Boontongto Tittaya, Burakham Rodjana
Materials Chemistry Research Center, Department of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Khon Kaen University, Khon Kaen, 40002, Thailand.
Heliyon. 2019 Nov 16;5(11):e02848. doi: 10.1016/j.heliyon.2019.e02848. eCollection 2019 Nov.
This work proposes an application of amine-functionalized metal-organic framework (NH-MIL-101(Fe)) as sorbent for dispersive micro-solid phase extraction (D-μSPE) of ten priority phenolic pollutants. The sorbent was simply synthesized under facile condition. The entire D-μSPE process was optimized by studying the effect of experimental parameters affecting the extraction recovery of the target analytes. The final extract was analyzed using high performance liquid chromatography with photodiode array detector. Under the optimum condition, the proposed procedure can be applied for wide linear calibration ranges between 1.25-5000 μg L with the correlation coefficients of greater than 0.9900. The limits of detection (LODs) and limits of quantitation (LOQs) were in the ranges of 0.4-9.5 μg L and 1.25-30 μg L, respectively. The precision evaluated in terms of the relative standard deviations (RSDs) of the intra- and inter-day determinations of the phenol compounds at their LOQ concentrations were below 13.9% and 12.2%, respectively. High enrichment factors up to 120 were reached. The developed method has been successfully applied to determine phenol residues in environmental water samples. The satisfactory recoveries obtained by spiking phenol standards at two different concentrations (near LOQs and 5 times as high as LOQs) ranged from 68.4-114.4%. The results demonstrate that the NH-MIL-101(Fe) material is promising sorbent in the D-μSPE of phenolic pollutants.
本研究提出将胺功能化金属有机框架材料（NH-MIL-101(Fe)）作为吸附剂，用于分散微固相萃取（D-μSPE）十种优先控制酚类污染物。该吸附剂在简便条件下即可简单合成。通过研究影响目标分析物萃取回收率的实验参数，对整个D-μSPE过程进行了优化。最终提取物采用配备光电二极管阵列检测器的高效液相色谱进行分析。在最佳条件下，所提出的方法可用于1.25 - 5000 μg/L的宽线性校准范围，相关系数大于0.9900。检测限（LOD）和定量限（LOQ）分别在0.4 - 9.5 μg/L和1.25 - 30 μg/L范围内。在酚类化合物定量限浓度下，日内和日间测定的相对标准偏差（RSD）评估的精密度分别低于13.9%和12.2%。实现了高达120的高富集因子。所开发的方法已成功应用于测定环境水样中的酚类残留。通过在两个不同浓度（接近定量限和定量限的5倍）添加酚类标准品获得的回收率令人满意，范围为68.4 - 114.4%。结果表明，NH-MIL-101(Fe)材料在酚类污染物的D-μSPE中是一种有前景的吸附剂。
