Performance Study of Prothioconazole Microcapsules Prepared by Solvent Evaporation Method
CHEN Ge,, CAO LiDong,, XU ChunLi, ZHAO PengYue, CAO Chong, LI FengMin, HUANG QiLiang,Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193
Abstract 【Objective】The biodegradable material poly (3-hydroxybutyrate-co-4-hydroxybutyrate) (P (3HB-co-4HB)) was used as the wall material to prepare prothioconazole microcapsules. The effect of preparation process on the microcapsule size, pesticide loading and encapsulation efficiency was optimized. The microcapsules with good dispersion, small particle size, and high pesticide loading were screened out, and the preliminary researches on the release kinetics, photodegradation, and indoor biological activity on Sclerotium rolfsii were carried out. The purpose of this study is to provide a theoretical basis and technical support for improving the stability and utilization efficiency of prothioconazole in the environment.【Method】The solvent evaporation method was used to prepare prothioconazole microcapsules, and the effects of the mass ratio of core to wall material, volume ratio of oil to water, mass fraction of emulsifier and shearing speed on the particle size, pesticide loading and encapsulation efficiency of the microcapsules were investigated through a single factor test. Taking pesticide loading and particle size as the key technical indicators, the optimal preparation parameters were screened out through the L9 (34) orthogonal test, which was further verified. The morphological and structural features, release performance and photodegradability of the microcapsules were determined by scanning electron microscope (SEM), fourier transform infrared (FTIR) spectrometer, and high performance liquid chromatography (HPLC). The toxicity of prothioconazole microcapsules on S. rolfsii was investigated by indoor bioassay.【Result】The mass ratio of core to wall material had a significant effect on the pesticide loading capacity of the microcapsules. As the ratio of core material increased, the loading capacity gradually increased. The volume ratio of oil to water, PVA mass fraction, and shearing speed had significant effects on the microcapsule particle size. As the shearing speed and PVA mass fraction increased, the microcapsule particle size gradually decreased. The volume ratio of oil to water had a great influence on the morphology and dispersion of microcapsules, and the influence of various factors on the encapsulation efficiency of the microcapsules was not significant. The optimal preparation parameters obtained through the L9 (34) orthogonal test was as follows: the mass ratio of core to wall material of 1﹕5, volume ratio of oil to water of 1﹕5, PVA mass fraction of 2%, and shearing speed of 12 000 r/min. Under the optimal preparation process, spherical prothioconazole microcapsules with a particle size (D50) of 3.32 μm and a span of 2.82 were prepared with a loading content of 15.52% and an encapsulation efficiency of 80.24%. Compared with prothioconazole technical material, the microcapsules had better sustained-release performance, and the release kinetics conformed to Fick’s diffusion law, presenting two processes of “burst release” followed by “sustained release”. The photostability of prothioconazole in the microcapsules in aqueous solution was enhanced, and the half-life of photolysis was doubled. The mycelial growth rate inhibition result showed that the fungicidal activity of prothioconazole microcapsules against S. rolfsii was equivalent to that of prothioconazole technical material.【Conclusion】Prothioconazole microcapsules with biodegradable material P (3HB-co-4HB) as a carrier were prepared, and different preparation processes affect the pesticide loading, dispersion state and particle size of microcapsules. The slow and sustained release and photostability are of great significance for reducing the amount of pesticide applied and improving the utilization efficiency of pesticide, which has potential application in control of peanut southern blight. Keywords:prothioconazole;polyhydroxybutyrate;microcapsule;preparation process;controlled release;Sclerotium rolfsii
PDF (1803KB)元数据多维度评价相关文章导出EndNote|Ris|Bibtex收藏本文 本文引用格式 陈歌, 曹立冬, 许春丽, 赵鹏跃, 曹冲, 李凤敏, 黄啟良. 溶剂蒸发法制备丙硫菌唑微囊及其性能研究[J]. 中国农业科学, 2021, 54(4): 754-767 doi:10.3864/j.issn.0578-1752.2021.04.008 CHEN Ge, CAO LiDong, XU ChunLi, ZHAO PengYue, CAO Chong, LI FengMin, HUANG QiLiang. Performance Study of Prothioconazole Microcapsules Prepared by Solvent Evaporation Method[J]. Scientia Acricultura Sinica, 2021, 54(4): 754-767 doi:10.3864/j.issn.0578-1752.2021.04.008
1.3.5 微囊缓释性能 采用透析袋法[21]研究丙硫菌唑原药与最优制备工艺条件下丙硫菌唑微囊的释放性能。将一定质量样品浸入含200 mL 30%甲醇水溶液的密封容器中,室温下于转速200 r/min搅拌,每隔一段时间取一定体积上清液,每次取样后立即补充相同体积缓冲溶液,通过HPLC测定丙硫菌唑的释放量。按公式(4)计算丙硫菌唑累积释放量并绘制累积释放曲线。
Er =$\frac{{{V}_{e}}\sum\limits_{i=0}^{n-1}{{{C}_{i}}+{{V}_{0}}{{C}_{n}}}}{{{m}_{pesticide}}}$×100% Er:累积释放量(%);Ve:每次取样体积(1 mL);Ci:第i次取样时释放液的浓度(mg·mL-1);V0:释放介质总体积(200 mL);Cn:第n次取样释放液的浓度(mg·mL-1);n:取样次数;mpesticide:丙硫菌唑微囊有效成分的总质量(mg)。
1.3.6 微囊水中光解 取一定量的丙硫菌唑微囊,分散于30 mL 0.2%吐温-80水溶液中,置于具塞石英管内,以高压氙灯作为光源,辐照度为25 mW·cm-2,石英管距光源10 cm,启动转动电机并不断搅拌使反应液均匀受光,温度保持在(20±1)℃,待光解仪稳定后进行光解试验。光照不同时间后分别取样1 mL,用甲醇稀释后超声处理30 min,过0.22 μm滤膜后用HPLC检测丙硫菌唑浓度(mg·L-1)。以丙硫菌唑原药作为对照。每个试验重复3次。
Table 3 表3 表3PVA质量分数对微囊性能的影响 Table 3Effect of mass fraction of PVA on microcapsule performance
PVA质量分数 Mass fraction of PVA (%)
载药量 Loading content (%)
包封率 Encapsulation efficiency (%)
粒径 D50 (μm)
跨距 Span
0.5
15.58±0.83a
77.47±5.79a
4.61±0.06a
3.70b
1
15.69±0.21a
78.90±1.47a
3.46±0.06b
4.26a
1.5
15.67±0.34a
80.47±4.07a
3.21±0.06c
3.69b
2
15.12±1.69a
78.70±3.04a
2.55±0.04d
2.91c
同列数据后不同小写字母表示经Duncan氏新复极差法检验在P<0.05水平差异显著。下同 Different lowercases after the data in the same column indicate significant difference at 0.05 level by Duncan’s new multiple range test. The same as below
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