薄层色谱和质谱法检测尿中托莫西汀及其代谢物

S. A. Karpushyna, S. V. Baiurka, T. Tomarovska
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引用次数: 0

摘要

本研究的目的是在TLC筛选条件下检测尿中托莫西汀及其生物转化产物,并用质谱法鉴定代谢产物。材料和方法。研究了志愿者在服用单次治疗剂量的阿托西汀(Strattera®2粒胶囊,每粒60毫克)后的尿液样本。样品制备包括稀释酸水解,然后从pH为11-12的硫酸铵饱和溶液中用氯仿提取天然化合物和代谢物。薄层色谱对提取物进行了18个流动相的研究,其中包括国际法医毒理学家协会提出的用于一般药物筛选的流动相和广泛用于法医毒理学研究的流动相。用一系列显色试剂进行显色反应。采用荷兰瓦里安1200 L质谱仪,配双四极杆质谱仪对色谱洗脱液进行分析。在直接将样品引入离子室、电子冲击电离(70 eV)和全离子扫描模式下进行鉴定。用Rf值对色谱上的原生药点进行识别。通过质谱中分子离子峰对应的分子量对两种托莫西汀生物转化产物进行了鉴定。在TLC筛选条件下检测尿中托莫西汀及其生物转化产物,并用质谱法进行鉴定。确定了天然化合物、羟基托莫西汀和二羟基托莫西汀在TLC筛选系统中的色谱迁移率,以及在系统毒理学分析中用于毒理学药物筛选的显色试剂对它们的可视化结果。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Detection of atomoxetine and its metabolites in the urine by thin-layer chromatography and mass spectrometry
The aim of the study was the detection of atomoxetine and its biotransformation products in the urine under TLC screening conditions and identification of the metabolites using mass spectrometry method. Materials and methods. The volunteer’s urine samples after taking a single therapeutic dose of atomoxetine (2 capsules of 60 mg each of Strattera®) were studied. Sample preparation included diluting acid hydrolysis followed by the native compound and metabolites extraction with chloroform from the saturated solution of ammonium sulfate at pH of 11–12. Thin-layer chromatography studies of the extracts were carried out in 18 mobile phases including those proposed by The International Association of Forensic Toxicologists for general drug screening, and those widely used in forensic toxicological studies. The color reactions were carried out using a range of chromogenic reagents. A Varian 1200 L mass spectrometer (Netherlands) equipped with a dual quadrupole mass analyzer was applied for analysis of the eluates from chromatograms. Identification was undertaken at the direct introduction of the sample into the ion chamber, electron-impact ionization (70 eV), and full ion scanning mode. Results. The spot of the native drug on the chromatogram was identified by the Rf, value. Two atomoxetine biotransformation products were identified by the molecular weights that correspond to the molecular ion peaks in the mass spectra. Conclusions. Atomoxetine and its biotransformation products were detected in the urine under TLC screening conditions and identified using mass spectrometry method. Chromatographic mobility of the native compound, hydroxyatomoxetine, and dihydroxyatomoxetine in the TLC screening systems as well as the results of their visualization using chromogenic reagents applied for toxicological drug screening in the systematic toxicological analysis have been determined.
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