scholarly journals Determination of Phthalate Esters in Beverages and Water Samples by Solid Phase Extraction with Resin Based COFs as Filler

Water ◽  
2021 ◽  
Vol 13 (23) ◽  
pp. 3338
Author(s):  
Yunjie Ma ◽  
Xin Gao ◽  
Yang Ruan ◽  
Hang Cui ◽  
Li Zhang ◽  
...  

Resin based covalent organic framework material was used as filler for solid phase extraction (SPE), and the solid phase extraction effect was compared with that of traditional COF material (TpBD COFs). The enrichment capacity of four phthalate esters (dimethyl phthalate, diethyl phthalate, dibutyl phthalate, dioctyl phthalate) in beverage samples was investigated by SPE. Adsorption experiments showed that the kinetic adsorption behavior of COF materials for phthalate esters (PAEs) was more consistent with the quasi-second-order kinetic adsorption model, and the static adsorption behavior is more in line with the Freundlich isothermal adsorption model. Solid phase extraction experiments proved that the SPE column prepared with two COF materials as adsorbents had good adsorption effects, high recovery (water: 97.99–100.56% and beverage: 97.93–100.23%) and were reusable (50 cycles), which could meet the requirements for trace detection of phthalate ester. It was found that the solid phase extraction effect was better than the four types of commercial SPE columns. The new COF material reduced the cost of monomer use and provided the possibility for its industrial production. Meanwhile, it also provided a new feasible scheme for enriching trace phthalate esters in practical samples.

2019 ◽  
Vol 102 (5) ◽  
pp. 1624-1631 ◽  
Author(s):  
Shuo Yin ◽  
Yi Yang ◽  
Danni Yang ◽  
Yongxin Li ◽  
Yang Jiang ◽  
...  

Abstract Background: Beverages can be easily contaminated by phthalate esters (PAEs) during the production, bottling, and transportation processes. It is necessary to determine the contamination level in beverages for assessment of human exposure. Objective: In this study, magnetic solid-phase extraction (MSPE) was combined with HPLC for the determination of 11 PAEs in beverages. Methods: Self-synthesized magnetic multiwalled carbon nanotubes (m-MWCNTs) were used as the adsorbent for PAE extraction. To extract the PAEs, an appropriate amount of m-MWCNTs and NaCl was added to the beverage sample. The mixture was mixed on a vortex mixer, the magnetic sorbent was collected with the aid of a magnet, and the supernatant was removed. Then, the analytes were eluted with n-hexane–acetone (1+1, v/v). Finally, the eluent was analyzed by the HPLC method. The separation was accomplished on a Phenomenex Luna-C18 column (250 × 4.6 mm, 5 μm), and the detection wavelength was set at 225 nm. Results: The linear ranges of the method were 2–300 μg/L with correlation coefficients greater than 0.9981. The LOD and LOQ were in the range of 0.659–5.33 × 10–2 μg/L and 2.20–17.8 × 10–2 μg/L, respectively. The recoveries of the method ranged from 79.8 to 114%, with the relative SDs less than 15.8%. The established method has been successfully applied for the determination of 11 PAEs in mineral water, carbonated soft drink, tea beverage, and fruit juice samples. PAEs were detected at 0.246–34.3 μg/L in these samples. Conclusions: The m-MWCNTs are the satisfactory sorbent for MSPE because of their strong adsorption capacity for PAEs. The established MSPE-HPLC method is rapid, easy, sensitive, green, and cost-effective. It can be applied to the analysis of trace PAEs in plastic bottled beverages. Highlights: Three magnetic nanoparticles (MNPs), including Fe3O4 MNPs, m-MWCNTs, and magnetic graphene oxide, were synthesized, and m-MWCNTs were chosen as the sorbent of MSPE for PAE extraction because of their strong adsorption capacity for PAEs. An MSPE–HPLC method has been developed for the analysis of 11 phthalates in plastic bottled beverages. The established method was successfully applied to the analysis of 11 phthalates in four types of beverage samples.


2020 ◽  
Vol 12 (40) ◽  
pp. 4906-4912
Author(s):  
Qingsong Zhang ◽  
Guangyang Liu ◽  
Xiaolin Cao ◽  
Jungang Yin ◽  
Ziping Zhang

In this paper, magnetic ZIF-67 composites were prepared by an in situ method and utilized in the magnetic solid-phase extraction of phthalate esters.


NANO ◽  
2014 ◽  
Vol 09 (04) ◽  
pp. 1450054 ◽  
Author(s):  
XIAOYING DENG ◽  
XIAOQING CHEN ◽  
XINYU JIANG

We report a novel solid-phase extraction adsorbent for the preconcentration of three phthalate esters (PAEs) from aqueous samples. The material was obtained by modifying multiwalled carbon nanotubes (MWCNTs) with mesoporous silica. The structural characterization of the adsorbent was conducted by Fourier transform infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM) and N 2 adsorption–desorption measurement, which confirmed the successful coating of mesoporous silica on MWCNTs and the adsorbent possessing large surface and porous structure. The effects of adsorbent amount, type and volume of eluent and sample pH on extraction efficiency were optimized. Following extraction, the PAEs were quantified by high performance liquid chromatography (HPLC). Under optimal conditions, the recoveries ranged from 89.8% to 96.3%. The calibration plot was linear in the 3–1000 ng⋅mL-1 concentration range, with correlation coefficients ranging from 0.9993 to 0.9995. The repeatability of the method, expressed as relative standard deviation (RSD), ranged from 3.8% to 7.7% (for n = 5). Limits of detection (LODs) were between 0.28 ng mL-1 and 0.53 ng⋅mL-1. The relative recoveries (RR) for spiked river water, pond water and tap water samples were in the ranges of 80.9–98.0%, 82.7–96.1% and 88.3–95.5%, respectively. The results showed that the method obviously had a large potential for preconcentration and determination of PAEs in environmental samples.


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