Belbasi Zeynab, Petr Jan, Sevcik Juraj, Jirovsky David, Hrbac Jan
Faculty of Science, Department of Analytical Chemistry, Palacky University, 17. Iistopadu 12, 771 46 Olomouc, Czech Republic.
Faculty of Science, Department of Chemistry, Masaryk University, Kamenice 5, 625 00 Brno, Czech Republic.
ACS Omega. 2024 Jan 20;9(4):5038-5045. doi: 10.1021/acsomega.3c09474. eCollection 2024 Jan 30.
In this work, we demonstrate a sensitive high-performance liquid chromatography (HPLC) method for the determination of piperazine antihistamine drugs employing innovative electrochemical detection based on a spark-generated nickel oxide nanoparticle-modified carbon fiber microelectrode built into a miniaturized electrochemical detector. The direct carbon fiber-to-nickel plate electrode spark discharge, carried at 0.8 kV DC, with the nickel electrode connected to the negative pole of the high-voltage power supply, provides extremely fast (1 s) in situ tailoring of the carbon fiber microelectrode surface by nickel oxide nanoparticles. It has been found that nickel oxide nanoparticles exhibit an electrocatalytic effect toward the piperazine moiety electrooxidation process, as confirmed by voltammetric experiments, revealing the shift in the peak potential from 1.25 to 1.09 V versus Ag/AgCl. Cetirizine, cyclizine, chlorcyclizine, flunarizine, meclizine, and buclizine were selected as sample piperazine antihistamine drugs, while diclofenac served as an internal standard. The isocratic reversed-phase separation of the above set was achieved within 15 min using an ARION-CN 3 μm column with a binary mobile phase consisting of 50 mM phosphate buffer (pH 3) and methanol (45/55, v/v). The limits of detection (LOD) were within the range of 3.8-120 nM (for cyclizine and buclizine) at = +1500 mV (vs Ag/AgCl), while the response was linear within the concentration range measured up to 5 μmol L. The method was successfully applied to the determination of piperazine antihistamine drugs in spiked plasma samples.
在本工作中，我们展示了一种灵敏的高效液相色谱（HPLC）方法，用于测定哌嗪类抗组胺药物。该方法采用基于火花产生的氧化镍纳米颗粒修饰的碳纤维微电极的创新电化学检测技术，该微电极内置在小型化电化学检测器中。在0.8 kV直流电压下进行的直接碳纤维到镍板电极的火花放电，镍电极连接到高压电源的负极，可通过氧化镍纳米颗粒在极短时间（1 s）内对碳纤维微电极表面进行原位修饰。伏安实验证实，氧化镍纳米颗粒对哌嗪部分的电氧化过程具有电催化作用，相对于Ag/AgCl，峰电位从1.25 V移至1.09 V。选择西替利嗪、赛克利嗪、氯环利嗪、氟桂利嗪、美克洛嗪和布克利嗪作为哌嗪类抗组胺药物样品，双氯芬酸作为内标。使用ARION-CN 3 μm色谱柱，以50 mM磷酸盐缓冲液（pH 3）和甲醇（45/55，v/v）组成的二元流动相，在15分钟内实现了上述物质的等度反相分离。在 = +1500 mV（相对于Ag/AgCl）时，检测限（LOD）在3.8 - 120 nM范围内（针对赛克利嗪和布克利嗪），而在高达5 μmol/L的测量浓度范围内响应呈线性。该方法成功应用于加标血浆样品中哌嗪类抗组胺药物的测定。
