Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan 250014, China.
School of Life Sciences, Shandong Normal University, 88 Wenhua East Road, Jinan 250014, China.
Talanta. 2017 Apr 1;165:18-26. doi: 10.1016/j.talanta.2016.12.021. Epub 2016 Dec 10.
In this research, the successfully developed molecularly imprinted solid-phase extraction (MISPE) method based on SH-Au modified silica gel for Sudan dyes determination has been described. Gold nanoparticles (Au NPs) were organized onto the surface of silica gel through the covalent binding between sulfydryl and Au. Subsequently, molecularly imprinted polymers (MIPs) were prepared via the graft polymerization using Au NPs as the functional monomer. The composition and morphology of MIPs were characterized by X-ray photoelectron spectroscopy (XPS), Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TG). Binding property was systematically evaluated through adsorption isotherm, adsorption kinetics, and selective recognition capacity. MISPE pretreatment was successfully established after optimizing various parameters. Under optimized conditions, good linearity for six investigated Sudan dyes was ranged from 0.005 to 10.0μgg (R>0.999) with low limits of detection and quantification (1.5-4.7 and 5.2-15.5ngg, respectively). The recoveries at three different spiked levels (0.05, 0.5, and 2.0μgg of each Sudan dye) were ranged from 87.2% to 94.7% with RSD below 6.1% (n=3). The results demonstrated one reliable, sensitive and accurate MISPE pretreatment technique with excellent reproducibility for the determination of six Sudan dyes in chili powder samples.
本研究描述了一种基于巯基-金（SH-Au）修饰硅胶的成功开发的苏丹染料分子印迹固相萃取（MISPE）方法。金纳米粒子（Au NPs）通过巯基与 Au 之间的共价键结合被组织到硅胶表面上。随后，通过使用 Au NPs 作为功能单体的接枝聚合制备了分子印迹聚合物（MIPs）。MIPs 的组成和形态通过 X 射线光电子能谱（XPS）、傅里叶变换红外光谱（FT-IR）、扫描电子显微镜（SEM）、透射电子显微镜（TEM）和热重分析（TG）进行了表征。通过吸附等温线、吸附动力学和选择性识别能力系统地评估了结合性能。经过优化各种参数后，成功建立了 MISPE 预处理。在优化条件下，六种研究的苏丹染料的线性范围为 0.005 至 10.0μg/g（R>0.999），检测限和定量限低（分别为 1.5-4.7 和 5.2-15.5ng/g）。在三个不同添加水平（每种苏丹染料的 0.05、0.5 和 2.0μg/g）下的回收率在 87.2%至 94.7%之间，相对标准偏差（RSD）低于 6.1%（n=3）。结果表明，该方法是一种可靠、灵敏、准确的 MISPE 预处理技术，具有良好的重现性，可用于辣椒粉样品中六种苏丹染料的测定。
