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通过织物相吸附萃取分离和富集芬戈莫德和西酞普兰活性药物成分,随后采用二极管阵列检测的高效液相色谱分析法进行分析。

Separation and enrichment of fingolimod and citalopram active drug ingredients by fabric phase sorptive extraction followed by high performance liquid chromatographic analysis with diode array detection.

作者信息

Durgun Esra, Ulusoy Halil İbrahim, Narin İbrahim, Kabir Abuzar, Locatelli Marcello

机构信息

Department of Analytical Chemistry, Institute of Health Sciences, Erciyes University, Kayseri, Turkiye.

Department of Analytical Chemistry, Faculty of Pharmacy, Sivas Cumhuriyet University, Sivas, Turkiye.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2025 Oct 1;1264:124730. doi: 10.1016/j.jchromb.2025.124730. Epub 2025 Jul 11.

Abstract

Multiple Sclerosis (MS) is a chronic disorder affecting the central nervous system. The treatment of MS often involves a combination of pharmaceutical agents, including Fingolimod (FIN) and Citalopram (CIT). The analysis of these drug compounds plays a crucial role in various stages of health sciences, ranging from drug development to therapeutic monitoring. In this study, a rapid and sensitive analytical method was developed for the trace determination of FIN and CIT using fabric phase sorptive extraction (FPSE) as a sample pretreatment technique, followed by high-performance liquid chromatography coupled with diode array detection (HPLC-DAD). Key FPSE parameters-including pH, adsorption and desorption conditions, and extraction time-were systematically optimized. Analytical performance characteristics of the proposed method were evaluated under optimized conditions in accordance with international guidelines. Chromatographic separation of FIN and CIT was achieved via isocratic elution using a mobile phase composed of acetonitrile, pH 3.0 phosphate buffer, and methanol (50:40:10, v/v/v) at a flow rate of 1.0 mL min. The limits of detection (LOD) for FIN and CIT were determined to be 7.46 ng mL and 5.97 ng mL, respectively. The method demonstrated good precision, with relative standard deviation (RSD) values below 6.0 % for spiked samples. Recovery rates from synthetic urine and saliva matrices ranged between 93.1 % and 105.0 % for both analytes, confirming the method's accuracy and applicability to biological samples.

摘要

多发性硬化症(MS)是一种影响中枢神经系统的慢性疾病。MS的治疗通常涉及多种药物联合使用,包括芬戈莫德(FIN)和西酞普兰(CIT)。这些药物化合物的分析在健康科学的各个阶段都起着至关重要的作用,从药物开发到治疗监测。在本研究中,开发了一种快速灵敏的分析方法,采用织物相吸附萃取(FPSE)作为样品预处理技术,随后结合二极管阵列检测的高效液相色谱法(HPLC-DAD)对FIN和CIT进行痕量测定。系统优化了关键的FPSE参数,包括pH值、吸附和解吸条件以及萃取时间。根据国际指南在优化条件下评估了该方法的分析性能特征。通过等度洗脱实现FIN和CIT的色谱分离,流动相由乙腈、pH 3.0的磷酸盐缓冲液和甲醇(50:40:10,v/v/v)组成,流速为1.0 mL/min。FIN和CIT的检测限分别确定为7.46 ng/mL和5.97 ng/mL。该方法具有良好的精密度,加标样品的相对标准偏差(RSD)值低于6.0%。两种分析物在合成尿液和唾液基质中的回收率在93.1%至105.0%之间,证实了该方法的准确性和对生物样品的适用性。

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