Laboratory of Pharmaceutical Analysis, Department of Pharmacy, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece.
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki 54124, Greece.
J Chromatogr B Analyt Technol Biomed Life Sci. 2024 Mar 1;1235:124060. doi: 10.1016/j.jchromb.2024.124060. Epub 2024 Feb 23.
Clomipramine (CLP) is a tricyclic antidepressant drug, and its determination in biological samples is of high importance in clinical and forensic evaluations to assure appropriate drug concentrations. In the present study, benzoic acid was employed as a pH-switchable hydrophilicity solvent (SHS) for the microextraction of CLP from authentic human urine samples prior to its determination by high performance liquid chromatography-ultraviolet detection (HPLC-UV). The microextraction protocol was based on the phase transition of the SHS through pH alteration that resulted in its rapid dispersion and simultaneous phase separation. The obtained solid was collected in a syringe filter, dissolved in methanol, and analyzed. The main parameters that affected the efficiency of the microextraction procedure were studied and optimized to ensure high extraction efficiency for CLP and the analytical method was validated. Under optimum conditions, good linearity was observed between 0.05 and 5.0 μg mL. The limit of detection and limit of quantification were found to be 0.015 and 0.05 μg mL, respectively. The RSD values for intra-day repeatability and inter-day precision were 2.4-8.9 % and 1.7-9.1 %, respectively. The relative recovery values were within 90.0 and 110.0 % in all cases, demonstrating good method accuracy. The proposed SHS microextraction showed cost-efficiency, handling simplicity, and rapidity resulting in enhanced sample throughput. Moreover, the proposed method exhibited a green character and good applicability based on its evaluation by Green Analytical Procedure Index and Blue Applicability Grade Index.
氯米帕明(CLP)是一种三环类抗抑郁药,其在生物样品中的测定对于临床和法医评估中确保适当的药物浓度非常重要。在本研究中,苯甲酸被用作 pH 可切换亲水性溶剂(SHS),用于从真实的人类尿样中微萃取 CLP,然后通过高效液相色谱-紫外检测(HPLC-UV)进行测定。微萃取方案基于 SHS 通过 pH 变化的相转变,导致其快速分散和同时相分离。所得固体用注射器过滤器收集,溶解在甲醇中并进行分析。研究并优化了影响微萃取过程效率的主要参数,以确保 CLP 的高萃取效率,并对分析方法进行了验证。在最佳条件下,在 0.05 和 5.0 μg mL 之间观察到良好的线性关系。检测限和定量限分别为 0.015 和 0.05 μg mL。日内重复性和日间精密度的 RSD 值分别为 2.4-8.9%和 1.7-9.1%。在所有情况下,相对回收率均在 90.0%和 110.0%之间,表明方法具有良好的准确性。所提出的 SHS 微萃取具有成本效益、操作简单和快速的特点,从而提高了样品通量。此外,根据其对绿色分析程序指数和蓝色适用性等级指数的评估,该方法具有绿色特性和良好的适用性。