Department of Chemistry, Semnan University, Semnan, Iran.
Department of Chemistry, Semnan University, Semnan, Iran.
Anal Chim Acta. 2019 Jan 24;1047:275-284. doi: 10.1016/j.aca.2018.10.028. Epub 2018 Oct 26.
In this work, a rapid and simple method is applied using a newly synthesized nanoadsorbent for the extraction and preconcentration of the drugs Amitriptyline (AMT) and Nortriptyline (NRT), which are then determined using high performance liquid chromatography. We focus on the facile synthesis of FeO@SiO@N, as a new and effective adsorbent, and the effervescent salt-assisted dispersive magnetic micro solid-phase extraction method. The applied method and modification of the surface of FeO@SiO with the nitrogen-rich group lead to an increase in the interaction between the nanoadsorbent used and the analytes, and increase the extraction recovery. The accuracy of the synthesized nanoadsorbent is confirmed by the FT-IR, FE-SEM, XRD, and VSM analytical techniques. In order to obtain the best experimental conditions, optimization of the main variables involved is carried out using the central composite design method. Under the optimum experimental conditions, the limits of detection (LODs), linear dynamic ranges (LDRs), and relative standard deviations (RSDs for n = 5) for NRT and AMT were found to be as follow: LODs, 0.03 and 0.05 ng/mL; RSDs, 2.04 and 1.1 for NRT and AMT, respectively; and LDRs, 0.07-2000 ng/mL. Furthermore, the results obtained show that the nanoadsorbent can be used for five times with an extraction recovery more than 80% and 70% for AMT and NRT, respectively.
在这项工作中,应用了一种新合成的纳米吸附剂,用于提取和预浓缩阿米替林(AMT)和去甲替林(NRT)药物,然后使用高效液相色谱法进行测定。我们专注于简便合成 FeO@SiO@N,作为一种新的有效吸附剂,以及使用发泡盐辅助分散磁微固相萃取方法。应用的方法和 FeO@SiO 的表面改性导致纳米吸附剂与分析物之间的相互作用增强,从而提高了萃取回收率。通过傅里叶变换红外光谱(FT-IR)、场发射扫描电子显微镜(FE-SEM)、X 射线衍射(XRD)和振动样品磁强计(VSM)分析技术来验证合成纳米吸附剂的准确性。为了获得最佳的实验条件,采用中心复合设计方法对涉及的主要变量进行优化。在最佳实验条件下,NRT 和 AMT 的检测限(LOD)、线性动态范围(LDR)和相对标准偏差(n=5 时的 RSD)分别为:LOD,0.03 和 0.05 ng/mL;RSD,NRT 和 AMT 分别为 2.04 和 1.1;LDR,0.07-2000 ng/mL。此外,所得结果表明,纳米吸附剂可重复使用五次,对 AMT 和 NRT 的萃取回收率分别超过 80%和 70%。