College of Science, Beijing Key Laboratory of Environmentally Harmful Chemical Analysis, Beijing University of Chemical Technology, Beijing, P. R. China.
J Sep Sci. 2019 Apr;42(8):1600-1609. doi: 10.1002/jssc.201801244. Epub 2019 Feb 21.
In this study, magnetized MOF-74 (Ni) was prepared using an ultrasound-assisted synthesis method. This novel functional magnetic adsorbent was characterized using various techniques. Using the prepared material as adsorbents, a magnetic solid-phase extraction method coupled with high-performance liquid chromatography was proposed for determining four phthalate esters in Chinese liquor samples. The extraction parameters, including solution pH, adsorbent amount, extraction time, and eluent type and volume, were optimized. Under the optimized conditions, proposed method showed good linearity within the range of 1.53-200 μg/L for diphenyl phthalate, 2.03-200 μg/L for butyl benzyl phthalate, 7.02-200 μg/L for diamyl phthalate, and 6.03-200 μg/L for dicyclohexyl phthalate, with correlation coefficients > 0.9944, low limits of detection (0.46-2.10 μg/L, S/N = 3), and good extraction repeatability (relative standard deviations of 3.7%, n = 6). This method was successfully used to analyze phthalate esters in Chinese liquor samples with recoveries of 74.4-104.8%. Two phthalate esters were detected in two samples, both at concentrations that satisfied the Chinese national standard, indicating this method has practical application prospects. The extraction efficiency of this method was also compared with conventional solid-phase extraction using commercial C cartridges. The results demonstrated that the proposed magnetic solid-phase extraction is a simple, time-saving, efficient, and low-cost method.
在这项研究中，使用超声辅助合成方法制备了磁性 MOF-74（Ni）。通过各种技术对这种新型功能磁性吸附剂进行了表征。使用制备的材料作为吸附剂，提出了一种结合高效液相色谱的磁性固相萃取法，用于测定白酒样品中的四种邻苯二甲酸酯。优化了萃取参数，包括溶液 pH 值、吸附剂用量、萃取时间以及洗脱剂类型和体积。在优化条件下，提出的方法在二苯酯、丁基苄基邻苯二甲酸酯、二戊酯和二环己基邻苯二甲酸酯的 1.53-200μg/L 范围内、2.03-200μg/L 范围内、7.02-200μg/L 范围内和 6.03-200μg/L 范围内均表现出良好的线性关系，相关系数均>0.9944，检出限低（0.46-2.10μg/L，S/N=3），萃取重复性好（相对标准偏差为 3.7%，n=6）。该方法成功地用于分析白酒样品中的邻苯二甲酸酯，回收率为 74.4-104.8%。在两个样品中都检测到两种邻苯二甲酸酯，浓度均满足中国国家标准，表明该方法具有实际应用前景。还将该方法的萃取效率与商用 C 柱的常规固相萃取进行了比较。结果表明，所提出的磁性固相萃取是一种简单、省时、高效且低成本的方法。
