Departamento de Química, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, 14040-901 Ribeirão Preto, SP, Brazil.
Molecules. 2019 Jan 16;24(2):310. doi: 10.3390/molecules24020310.
This manuscript describes a sensitive, selective, and online in-tube solid-phase microextraction coupled with an ultrahigh performance liquid chromatography-tandem mass spectrometry (in-tube SPME-UHPLC-MS/MS) method to determine chlopromazine, clozapine, quetiapine, olanzapine, and their metabolites in plasma samples from schizophrenic patients. Organic poly(butyl methacrylate-co-ethylene glycol dimethacrylate) monolith was synthesized on the internal surface of a fused silica capillary (covalent bonds) for in-tube SPME. Analyte extraction and analysis was conducted by connecting the monolithic capillary to an UHPLC-MS/MS system. The monolith was characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectrometry (FTIR). The developed method presented adequate linearity for all the target antipsychotics: R² was higher than 0.9975, lack-of-fit ranged from 0.115 to 0.955, precision had variation coefficients lower than 14.2%, and accuracy had relative standard error values ranging from -13.5% to 14.6%, with the exception of the lower limit of quantification (LLOQ). The LLOQ values in plasma samples were 10 ng mL for all analytes. The developed method was successfully applied to determine antipsychotics and their metabolites in plasma samples from schizophrenic patients.
本文描述了一种灵敏、选择性强且在线的管内固相微萃取与超高效液相色谱-串联质谱（in-tube SPME-UHPLC-MS/MS）联用方法，用于测定精神分裂症患者血浆样品中的氯丙嗪、氯氮平、喹硫平、奥氮平和它们的代谢物。有机聚（甲基丙烯酸丁酯-co-乙二醇二甲基丙烯酸酯）整体柱在熔融石英毛细管的内表面上合成（共价键），用于管内 SPME。通过将整体毛细管连接到 UHPLC-MS/MS 系统来进行分析物的萃取和分析。通过扫描电子显微镜（SEM）和傅里叶变换红外光谱（FTIR）对整体柱进行了表征。所开发的方法对所有目标抗精神病药物均具有足够的线性：R²均高于 0.9975，失拟度范围为 0.115 至 0.955，精密度的变异系数低于 14.2%，准确度的相对标准误差值在-13.5%至 14.6%之间，除了定量下限（LLOQ）。所有分析物在血浆样品中的LLOQ 值均为 10 ng/mL。该方法成功应用于测定精神分裂症患者血浆样品中的抗精神病药物及其代谢物。
