. Moreover, pot experiments indicated that MEZ@PBO achieved long-lasting control of the Fusarium crown rot. After 14 days, the inhibition rate against Fusarium crown rot was 37.9 and 22.4% higher than those of the metconazole technical material and commercial formulation, respectively. Biosafety evaluation and degradation tests further confirmed the environmental friendliness and crop safety. This work offers a promising strategy for enhancing the stability, release control, and efficacy of fungicides in sustainable agriculture.
研究领域:
农业化学
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植物病理学
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高分子材料科学
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纳米药物递送
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可持续农业
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PubMed
高影响因子
CHEMICAL ENGINEERING JOURNAL
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2026
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IF 13.2
Haonan Zhang,Yun Fang,Bin Yu,Zhengang Xie,Qiuyu Xiong,Donglai Zhang,Zifeng Yang,Zerui Li,Jingli Cheng,Jinhao Zhao
The persistent outbreaks of Fusarium crown rot (FCR) pose significant challenges to food security, while traditional fungicide formulations provide short-term control and are associated with potential environmental safety risks. This study developed a stimulus-responsive, controlled-release fungicide system (MEZ@CM-VEAL) tailored to high-risk environmental conditions of FCR. It achieved an optimized loading capacity of 60.0 ± 1.7% and a loading efficiency of 87.0 ± 2.4%, with an average particle size of 454.8 nm. MEZ@CM-VEAL enhanced metconazole (MEZ) utilization during application through pH/enzyme-triggered controlled release, improved photostability, and enhanced horizontal migration in soil. In vitro antifungal activity tests showed that MEZ@CM-VEAL exhibited inhibitory effects on Fusarium pseudograminearum comparable to commercial formulations. Subsequent pot experiments confirmed the long-lasting effectiveness of MEZ@CM-VEAL in controlling FCR, with inhibition rates against F. pseudograminearum 46.7% and 30.7% higher than those of MEZ technical (MEZ TC) and commercial suspension concentrate (MEZ SC), respectively. Furthermore, MEZ@CM-VEAL exhibited significantly lower toxicity, with reductions of 2.4- and 2.3-fold to zebrafish, and 6.0- and 7.2-fold to earthworms, compared to MEZ TC and MEZ SC, respectively. This approach not only provides long-lasting protection against diseases and reduces pesticide usage, but also minimizes negative impacts on the ecological environment, thereby promoting sustainable agricultural development.
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高影响因子
FOOD CHEMISTRY
·
2024
·
IF 8.5
Jin Liu,Yuanjun Nie,Yu Niu,Li Li,Xu Jing
A universal, green, and rapid lignin-based emulsive liquid-liquid microextraction (ELLME) method was established to detect nine triazole fungicides in water, juice, vinegar , and alcoholic beverages via UHPLC-MS/MS. By employing an environmentally friendly emulsifier (lignin), the proposed ELLME was compatible with more extractants, and not restricted to fatty acids. Due to the high amphiphilic properties and three-dimensional structure of lignin, the emulsion was quickly formed through several aspirate-dispense cycles of the green extractant (guaiacol) and lignin solution. And a micropipette was used for rapid microextraction . The limit of detection was 0.0002–0.0057 μg L −1 . The extraction recoveries and relative standard deviation were 81.7%–102.0% and 0.9%–7.1%, respectively. Finally, three green metric tools were used to verify the greenness of the whole procedure. The proposed lignin-based ELLME successfully emulsified green solvents , indicating that emerging solvents may be excellent alternatives as extractants in ELLME for pesticide residue analysis in food samples.
研究领域:
分析化学
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环境科学
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食品科学
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DOI
PubMed
高影响因子
TOXICOLOGY LETTERS
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2023
·
IF 3.5
Yingna Zhai,Shaowei Wang,Bingru Zhang,Yunbing Tang,Hong Wang,Jingjing Li,Zhiyan Hu,Yiyan Wang,Huitao Li,Ren-shan Ge
3β-Hydroxysteroid dehydrogenase/steroid Δ 5,4 -isomerase 1 (3β-HSD1) plays a critical role in the biosynthesis of progesterone from pregnenolone in the human placenta to maintain normal pregnancy. Whether they inhibit placental 3β-HSD1 and mode of inhibition remains unclear. In this study, we screened 21 pesticides and fungicides in five classes to inhibit human 3β-HSD1 and compared them to rat homolog 3β-HSD4. 3β-HSD activity was measured by catalyzing pregnenolone to progesterone in the presence of NAD + . Of the 21 chemicals, azoles (difenoconazole), thiocarbamates (thiram and ferbam) and organochlorine (hexachlorophene) significantly inhibited human 3β-HSD1 with half maximal inhibitory concentration (IC 50 ) values of 2.77, 0.24, 0.68, and 17.96 μM, respectively. We also found that difenoconazole, ferbam and hexachlorophene are mixed/competitive inhibitors of 3β-HSD1 while thiram is a mixed/noncompetitive inhibitor. Docking analysis showed that difenoconazole and hexachlorophene bound steroid-binding site. Difenoconazole and hexachlorophene except thiram and ferbam also significantly inhibited rat 3β-HSD4 activity with IC 50 of 1.12 and 2.28 µM, respectively. Thiram and ferbam significantly inhibited human 3β-HSD1 possibly by interfering with cysteine residues, while they had no effects on rat 3β-HSD4. In conclusion, some pesticides potently inhibit placental 3β-HSD, leading to the reduction of progesterone formation.
