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采用胶束液相色谱-电化学检测法测定血液和尿液中的帕罗西汀。

Determination of paroxetine in blood and urine using micellar liquid chromatography with electrochemical detection.

作者信息

Agrawal Nitasha, Marco-Peiró Sergio, Esteve-Romero Josep, Durgbanshi Abhilasha, Bose Devasish, Peris-Vicente Juan, Carda-Broch Samuel

机构信息

Department of Criminology and Forensic Sciences, Dr. H.S. Gour University, Sagar, India.

Àrea de Química Analítica, Universitat Jaume I, Castelló 12071, Spain.

出版信息

J Chromatogr Sci. 2014 Nov-Dec;52(10):1217-23. doi: 10.1093/chromsci/bmt200. Epub 2014 Jan 20.

DOI:10.1093/chromsci/bmt200
PMID:24448669
Abstract

Paroxetine is a potent selective serotonin reuptake inhibitor used for the treatment of depression and related mood disorders. A micellar liquid chromatographic method was developed for the determination of paroxetine in serum and urine. Detection of paroxetine was carried out using a C18 column and a mobile phase of 0.15 M sodium dodecyl sulfate, 6% 1-pentanol at pH 3 (buffer salt 0.01 M NaH2PO4) running under isocratic mode at 1.0 mL/min and electrochemical detection at 0.8 V. The analyte was eluted without interferences in <15 min. The proposed methodology was validated under the guidelines of the International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use in matrix in terms of specificity, linearity (r(2) > 0.9999; 0.5-5 μg/mL range), accuracy (88-97.5%, recovery), repeatability (RSD < 0.54%), intermediate precision (RSD < 0.54%), limit of detection and quantification (0.001 and 0.005 μg/mL, respectively) and robustness (RSD < 3.63%). Developed method was successfully applied to real blood and urine samples as well as in spiked serum and urine samples. The developed method was specific, rapid, precise, reliable, accurate, inexpensive and then suitable for routine analysis of paroxetine in monitorized samples.

摘要

帕罗西汀是一种强效的选择性5-羟色胺再摄取抑制剂,用于治疗抑郁症及相关情绪障碍。已开发出一种胶束液相色谱法用于测定血清和尿液中的帕罗西汀。使用C18柱和流动相进行帕罗西汀的检测,流动相为0.15 M十二烷基硫酸钠、6% 1-戊醇,pH值为3(缓冲盐为0.01 M NaH2PO4),在等度模式下以1.0 mL/min流速运行,并在0.8 V下进行电化学检测。分析物在不到15分钟内洗脱且无干扰。所提出的方法按照人用药品注册技术要求国际协调会议的指导原则在基质中进行了验证,验证内容包括特异性、线性(r(2) > 0.9999;0.5 - 5 μg/mL范围)、准确度(88 - 97.5%,回收率)、重复性(RSD < 0.54%)、中间精密度(RSD < 0.54%)、检测限和定量限(分别为0.001和0.005 μg/mL)以及稳健性(RSD < 3.63%)。所开发的方法成功应用于实际血液和尿液样本以及加标血清和尿液样本。该方法具有特异性、快速、精确、可靠、准确、成本低的特点,适用于监测样本中帕罗西汀的常规分析。

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