程敬丽, 肖豆鑫, 梁文龙, 方逊, 张家栋, 赵金浩. pH响应性吡唑醚菌酯/沸石咪唑酯骨架材料纳米颗粒的制备及抑菌活性[J]. 农药学学报, 2022, 24(1): 105-113. DOI: 10.16801/j.issn.1008-7303.2021.0165
    引用本文: 程敬丽, 肖豆鑫, 梁文龙, 方逊, 张家栋, 赵金浩. pH响应性吡唑醚菌酯/沸石咪唑酯骨架材料纳米颗粒的制备及抑菌活性[J]. 农药学学报, 2022, 24(1): 105-113. DOI: 10.16801/j.issn.1008-7303.2021.0165
    CHENG Jingli, XIAO Douxin, LIANG Wenlong, FANG Xun, ZHANG Jiadong, ZHAO Jinhao. Synthesis and fungicidal activity of pH-responsive pyraclostrobin/zeolite imidazole ester framework material nanoparticles[J]. Chinese Journal of Pesticide Science, 2022, 24(1): 105-113. DOI: 10.16801/j.issn.1008-7303.2021.0165
    Citation: CHENG Jingli, XIAO Douxin, LIANG Wenlong, FANG Xun, ZHANG Jiadong, ZHAO Jinhao. Synthesis and fungicidal activity of pH-responsive pyraclostrobin/zeolite imidazole ester framework material nanoparticles[J]. Chinese Journal of Pesticide Science, 2022, 24(1): 105-113. DOI: 10.16801/j.issn.1008-7303.2021.0165

    pH响应性吡唑醚菌酯/沸石咪唑酯骨架材料纳米颗粒的制备及抑菌活性

    Synthesis and fungicidal activity of pH-responsive pyraclostrobin/zeolite imidazole ester framework material nanoparticles

    • 摘要: 沸石咪唑酯骨架材料 (ZIF-8)稳定性好,比表面积大,纳米粒径可调,具有酸敏感性。为研究其在农药递送中作为缓控释载体的性能和应用,以吡唑醚菌酯 (pyraclostrobin,以下简称Pyr)为模式农药,以二价锌为配位中心,二甲基咪唑为有机配体,采用 “一锅法” 制备了pH响应性吡唑醚菌酯控释剂Pyr@ZIF-8;通过扫描电子显微镜(SEM)、动态光散射激光粒度仪(DLS)、傅里叶红外光谱(FTIR)、X射线衍射(XRD)和热重分析(TGA)等物理手段对Pyr@ZIF-8的形貌、粒径和Zeta电位等进行了表征;采用高效液相色谱(HPLC)考察了其在紫外光源下的光解稳定性和不同pH值下的酸控释放性能;最后分别采用菌丝生长速率法和盆栽试验研究了其对油菜菌核病菌的抑制效果。结果表明:所制备的Pyr@ZIF-8的平均粒径为143.1 nm,载体ZIF-8对Pyr的负载率为10.8%;与Pyr原药相比,紫外光照下Pyr@ZIF-8中Pyr的降解率降低了6.2%;在pH值分别为4.0、6.0、8.0的环境下静置24 h,Pyr@ZIF-8中Pyr的释放率分别为88.1% ± 2.5%、67.3% ± 3.1%和25.6% ± 2.9%,表现出pH响应性释放性能;在0.1 μg/mL质量浓度下,Pyr@ZIF-8对油菜菌核病菌的抑制效果比其乳油高16.4% (生长速率法)和9.4% (盆栽试验)。上述结果表明,所制备的纳米递送体系Pyr@ZIF-8不仅具有减缓吡唑醚菌酯光降解的作用,还有良好的酸控缓释和更高的抑菌效果。

       

      Abstract: Zeolite imidazole framework-8 (ZIF-8) has good stability, large specific surface area, adjustable nanometer particle size and the easy decomposition under acidic conditions. In order to study its performance and application prospects as a slow and controlled release carrier in pesticide delivery, pH-responsive release formulation Pyr@ZIF-8 was prepared by one-pot method using pyraclostrobin (Pyr) as the model pesticide, with divalent zinc as the ligand center and dimethylimidazole as the organic ligand. In addition, the morphology, particle size and Zeta potential were characterized by the scanning electron microscope (SEM), dynamic light scattering laser particle size analyzer (DLS), fourier infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA) and other physical means to Pyr@ZIF-8. The morphology, particle size and Zeta potential were characterized. And high performance liquid chromatography (HPLC) was used to investigate its photolysis stability under ultraviolet light source and its acid controlled release performance under different pH values. Finally, fungicidal activity in vitro and in pot experiment were studied. The results showed that the average particle size of Pyr@ZIF-8 was 143.1 nm, and the loading rate was 10.8%. The anti-photodegradation experiments showed a 6.2% reduction in the degradation rate of Pyr in Pyr@ZIF-8 nanoparticle under UV light. After standing for 24 h under the environment of pH 4.0, 6.0 and 8.0, the release rate of Pyr in Pyr@ZIF-8 was 88.1% ± 2.5%, 67.3% ± 3.1% and 25.6% ± 2.9%, respectively, suggesting that Pyr@ZIF-8 had pH-responsive release performance. At a concentration of 0.1 μg/mL, the inhibitory effect of Pyr@ZIF-8 on Sclerotinia sclerotiorum was 16.4% (in vitro) and 9.4% (in pot experiment) higher than its EC. The above results showed that the nano-delivery system Pyr@ZIF-8 not only had the effect of slowing down the photo degradation of Pyr, but also had good pH responsive slow-release performance and higher antifungal efficacy.

       

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