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An electrodeposited terephthalic acid-layered double hydroxide (Cu-Cr) nanosheet coating for in-tube solid-phase microextraction of phthalate esters
Microchimica Acta ( IF 5.3 ) Pub Date : 2020-01-10 , DOI: 10.1007/s00604-019-4102-5
Mohsen Aghaziarati 1 , Yadollah Yamini 1 , Maryam Shamsayei 1
Affiliation  

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 two-electrode 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. Graphical abstract A CuCr-layered double hydroxide nanosheet intercalated with terephthalic acid was used as a coating for in-tube solid phase microextraction of some phthalate esters from beverage samples.

中文翻译:

用于管内固相微萃取邻苯二甲酸酯的电沉积对苯二甲酸层状双氢氧化物 (Cu-Cr) 纳米片涂层

引入了对苯二甲酸 (TPA/LDH) 插入的 CuCr 层状双氢氧化物纳米片作为管内固相微萃取 (IT-SPME) 的涂层。通过使用双电极电沉积将涂层放置在不锈钢管的内表面上。通过 X 射线衍射、扫描电子显微镜和傅里叶变换红外光谱对吸附剂进行了表征。与硝酸盐-LDH 涂层相比,TPA/LDH 涂层具有更高的提取效率、长寿命、良好的机械稳定性和大比表面积。该方法用于邻苯二甲酸二甲酯 (DMP)、邻苯二甲酸二丁酯 (DBP)、邻苯二甲酸二烯丙酯 (DAP) 和邻苯二甲酸二乙基己酯 (DEHP) 的萃取、预浓缩和后续基于 HPLC 的测定。溶液pH值、盐浓度、优化了提取解吸条件,以及溶液中酒精含量对提取效率的影响。在最佳条件下,响应在 0.05 至 1000 μg L -1 酯浓度范围内呈线性,检测限(S/N = 3)范围在 0.01 至 0.1 μg L -1 之间。批间和批内精密度(RSD%,对于 n = 3)范围分别为 3.8 至 6.8% 和 3.5 至 5.7%。该方法已成功应用于不同饮料样品中四种邻苯二甲酸酯的测定。图形摘要 嵌有对苯二甲酸的 CuCr 层状双氢氧化物纳米片用作涂层,用于从饮料样品中对某些邻苯二甲酸酯进行管内固相微萃取。并对溶液中酒精含量对提取效率的影响进行了优化。在最佳条件下,响应在 0.05 至 1000 μg L -1 酯浓度范围内呈线性,检测限(S/N = 3)范围在 0.01 至 0.1 μg L -1 之间。批间和批内精密度(RSD%,对于 n = 3)范围分别为 3.8 至 6.8% 和 3.5 至 5.7%。该方法已成功应用于不同饮料样品中四种邻苯二甲酸酯的测定。图形摘要 嵌有对苯二甲酸的 CuCr 层状双氢氧化物纳米片用作涂层,用于从饮料样品中对某些邻苯二甲酸酯进行管内固相微萃取。并对溶液中酒精含量对提取效率的影响进行了优化。在最佳条件下,响应在 0.05 至 1000 μg L -1 酯浓度范围内呈线性,检测限(S/N = 3)范围在 0.01 至 0.1 μg L -1 之间。批间和批内精密度(RSD%,对于 n = 3)范围分别为 3.8 至 6.8% 和 3.5 至 5.7%。该方法已成功应用于不同饮料样品中四种邻苯二甲酸酯的测定。图形摘要 嵌有对苯二甲酸的 CuCr 层状双氢氧化物纳米片用作涂层,用于从饮料样品中对某些邻苯二甲酸酯进行管内固相微萃取。并且检测限(在 S/N = 3 时)范围在 0.01 到 0.1 μg L -1 之间。批间和批内精密度(RSD%,对于 n = 3)范围分别为 3.8 至 6.8% 和 3.5 至 5.7%。该方法已成功应用于不同饮料样品中四种邻苯二甲酸酯的测定。图形摘要 嵌有对苯二甲酸的 CuCr 层状双氢氧化物纳米片用作涂层,用于从饮料样品中对某些邻苯二甲酸酯进行管内固相微萃取。并且检测限(在 S/N = 3 时)范围在 0.01 到 0.1 μg L -1 之间。批间和批内精密度(RSD%,对于 n = 3)范围分别为 3.8 至 6.8% 和 3.5 至 5.7%。该方法已成功应用于不同饮料样品中四种邻苯二甲酸酯的测定。图形摘要 嵌有对苯二甲酸的 CuCr 层状双氢氧化物纳米片用作涂层,用于从饮料样品中对某些邻苯二甲酸酯进行管内固相微萃取。
更新日期:2020-01-10
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