An electrodeposited terephthalic acid-layered double hydroxide (Cu-Cr) nanosheet coating for in-tube solid-phase microex
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ORIGINAL PAPER
An electrodeposited terephthalic acid-layered double hydroxide (Cu-Cr) nanosheet coating for in-tube solid-phase microextraction of phthalate esters Mohsen Aghaziarati 1 & Yadollah Yamini 1 & Maryam Shamsayei 1 Received: 5 August 2019 / Accepted: 28 December 2019 # Springer-Verlag GmbH Austria, part of Springer Nature 2020
Abstract A CuCr-layered double hydroxide nanosheet intercalated with terephthalic acid (TPA/LDH) was introduced as a coating for the in-tube solid phase microextraction (IT-SPME). The coating was placed on the inner surface of a stainless steel tube by using twoelectrode electrodeposition. The sorbent was characterized by X-ray diffraction, scanning electronic microscopy, and Fourier transform infrared spectroscopy. The TPA/LDH coating, compared to a nitrate-LDH coating, exhibits enhanced extraction efficiency, long lifetime, good mechanical stability, and a large specific surface. The method was used for the extraction, preconcentration, and subsequent HPLC-based determination of dimethyl phthalate (DMP), dibutyl phthalate (DBP), diallyl phthalate (DAP), and diethylhexyl phthalate (DEHP). The effects of pH value of the solution, salt concentration, extraction and desorption conditions, and the effect of the alcohol content of the solution on the extraction efficiency were optimized. Under optimal conditions, the response is linear in the 0.05 to 1000 μg L−1 ester concentration range, and the limits of detection (at S/N = 3) range between 0.01 to 0.1 μg L−1. The inter- and intra-assay precisions (RSD%, for n = 3) range from 3.8 to 6.8% and from 3.5 to 5.7%, respectively. The method was successfully applied to the determination of four phthalate esters in different beverage samples. Keywords Alcoholic beverages . Coating . Dimethyl phthalate . Dibutyl phthalate . Diallyl phthalate . Diethylhexyl phthalate . Electrochemical synthesis . Nanosheets . Stainless steel . Tube
Introduction Since the invention of the solid-phase microextraction (SPME) [1], this technique has progressed rapidly. The outstanding features of this technique are as follows: eco-compatibility, automation capability, easy sampling, simple extraction, economical applications, and great efficiency. These features have made it a robust choice over conventional extraction/microextraction strategies for a wide range of anaElectronic supplementary material The online version of this article (https://doi.org/10.1007/s00604-019-4102-5) contains supplementary material, which is available to authorized users. * Yadollah Yamini [email protected] 1
Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran, Iran
lytical applications [2]. Several configurations and implementations, such as fibers, capillary tubes, stir bars, thin films, packed tubes, and magnetic nanoparticles, have been introduced in order to facilitate convenient sampling, automation, and sample introduction, depending on the application [3]. Microextraction techniques using a capillary tube named in-tube SPME (IT-SPME) have sev
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