Faculty of Chemistry and Petroleum Sciences, Shahid Beheshti University, G.C., Evin, Tehran, Iran.
Faculty of Chemistry and Petroleum Sciences, Shahid Beheshti University, G.C., Evin, Tehran, Iran.
J Chromatogr A. 2019 Dec 20;1608:460426. doi: 10.1016/j.chroma.2019.460426. Epub 2019 Aug 5.
In the current study, MMWCNTs@MIL-101(Cr) (FeO/multiwalled carbon nanotubes/MIL-101(Cr)) was synthesized and utilized as a new sorbent for the first time. It was employed successfully for the extraction of parabens and phthalate esters (PEs) from water and cream samples prior to their quantification with HPLC-DAD. The prepared metal-organic-framework (MOF) was characterized by field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FT-IR), energy-dispersive X-ray spectroscopy (EDX), EDX mapping, thermogravimetric analysis (TGA), vibrating-sample magnetometer (VSM) and X-ray powder diffraction (XRD). Three phthalate esters (dimethyl phthalate (DMP), diethyl phthalate (DEP), diallyl phthalate (DAP)) and two parabens (methylparaben (MP) and butylparaben (BP)) were chosen as model analytes. Several experimental factors affecting the extraction efficiency, including pH value, nanosorbent amount, sorption time, salt concentration, sample volume, type and volume of the eluent, and elution time were investigated. The optimization of the extraction method was carried out by response surface methodology (RSM) and desirability function (DF) approach. Under the opted conditions, the method was linear in the range of 0.1-1500 μg L with coefficients of determination > 0.9991. The limits of detection of PEs and parabens were found in the range of 0.03-0.15 μg L (S/N = 3). The relative standard deviations were less than 7.5% and the extraction recoveries ranged from 38.04 to 70.62%. The present method was simple, rapid, inexpensive and environmentally friendly and was successfully utilized for the determination of PEs and parabens in water samples and various types of cream samples with satisfactory results.
在当前的研究中，合成了 MMWCNTs@MIL-101(Cr)（FeO/多壁碳纳米管/MIL-101(Cr)），并首次将其用作新型吸附剂。它被成功地用于从水样和乳样中提取对羟基苯甲酸酯和邻苯二甲酸酯（PEs），然后用 HPLC-DAD 进行定量分析。所制备的金属有机骨架（MOF）通过场发射扫描电子显微镜（FESEM）、透射电子显微镜（TEM）、傅里叶变换红外光谱（FT-IR）、能谱（EDX）、能谱mapping、热重分析（TGA）、振动样品磁强计（VSM）和 X 射线粉末衍射（XRD）进行了表征。选择了三种邻苯二甲酸酯（邻苯二甲酸二甲酯（DMP）、邻苯二甲酸二乙酯（DEP）、邻苯二甲酸二烯丙酯（DAP））和两种对羟基苯甲酸酯（对羟基苯甲酸甲酯（MP）和对羟基苯甲酸丁酯（BP））作为模型分析物。考察了影响萃取效率的几个实验因素，包括 pH 值、纳米吸附剂用量、吸附时间、盐浓度、样品体积、洗脱剂类型和体积以及洗脱时间。通过响应面法（RSM）和理想函数（DF）方法对萃取方法进行了优化。在优化条件下，该方法在 0.1-1500μg/L 范围内呈线性，相关系数>0.9991。PEs 和对羟基苯甲酸酯的检出限在 0.03-0.15μg/L（S/N=3）范围内。相对标准偏差小于 7.5%，萃取回收率在 38.04-70.62%之间。本方法简单、快速、经济、环保，成功地用于水样和各种类型乳样中 PEs 和对羟基苯甲酸酯的测定，结果令人满意。
