胶束电动色谱-紫外检测法测定血浆中亚甲基蓝及其去甲基化代谢物

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis Pub Date : 2025-09-23 DOI:10.1016/j.jpba.2025.117155

Alexander Vladimirovich Ivanov , Valery Vasil’evich Aleksandrin , Polina Alexandrovna Pudova , Maria Pavlovna Galdobina , Alexander Gennadievich Filippov , Mikhail Aleksandrovich Popov , Ruslan Andreevich Maslennikov , Aslan Amirkhanovich Kubatiev

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引用次数: 0

摘要

建立了一种基于MEKC直接测定血浆中药物亚甲基蓝（MB）的新方法。我们采用乙腈和二氯甲烷液相萃取和强阳离子交换吸附剂固相萃取的方法从基质中提取分析物。使用紫外检测(292 海里)和50μm内直径石英毛细管的总长度38 厘米(31.5 厘米有效)满40 mM磷酸Na, SDS 150毫米,5 % (v / v)异丙醇,和12 % (v / v)正丁醇(pH值2.06),5.8 ng / mL的LOD MB和 总分析时间16.5分钟。准确度为97.4 ~ 103 %，日内、日间不精密度分别为5.7、2.5 %。该方法在注射了MB的大鼠的血液样本上进行了测试。所开发的方法还允许检测去甲基化MB代谢物（蓝色A和蓝色B），并适用于器官（脑，肝脏和肾脏）的分析。

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Determination of methylene blue and detection of its demethylated metabolites in blood plasma using micellar electrokinetic chromatography with UV detection

A new approach to the direct determination of the drug methylene blue (MB) in blood plasma was developed based on MEKC. We used liquid-phase extraction with acetonitrile and dichloromethane and solid-phase extraction on a strong cation exchange sorbent to extract the analyte from the matrix. Using UV detection (292 nm) and a 50 μm internal diameter silica capillary with a total length of 38 cm (31.5 cm effective) filled with 40 mM phosphate Na, 150 mM SDS, 5 % (v/v) isopropanol, and 12 % (v/v) n-butanol (pH 2.06), an LOD of 5.8 ng/mL for MB and a total analysis time of 16.5 min were obtained. The accuracy was 97.4–103 %, and intra- and interday imprecision were 5.7 and 2.5 %, respectively. This approach was tested on blood samples from rats that were injected with MB. The developed approach also allows for the detection of demethylated MB metabolites (azure A and azure B) and is suitable for the analysis of organs (the brain, liver, and kidneys).

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来源期刊

Journal of pharmaceutical and biomedical analysis 医学-分析化学

CiteScore

6.70

自引率

5.90%

发文量

588

审稿时长

37 days

期刊介绍： This journal is an international medium directed towards the needs of academic, clinical, government and industrial analysis by publishing original research reports and critical reviews on pharmaceutical and biomedical analysis. It covers the interdisciplinary aspects of analysis in the pharmaceutical, biomedical and clinical sciences, including developments in analytical methodology, instrumentation, computation and interpretation. Submissions on novel applications focusing on drug purity and stability studies, pharmacokinetics, therapeutic monitoring, metabolic profiling; drug-related aspects of analytical biochemistry and forensic toxicology; quality assurance in the pharmaceutical industry are also welcome. Studies from areas of well established and poorly selective methods, such as UV-VIS spectrophotometry (including derivative and multi-wavelength measurements), basic electroanalytical (potentiometric, polarographic and voltammetric) methods, fluorimetry, flow-injection analysis, etc. are accepted for publication in exceptional cases only, if a unique and substantial advantage over presently known systems is demonstrated. The same applies to the assay of simple drug formulations by any kind of methods and the determination of drugs in biological samples based merely on spiked samples. Drug purity/stability studies should contain information on the structure elucidation of the impurities/degradants.