Luo Yuqiong, Shen Suqin, Luo Jiwen, Wang Xiaoying, Sun Runcang
State Key Laboratory of Pulp & Paper Engineering, South China University of Technology, Guangzhou 510640, China.
Nanoscale. 2015 Jan 14;7(2):690-700. doi: 10.1039/c4nr05999a.
This work reported a facile and green method to prepare highly stable and uniformly distributed Ag nanoparticles (AgNPs), in which a biopolymer xylan was used as the stabilizing and reducing agent via the Tollens reaction under microwave irradiation. Different variables were evaluated to optimize the reaction conditions. Complete characterization was performed using UV-Vis, XRD, TEM, size distribution analysis and XPS. The results revealed that AgNPs were well dispersed with diameters of 20-35 nm due to the packing of xylan. The optimal conditions were as follows: microwave irradiation temperature was 60-70 °C, microwave power was 800 W, microwave time was 30 min, the ratio of xylan to AgNO3 was 50 mg: 0.13 mmol, and ammonia concentration was 2%. In addition, the AgNPs were collected via high-speed centrifugal separation, and the supernatant was tested by HPAEC, GPC, FT-IR, and NMR. By comparing the structure of xylan before and after the reaction, the reaction mechanism was discussed. It was noted that the xylan-AgNPs composites showed high selectivity and sensitivity for Hg(2+) detection. The other 15 metal ions used had no obvious effect on the detection of Hg(2+), and the limit of detection (LOD) was 4.6 nM, which is lower than the allowed maximum level of 30 nM for drinking water by WHO. In addition, the xylan-AgNPs composites can be applied for Hg(2+) detection in real water samples. This study provides a novel way for the high-value utilization of a rich biomass resource, and a green method for the synthesis of AgNPs for the selective and sensitive detection of harmful heavy metals.
本工作报道了一种简便、绿色的方法来制备高度稳定且分布均匀的银纳米颗粒(AgNPs),其中生物聚合物木聚糖在微波辐射下通过托伦反应用作稳定剂和还原剂。评估了不同变量以优化反应条件。使用紫外可见光谱(UV-Vis)、X射线衍射(XRD)、透射电子显微镜(TEM)、尺寸分布分析和X射线光电子能谱(XPS)进行了全面表征。结果表明,由于木聚糖的包裹作用,AgNPs分散良好,直径为20 - 35纳米。最佳条件如下:微波辐射温度为60 - 70℃,微波功率为800瓦,微波时间为30分钟,木聚糖与硝酸银的比例为50毫克:0.13毫摩尔,氨浓度为2%。此外,通过高速离心分离收集AgNPs,并对上清液进行高效阴离子交换色谱(HPAEC)、凝胶渗透色谱(GPC)、傅里叶变换红外光谱(FT-IR)和核磁共振(NMR)测试。通过比较反应前后木聚糖的结构,讨论了反应机理。值得注意的是,木聚糖-AgNPs复合材料对Hg(2+)检测具有高选择性和灵敏度。所使用的其他15种金属离子对Hg(2+)的检测没有明显影响,检测限(LOD)为4.6 nM,低于世界卫生组织规定的饮用水允许最大含量30 nM。此外,木聚糖-AgNPs复合材料可用于实际水样中Hg(2+)的检测。本研究为丰富的生物质资源的高值利用提供了一种新途径,以及一种绿色合成AgNPs用于选择性和灵敏检测有害重金属的方法。