This work focused on the development and validation of a method based on hollow fiber-based solid-phase microextraction coupled to ultra-performance liquid chromatography tandem mass spectrometry (HF-based-SPME-UPLC-MS/MS) for the determination of five antipsychotics at a pg mL-1 level in human whole blood and urine. Four types of hollow fiber membrane materials, including polyether sulfone, polypropylene, polyvinyl chloride and polyvinylidene fluoride were investigated. Finally, polyether sulfone hollow fiber without any modification was selected as the adsorption medium for solid-phase microextraction (SPME) with the following extraction procedure: the analytes were adsorbed onto the hollow fiber in the sample bottle with application of ultrasonication. Subsequently, the hollow fiber was transferred into a slim glass tube containing an appropriate solvent, and the analytes were desorbed by ultrasound treatment before detection by UPLC-MS/MS. In order to obtain satisfactory extraction efficiency, extraction parameters such as hollow fiber membrane material, pH, hollow fiber length, extraction time, desorption solvent and desorption time were investigated. Under the optimum experimental conditions, this method allowed for determination of five antipsychotics in human whole blood with excellent limits of quantification (LOQs) (25.0, 12.5, 25.0, 25.0 and 12.5 pg mL-1 for perphenazine, chlorpromazine, chlorprothixene, promethazine and trifluoperazine, respectively). The corresponding LOQs in human urine were 25.0, 12.5, 12.5, 12.5 and 12.5 pg mL-1 for the respective antipsychotics. The precision (RSD) was no more than 13.3%. The extraction recoveries for human whole blood and urine were in the range of 46.4-96.6% and 65.2-101.9%, respectively. The proposed method was compared with other methods from the literature and the results demonstrate that it is a simple, sensitive, efficient and green technique. It is suitable for analyzing trace target analytes in complex matrices such as biological samples and can provide a reliable tool for drug monitoring especially in forensic analysis and case of drug abuse.

中文翻译：

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开发一种基于中空纤维的固相微萃取方法，然后用超高效液相色谱-串联质谱法测定人全血和尿液中的五种抗精神病药。

这项工作的重点是开发和验证基于中空纤维的固相微萃取结合超高效液相色谱串联质谱法（HF-based-SPME-UPLC-MS / MS）来测定五种抗精神病药的方法在人类全血和尿液中的浓度为pg mL-1。研究了四种中空纤维膜材料，包括聚醚砜，聚丙烯，聚氯乙烯和聚偏二氟乙烯。最后，采用以下萃取步骤，选择未经任何改性的聚醚砜中空纤维作为固相微萃取（SPME）的吸附介质：通过超声处理将分析物吸附到样品瓶中的中空纤维上。后来，将中空纤维转移到装有适当溶剂的细玻璃管中，然后在通过UPLC-MS / MS检测之前，先通过超声处理使分析物脱附。为了获得令人满意的提取效率，研究了中空纤维膜材料，pH，中空纤维长度，提取时间，解吸溶剂和解吸时间等提取参数。在最佳实验条件下，该方法可测定人全血中的五种抗精神病药，具有极好的定量限（LOQ）（奋乃静，氯丙嗪，氯丙噻吩，异丙嗪和三氟拉嗪的定量分别为25.0、12.5、25.0、25.0和12.5 pg mL-1 ， 分别）。对于相应的抗精神病药，人尿中相应的LOQ为25.0、12.5、12.5、12.5和12.5 pg mL-1。精度（RSD）不超过13.3％。人全血和尿液的提取回收率分别为46.4-96.6％和65.2-101.9％。将该方法与文献中的其他方法进行了比较，结果表明该方法是一种简单，灵敏，高效且绿色的技术。它适用于分析复杂基质（例如生物样品）中的痕量目标分析物，并且可以提供可靠的药物监控工具，尤其是在法医分析和药物滥用案例中。