研究领域:
药理学
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毒理学
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生殖生物学
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酶学
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PubMed
高影响因子
MICROCHEMICAL JOURNAL
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2022
·
IF 5.304
Xin-Li Xu,Bin Wang,Yu-Wei Liu,Wen-Xuan Li,Jian-Yuan Wu,Hang Yuan,Xia Xu,Di Chen
In this study, a novel in-pipette-tip natural-feather-supported liquid microextraction (NF-SLME) method was developed for conveniently extracting hydrophobic compounds in aqueous samples. Natural feathers were used as the support medium of an oily extraction solvent and an in-pipette-tip extraction device was simply constructed with the cost less than 0.1 CNY. The whole extraction process could be conveniently conducted with a pipettor. As a proof of concept, the in-pipette-tip NF-SLME method was applied to extract antidepressants in urines. The best extraction recoveries were obtained when the extraction solvent was 15 μL of n -octanol, the pH of the sampling solution was 10.0, the desorption solution was 200 μL of acetonitrile, and the numbers of cycles of drawing solution in/out for extraction and elution were 5 and 2, respectively. Coupled with high-performance liquid chromatography–ultraviolet, a quantification method was validated in ranges of 0.05–10 μg/mL with satisfactory linearities (R 2 ≥ 0.988). The limits of quantification were calculated to range from 0.032 to 0.048 μg/mL, which is adequate for antidepressant analysis in urine. The potential of the in-pipette-tip NF-SLME method was further illustrated by the successful extraction of triazole pesticides and androgenic steroids with good recoveries.
研究领域:
分析化学
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环境科学
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医学检测
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DOI
高影响因子
FOOD AND CHEMICAL TOXICOLOGY
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2023
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IF 4.3
Jianmin Sang,Hong Wang,Yang Yu,Zhongyao Ji,Miaomiao Xia,Ting Hao,Linxi Li,Ren-shan Ge
Azole fungicides are widely used in the agricultural industry to control fungal infections in crops. However, recent studies have shown that some azole fungicides inhibit the activity of 3β-hydroxysteroid dehydrogenases (3β-HSDs) in the gonads. Out of the 16 azole fungicides tested, 8 were found to inhibit human KGN cell 3β-HSD2 with IC 50 values of less than 100 μM. The strongest inhibitor was difenoconazole, with an IC 50 value of 1.88 μM. In contrast, only 3 of the azole fungicides inhibited rat testicular 3β-HSD1, which was less sensitive to inhibition. Azole fungicides potently inhibited progesterone secretion by KGN cells under basal and forskolin stimulated conditions at ≥ 5 μM. The inhibitory strength of azole fungicides was determined by their lipophilicity (LogP), molecular weight, pKa, and binding energy. A pharmacophore analysis revealed that the hydrogen bond acceptor-lipid group was a critical feature required for inhibition. Overall, these findings suggest that the use of azole fungicides have unintended consequences on reproductive health due to their inhibition of gonadal 3β-HSDs. Key words: Azole fungicides; steroid hormones; 3β-hydroxysteroid dehydrogenase; docking analysis; lipophilicity.
研究领域:
药理学
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毒理学
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生殖健康
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PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Fanglin Liu,Yongqiang Pang,Dexiang Liu,Qianwen Cao,Ying Rong,Xinglin Liao,Qiman Jiang,Peirong Xu,Di Chen,Xia Xu
In this study, Artemisia argyi essential oil (AAEO), extracted from the leaves of Artemisia argyi , was employed as a green extraction solvent for in-syringe kapok fiber-supported liquid-phase microextraction (KF-SLME) of hydrophobic compounds in aqueous samples. The wheat of natural kapok fiber as the support medium was 2 mg, and the optimum volume of the extraction solvent AAEO was 12.5 μL. The volume of green desorption solvent 75 % ethanol was 100 μL, which realized a highly environmentally friendly sample preparation method. By simply pulling and pushing the syringe plunger five times, the extraction process enabled rapid and convenient enrichment of analytes while removing most interferences. Coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS), the AAEO-based in-syringe SLME method was applied as a proof-of-concept study to determine triazole fungicides (TFs) residues in fruit juices, herbal oral liquids and herbal extract granules. Employing in-syringe KF-SLME prior to LC-MS/MS detection significantly reduced the limits of quantification (LOQs) by 5–50-fold. The integrated AAEO-based in-syringe KF-SLME-LC-MS/MS method demonstrated satisfactory linearity (R 2 ≥ 0.995), accuracies (86.5 %–115.1 %), and precisions (1.2 %–12.7 %) using an isotope calibration method. Furthermore, three greenness assessment metrics uniformly highlighted its outstanding environmental friendliness. The proposed method offers competitive advantages in terms of its environmentally friendly approach, detection sensitivity, analysis cost, and operational convenience.
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
危险品化学品经营许可证（带存储）