Departamento de Química, Universidade Federal de Santa Catarina, Florianópolis 88040900, SC, Brazil.
Departamento de Farmacociências, Universidade Federal de Ciências da Saúde de Porto Alegre, Porto Alegre 90050170, RS, Brazil.
J Chromatogr B Analyt Technol Biomed Life Sci. 2020 Apr 15;1143:122069. doi: 10.1016/j.jchromb.2020.122069. Epub 2020 Mar 19.
In this study, the use of switchable hydrophilicity solvent with a simple and low-cost lab-made device for the extraction procedure in homogeneous liquid-liquid microextraction is proposed for the first time in the determination of antidepressants in human urine. The antidepressants studied consisted of fluoxetine, amitriptyline, nortriptyline, imipramine, desipramine and sertraline. The optimization of the main parameters that can influence on the extraction efficiency was performed through multivariate approaches. The analytes were separated and identified by gas chromatography coupled to mass spectrometry (GC-MS). The optimal extraction conditions consisted of using N,N-dimethylcyclohexylamine (DMCHA) as the switchable hydrophilicity solvent (SHS), 500 µL of urine sample previously diluted with ultrapure water at 1:1 ratio (v/v), 200 μL of a mixture of SHS:HCl 6 mol L (1:1 v/v), 600 μL of NaOH 10 mol L and 3 min of extraction time. A volume of 40 µL of diphenylamine at concentration of 500 µg L (20 ng) was used as internal standard. The method developed was in-house validated, providing coefficients of determination higher than 0.995 for all analytes, limits of detection (LOD) from 0.02 to 0.88 µg L, limits of quantification (LOQ) from 0.05 to 2.92 µg L, relative recoveries of 68 to 102%, intra-day precision from 0.5 to 15.9%, inter-day precision from 4.2 to 19.3%, selectivity and robustness. The method proposed was successfully applied in five human urine samples from a Toxicological Information Center located in Porto Alegre (Brazil). The results demonstrated that the µP-SHS-HLLME approach is highly cost-effective, rapid, simple and environmentally-friendly with satisfactory analytical performance.
在这项研究中，首次提出了使用具有简单、低成本实验室制造设备的可切换亲水性溶剂，用于均相液-液微萃取中的提取程序，以测定人尿中的抗抑郁药。所研究的抗抑郁药包括氟西汀、阿米替林、去甲替林、丙咪嗪、去甲丙咪嗪和舍曲林。通过多元方法对可能影响萃取效率的主要参数进行了优化。采用气相色谱-质谱联用（GC-MS）对分析物进行分离和鉴定。最佳萃取条件为使用 N,N-二甲基环己胺（DMCHA）作为可切换亲水性溶剂（SHS），尿液样品 500µL 与超纯水按 1:1 比例（v/v）稀释，200µL SHS：HCl 6mol/L（1:1 v/v）混合物，600µL NaOH 10mol/L，萃取时间 3min。使用浓度为 500µg/L（20ng）的二苯胺 40µL 作为内标。所开发的方法经过内部验证，所有分析物的相关系数均高于 0.995，检测限（LOD）为 0.02-0.88µg/L，定量限（LOQ）为 0.05-2.92µg/L，相对回收率为 68-102%，日内精密度为 0.5-15.9%，日间精密度为 4.2-19.3%，选择性和稳健性。该方法成功应用于来自位于阿雷格里港（巴西）的毒理学信息中心的五个人类尿液样本。结果表明，µP-SHS-HLLME 方法具有成本效益高、快速、简单、环保的特点，具有令人满意的分析性能。
