Department of Chemistry, Semnan University, Semnan 2333383-193, Iran.
Department of Chemistry, Semnan University, Semnan 2333383-193, Iran.
Ultrason Sonochem. 2017 Nov;39:12-24. doi: 10.1016/j.ultsonch.2017.03.024. Epub 2017 Mar 14.
In this work, a rapid and efficient procedure named ultrasound meliorated dispersive micro solid-phase extraction followed by high performance liquid chromatography-ultra violet detection (US-D-μSPE-HPLC-UV) was developed for the pre-concentration of the main trace anti-hypertensive drugs in complex matrices. The basis of this procedure was a polypyrrole-sodium dodecylbenzenesulfonate/zinc oxide (PPy-DBSNa/ZnO) nanocomposite. It was readily synthesized by the impressive way of in situ sonochemical oxidative polymerization in the presence of some additives such as FeCl and DBSNa, ultimately leading to the effective coating of PPy on the ZnO nanoparticle cores. Characterization of the proposed nanosorbent was performed by different techniques such as FESEM, XRD,EDX, and TGA, confirming the high quality and proper physico-chemical properties of the proposed sorbent. In order to better investigate the input variables, the central composite design (CCD) combined with the desirability function (DF) was utilized. The enriched optimum conditions consisted of the initial pH value of 11.8, 15mg of the PPy-DBSNa/ZnO nanocomposite, a sonication time of 4.6min, and 100μL of methanol, resulting in maximum responses at a relatively low extraction time with a logical DF. Under the optimum conditions, good linearity (5-5000, 2.5-3500, and 2.5-3000ngmL for metoprolol, propranolol, and carvedilol, respectively, with the correlation of determinations (Rs) higher than 0.99), low limits of detection (LODs) (0.8-1.5ngmL), proper repeatabilities (relative standard deviation values (RSDs) below 6.3%, n=3), reasonable enrichment factors (EFs) (60-72), and good extraction recoveries (ERs) (higher than %75) were obtainable. These appropriate validations corroborated a good effectiveness of ultrasonic waves in the achievement of a supreme solid phase as well as a facile and efficient microextraction of the low therapeutic concentrations in human plasma and urine samples.
在这项工作中，开发了一种名为超声改良分散微固相萃取结合高效液相色谱-紫外检测（US-D-μSPE-HPLC-UV）的快速高效程序，用于预浓缩复杂基质中的主要痕量抗高血压药物。该程序的基础是聚吡咯-十二烷基苯磺酸钠/氧化锌（PPy-DBSNa/ZnO）纳米复合材料。它是通过在一些添加剂如 FeCl 和 DBSNa 的存在下进行原位超声化学氧化聚合的令人印象深刻的方式轻易合成的，最终导致 PPy 有效地涂覆在 ZnO 纳米颗粒核心上。通过 FESEM、XRD、EDX 和 TGA 等不同技术对所提出的纳米吸附剂进行了表征，证实了所提出的吸附剂具有高质量和适当的物理化学性质。为了更好地研究输入变量，采用了中心复合设计（CCD）与期望函数（DF）相结合的方法。富集的最佳条件包括初始 pH 值为 11.8、15mg PPy-DBSNa/ZnO 纳米复合材料、超声时间 4.6min 和 100μL 甲醇，在相对较低的提取时间内获得最大响应，具有合理的 DF。在最佳条件下，具有良好的线性（分别为 5-5000、2.5-3500 和 2.5-3000ngmL 的 metoprolol、propranolol 和 carvedilol，相关系数（Rs）高于 0.99）、低检测限（LODs）（0.8-1.5ngmL）、适当的重复性（相对标准偏差值（RSDs）低于 6.3%，n=3）、合理的富集因子（EFs）（60-72）和良好的萃取回收率（ERs）（高于 75%）。这些适当的验证证实了超声波在实现高固相以及在人血浆和尿液样品中痕量治疗浓度的简便高效微萃取方面的有效性。
