School of Ecology and Environment, Anhui Normal University, Wuhu 241000, PR China.
Anal Methods. 2021 Jan 28;13(3):381-389. doi: 10.1039/d0ay02140g.
A direct immersion solid-phase microextraction method for determining tetracyclines (TCs) was developed by coupling with high-performance liquid chromatography. A carbon aerogel (CA) was synthesized as a fiber coating with high extractive properties and a low density of 0.1855 g cm-3via ambient pressure drying and carbonization. The as-synthesized CA exhibited a high specific surface area and a cross-linked structure; it was characterized via scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and Brunauer-Emmett-Teller analysis, etc. The extraction performance for six TCs was investigated, and the main experimental parameters were optimized by the Box-Behnken design. Adsorption kinetics, Langmuir and Freundlich models were used to clarify the extraction mechanism. This method showed wide linear ranges of 1-500 μg L-1, low limits of detection of 0.52-1.05 μg L-1, good repeatability of 1.37-12.47%, and satisfactory inter-fiber reproducibility of 8.51-15.81% relative standard deviation for the detection of six TCs. Moreover, this study provided an interesting insight into the detection of TCs residues in food samples.
一种直接浸入式固相微萃取方法,用于与高效液相色谱法相结合来测定四环素(TCs)。通过常压干燥和碳化合成了一种具有高萃取性能和低密度(0.1855 g cm-3)的碳纤维涂层——碳气凝胶(CA)。所合成的 CA 表现出高比表面积和交联结构;通过扫描电子显微镜、透射电子显微镜、傅里叶变换红外光谱和 Brunauer-Emmett-Teller 分析等进行了表征。考察了六种 TCs 的萃取性能,并通过 Box-Behnken 设计优化了主要实验参数。采用吸附动力学、朗缪尔和弗伦德利希模型来阐明萃取机理。该方法对六种 TCs 的线性范围为 1-500 μg L-1,检测限低至 0.52-1.05 μg L-1,重复性好(1.37-12.47%),纤维间重现性好(相对标准偏差为 8.51-15.81%),可用于检测食品样品中的 TCs 残留。