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Vortex-assisted Dispersive Solid-phase Extraction Using Schiff-base Ligand Anchored Nanomagnetic Iron Oxide for Preconcentration of Phthalate Esters and Determination by Gas Chromatography and Flame Ionization Detector
Analytical Sciences ( IF 1.6 ) Pub Date : 2021-09-10 , DOI: 10.2116/analsci.20p363
Nahid Pourreza 1 , Reza Zadeh-dabbagh 1
Affiliation  

Phthalate esters are synthetic chemicals that are widely used in plastic industries as plasticizer. They are harmful to humans and could be carcinogenic. In this research, a new nanosorbent was prepared via a Schiff-base reaction between p-dimethylaminobenzaldehyde and Fe3O4@SiO2-NH2 nanoparticles. A characterization of the sorbent was performed by Fourier-transform infrared spectroscopy, transmission electron microscopy, scanning electron microscopy, and energy-dispersive spectroscopy. A modified nanosorbent has a core shell structure, and shows a great tendency towards the sorption of phthalate esters. Hence, it was utilized for the dispersive solid-phase extraction of six phthalate esters and determination by gas chromatography–flame ionization detection. Several variables, such as the pH, sorbent amount, salt effects, extraction and desorption time, extraction solvent type and volume, were investigated to establish the optimal conditions. Calibration graphs were linear in the range of 1.0 – 150.0 μg L−1 for dimethyl phthalate, bis-(2-ethylhexyl) phthalate, di-n-octyl phthalate and 0.1 – 200.0 μg L−1 for diethyl phthalate, di-n-butyl phthalate and butyl benzyl phthalate, respectively. The obtained limits of detections (S/N = 3) were in the range of 0.02 – 0.31 μg L−1. Application of the method for the enrichment and determination of phthalate esters in mineral water, natural low fat yogurt and sodium chloride infusion (0.9%, w/v) was investigated.

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中文翻译:

席夫碱配体锚定纳米磁性氧化铁涡流辅助分散固相萃取预浓缩邻苯二甲酸酯及气相色谱和火焰离子化检测器测定

邻苯二甲酸酯是合成化学品,在塑料工业中广泛用作增塑剂。它们对人体有害,可能致癌。在这项研究中,一个新的nanosorbent制备经由之间的席夫碱反应p -dimethylaminobenzaldehyde和Fe 3 ö 4 @SiO 2 -NH 2纳米粒子。通过傅里叶变换红外光谱、透射电子显微镜、扫描电子显微镜和能量色散光谱对吸附剂进行表征。改性纳米吸附剂具有核壳结构,对邻苯二甲酸酯的吸附作用很大。因此,它被用于六种邻苯二甲酸酯的分散固相萃取和气相色谱-火焰电离检测的测定。研究了几个变量,如 pH 值、吸附剂用量、盐效应、萃取和解吸时间、萃取溶剂类型和体积,以确定最佳条件。校准曲线是在1.0的范围内的线性- 150.0微克大号-1为邻苯二甲酸二甲酯,双- (2-乙基己基)邻苯二甲酸酯,二- Ñ- 邻苯二甲酸辛酯,邻苯二甲酸二乙酯、邻苯二甲酸二丁酯和邻苯二甲酸丁苄酯分别为0.1 – 200.0 μg L -1。获得的检测限 ( S/N = 3) 在 0.02 – 0.31 μg L -1的范围内。研究了该方法在矿泉水、天然低脂酸奶和氯化钠输液 (0.9%, w/v) 中邻苯二甲酸酯的富集和测定中的应用。

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更新日期:2021-09-10
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