Taghvimi Arezou, Jahed Fatemeh Soghra, Dastmalchi Siavoush, Javadzadeh Yousef
Biotechnology Research Centre, Tabriz University of Medical Science, Tabriz, Iran.
Department of chemistry, Faculty of Science, Azarbijan Shahid Madani University, Tabriz, Iran.
Adv Pharm Bull. 2022 May;12(3):561-567. doi: 10.34172/apb.2022.054. Epub 2021 Jul 4.
This research introduces a polymeric nanosphere as a new dispersive solid phase extraction (DSPE) adsorbent for the extraction of methylphenidate (MPH) from urine and its high performance liquid chromatography (HPLC) analysis. Polymeric nanosphere is a kind of copolymeric network obtained by copolymerization of an ionic liquid monomer and styrene in the presence of vinyltriethoxysilane and 2-hydroxyethylmethacrylate. HPLC coupled with ultra violet detector was applied for the determination and quantification of MPH. Dominant parameters in extraction were modified by the one-parameter-at-a-time method. The results are as follow: 10 mg of polymeric nanospheres (PNS), 400 μL of acetonitrile (ACT), 5 mL of urine with the pH value of 9, and the extraction and desorption times of 2 and 5 minutes, respectively, which can be selected as the optimum extraction conditions. Calibration curve was plotted through optimized conditions, and the proposed method was validated. The results demonstrated that the method presented linearity in the concentration range of 30-1200 ng/mL. Selectivity, matrix effect and metabolites interference effect were investigated and the method presented no obvious interference effect during the analysis run time. Repeatability, limit of detection (LOD) and limit of quantification (LOQ) values of the method can be reported in this section as well. The method showed satisfactory results with 98.8% relative recovery in the analysis of positive urine samples. The findings convinced the applicability of the introduced method for DSPE and HPLC analysis of the positive urine samples in different laboratories.
本研究引入一种聚合物纳米球作为新型分散固相萃取(DSPE)吸附剂,用于从尿液中萃取哌醋甲酯(MPH)并进行高效液相色谱(HPLC)分析。聚合物纳米球是一种共聚网络,由离子液体单体与苯乙烯在乙烯基三乙氧基硅烷和甲基丙烯酸2-羟乙酯存在下共聚得到。采用配备紫外检测器的HPLC对MPH进行测定和定量。通过一次改变一个参数的方法对萃取中的主要参数进行了优化。结果如下:10 mg聚合物纳米球(PNS)、400 μL乙腈(ACT)、5 mL pH值为9的尿液,萃取时间和洗脱时间分别为2分钟和5分钟,可将其选为最佳萃取条件。通过优化条件绘制校准曲线,并对所提出的方法进行了验证。结果表明,该方法在30 - 1200 ng/mL的浓度范围内呈线性。研究了选择性、基质效应和代谢物干扰效应,该方法在分析运行期间未呈现明显干扰效应。本节还可报告该方法的重复性、检测限(LOD)和定量限(LOQ)值。该方法在分析阳性尿液样本时相对回收率为98.8%,结果令人满意。这些发现证实了所引入的方法适用于不同实验室对阳性尿液样本进行DSPE和HPLC分析。