Department of Chemistry, Science and Research Branch, Islamic Azad University, Tehran, Iran.
Research Group of Food, Halal and Agricultural Products, Research Department of Food Technology and Agricultural Products, Standard Research Institute (SRI), P.O. Box 31745-139, Karaj, Iran.
Environ Monit Assess. 2020 Apr 3;192(5):262. doi: 10.1007/s10661-020-8185-6.
In this research, an efficient sorbent based on poly(β-cyclodextrin-ester)-functionalized silica-coated magnetic nanoparticles (MNPs-CDP) was prepared and used for magnetic solid-phase extraction of the malachite green (MG) and crystal violet (CV) from water samples prior to their determination by high-performance liquid chromatography-ultra violet detection (HPLC-UV). The synthesized nanoparticles were characterized by the field emission-scanning electron microscopy (FE-SEM) and Fourier transform infrared spectroscopy (FT-IR). Of course, the factors, which could influence the extraction efficiency like pH, sorbent amount, salt content, extraction time, desorption time, eluent type, and volume and sample volume, were optimized by response surface methodology. Then, for both of MG and CV, good linearity (0.1-200 μg L, r ≥ 0.99) was achieved under the optimized conditions. The limits of detection (LODs) and the limits of quantification (LOQs), for both of MG and CV, were 0.03 μg L and 0.1 μg L, respectively. Precision of the method expressed as the relative standard deviations (RSDs) at concentration level of 100 μg L was 5.6 and 4.2 for MG and CV, respectively. Ultimately, usability of proposed method was investigated by analysis of CV and MG in tap water, fish pond water, and the lake water, and the satisfactory recoveries were obtained in the range of 92-100.5%.
在这项研究中，制备了一种基于聚（β-环糊精酯）-功能化二氧化硅包覆磁性纳米粒子（MNPs-CDP）的高效吸附剂，并用于水样中孔雀石绿（MG）和结晶紫（CV）的磁固相萃取，然后采用高效液相色谱-紫外检测法（HPLC-UV）对其进行测定。通过场发射扫描电子显微镜（FE-SEM）和傅里叶变换红外光谱（FT-IR）对合成的纳米粒子进行了表征。当然，通过响应面法优化了影响萃取效率的因素，如 pH 值、吸附剂用量、盐含量、萃取时间、解吸时间、洗脱剂类型和体积以及样品体积。然后，在优化条件下，MG 和 CV 均获得了良好的线性关系（0.1-200μg/L，r≥0.99）。MG 和 CV 的检出限（LODs）和定量限（LOQs）分别为 0.03μg/L 和 0.1μg/L。在 100μg/L 浓度水平下，方法的精密度表示为相对标准偏差（RSDs），MG 和 CV 的 RSDs 分别为 5.6%和 4.2%。最终，通过对自来水、鱼塘水和湖水进行 CV 和 MG 的分析，考察了该方法的实用性，在 92-100.5%的范围内获得了令人满意的回收率。
