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采用有机-无机杂化氰丙基整体柱的柱切换液相色谱-串联质谱法分析精神分裂症患者血浆样本中的药物。

Analysis of drugs in plasma samples from schizophrenic patients by column-switching liquid chromatography-tandem mass spectrometry with organic-inorganic hybrid cyanopropyl monolithic column.

作者信息

Domingues Diego Soares, Souza Israel Donizeti de, Queiroz Maria Eugênia Costa

机构信息

Departamento de Química, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, Brazil.

Departamento de Química, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, Brazil.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Jul 1;993-994:26-35. doi: 10.1016/j.jchromb.2015.04.040. Epub 2015 May 5.

DOI:10.1016/j.jchromb.2015.04.040
PMID:25984963
Abstract

This study reports on the development of a rapid, selective, and sensitive column-switching liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to analyze sixteen drugs (antidepressants, anticonvulsants, anxiolytics, and antipsychotics) in plasma samples from schizophrenic patients. The developed organic-inorganic hybrid monolithic column with cyanopropyl groups was used for the first dimension of the column-switching arrangement. This arrangement enabled online pre-concentration of the drugs (monolithic column) and their subsequent analytical separation on an XSelect SCH C18 column. The drugs were detected on a triple quadrupole tandem mass spectrometer (multiple reactions monitoring mode) with an electrospray ionization source in the positive ion mode. The developed method afforded adequate linearity for the sixteen target drugs; the coefficients of determination (R(2)) lay above 0.9932, the interassay precision had coefficients of variation lower than 6.5%, and the relative standard error values of the accuracy ranged from -14.0 to 11.8%. The lower limits of quantification in plasma samples ranged from 63 to 1250pgmL(-1). The developed method successfully analyzed the target drugs in plasma samples from schizophrenic patients for therapeutic drug monitoring (TDM).

摘要

本研究报告了一种快速、选择性和灵敏的柱切换液相色谱-串联质谱(LC-MS/MS)方法的开发,用于分析精神分裂症患者血浆样本中的16种药物(抗抑郁药、抗惊厥药、抗焦虑药和抗精神病药)。所开发的带有氰丙基的有机-无机杂化整体柱用于柱切换装置的第一维。这种装置能够在线预富集药物(整体柱),并随后在XSelect SCH C18柱上进行分析分离。在配备电喷雾电离源的三重四极杆串联质谱仪上以正离子模式的多反应监测模式检测药物。所开发的方法为16种目标药物提供了足够的线性;决定系数(R(2))大于0.9932,批间精密度的变异系数低于6.5%,准确度的相对标准误差值在-14.0%至11.8%之间。血浆样本中的定量下限范围为63至1250pgmL(-1)。所开发的方法成功地分析了精神分裂症患者血浆样本中的目标药物,用于治疗药物监测(TDM)。

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