Wang Ling-Juan, Han Wei, Lou Ting-Ting, Ma Lin-Lin, Xiao Ya-Bing, Xu Zhou, Chen Mao-Long, Cheng Yun-Hui, Ding Li
School of Food Science and Bioengineering, Changsha University of Science & Technology, Changsha 410114, China.
Technical Center for Animal, Plant, Foodstuffs and Industrial Product Safety, Tianjin Customs, Tianjin 300457, China.
Anal Methods. 2023 Jan 19;15(3):343-352. doi: 10.1039/d2ay01287a.
For environmental safety, it is important to establish a simple, rapid, and sensitive method for emerging pollutants. Here, a dispersive solid-phase extraction (d-SPE) method based on an iron-based metal-organic framework (Fe-MIL-88-NH) combined with high-performance liquid chromatography (HPLC) was developed for tetrabromobisphenol A (TBBPA) in water samples. Fe-MIL-88-NH was synthesized using a solvothermal method and completely characterized. Fe-MIL-88-NH had good water stability and gave a maximum adsorption capacity of 40.97 mg g for TBBPA. The adsorption of TBBPA on Fe-MIL-88-NH followed Langmuir adsorption models and a pseudo-second-order kinetic model. The bromine ion and the hydroxyl group of TBBPA could form strong hydrogen bond interactions with the amino protons around the cavity of Fe-MIL-88-NH, which was in accord with the molecular simulation calculations. Furthermore, several important d-SPE parameters were optimized, such as the amount of materials, extraction time, pH, ionic strength, elution solvent type, and volume. The established method showed good linearity in the concentration range of 0.005-100 μg g ( ≥ 0.9996). This method's limits of detection (LOD) and quantification (LOQ) were 0.001 μg g and 0.005 μg g, respectively. The recoveries in spiked water samples ranged from 87.5% to 104.9%. The proposed method was applied successfully to detect TBBPA in environmental water samples.
为确保环境安全,建立一种针对新兴污染物的简单、快速且灵敏的方法至关重要。在此,开发了一种基于铁基金属有机框架(Fe-MIL-88-NH)结合高效液相色谱(HPLC)的分散固相萃取(d-SPE)方法,用于测定水样中的四溴双酚A(TBBPA)。采用溶剂热法合成了Fe-MIL-88-NH,并对其进行了全面表征。Fe-MIL-88-NH具有良好的水稳定性,对TBBPA的最大吸附容量为40.97 mg/g。TBBPA在Fe-MIL-88-NH上的吸附遵循朗缪尔吸附模型和准二级动力学模型。TBBPA的溴离子和羟基可与Fe-MIL-88-NH孔腔周围的氨基质子形成强氢键相互作用,这与分子模拟计算结果一致。此外,还优化了几个重要的d-SPE参数,如材料用量、萃取时间、pH值、离子强度、洗脱溶剂类型和体积。所建立的方法在0.005 - 100 μg/g的浓度范围内具有良好的线性(≥ 0.9996)。该方法的检测限(LOD)和定量限(LOQ)分别为0.001 μg/g和0.005 μg/g。加标水样的回收率在87.5%至104.9%之间。所提出的方法成功应用于环境水样中TBBPA的检测。