紫苏籽壳提取物纳米银颗粒的制备及性能表征

Preparation and Performance Characterization of Silver Nanoparticles of Perilla Seed Shell Extract

为进一步提高紫苏资源的利用价值,本研究以紫苏籽壳提取物(PSHE)为原料,通过单因素实验,分别考察硝酸银浓度、提取液浓度、超声波功率、超声温度和超声时间对紫苏籽壳提取物纳米银(PSHE@AgNPs)银离子还原率的影响,并在单因素实验基础上,采用响应面法对超声波辅助制备PSHE@AgNPs的工艺进行优化,并采用X射线衍射、傅里叶变换红外光谱、热重分析及透射电子显微镜对PSHE@AgNPs的结构及性能进行表征。结果表明,PSHE@AgNPs制备最佳工艺为:硝酸银浓度15 mmol/L,提取液浓度0.4 g/mL,超声波功率480 W,超声温度80℃,超声时间7 h,在此工艺条件下制备的PSHE@AgNPs银离子还原率达92.37%。X射线衍射分析表明PSHE@AgNPs具有面心立方结构;傅里叶变换红外光谱表明PSHE@AgNPs表面存在植物化学物质,酚类化合物参与纳米银的合成;热重分析显示了PSHE@AgNPs的热稳定性,在276.7~420.3℃范围内存在主要的质量损失,质量减少46.74%;透射电子显微镜显示PSHE@AgNPs是粒径均值为27.97 nm的近球形分散颗粒。研究结果可为超声波辅助绿色合成粒径小、分散性高、具有热稳定性的面心立方结构的PSHE@AgNPs提供理论指导,并推动其在生物材料和医学领域的应用。

In order to further improve the utilization value of Perilla resources,this study used Perilla seed shell extract(PSHE)as raw material,through single factor experiments,the effects of silver nitrate concentration,extract concentration,ultrasonic power,ultrasonic temperature and ultrasonic time on the silver ion reduction rate of Perilla seed shell extract silver nanoparticles(PSHE@AgNPs)were investigated,response surface methodology(RSM)was used to optimize the ultrasonic-assisted preparation of PSHE@AgNPs,the structure and properties of PSHE@AgNPs were characterized by Xray diffraction,fourier transform infrared spectroscopy,thermogravimetric analysis and transmission electron microscope.The results showed that the optimal PSHE@AgNPs preparation process involved a silver nitrate concentration 15 mmol/L,extract concentration 0.4 g/mL,ultrasonic power 480 W,ultrasonic temperature 80℃,and ultrasonic time 7 hours.Under these conditions,the silver ion reduction rate of PSHE@AgNPs reached an impressive 92.37%.X-ray diffraction analysis confirmed the presence of a face-centered cubic structure in PSHE@AgNPs.Fourier-transform infrared spectroscopy showed that there were plant chemical substances on the surface of PSHE@AgNPs,and phenolic compounds were involved in the synthesis of nano-silver.Thermal gravimetric analysis demonstrated the exceptional thermal stability of PSHE@AgNPs,with a major mass loss of 46.74%in the range of 276.7~420.3℃.Transmission electron microscopy displayed PSHE@AgNPs as highly dispersed near-spherical particles with an average particle size of 27.97 nm.These research findings would provide valuable theoretical guidance for the ultrasound-assisted green synthesis of PSHE@AgNPs with small particle size,superior dispersion,and remarkable thermal stability in a face-centered cubic structure.Furthermore,these results contribute to advancing the application of PSHE@AgNPs in the fields of biomaterials and medicine.