Department of Chemistry, Faculty of Art and Science, Yıldız Technical University, Davutpasa, Esenler, Istanbul 34210, Turkey.
Department of Chemistry, Faculty of Art and Science, Yıldız Technical University, Davutpasa, Esenler, Istanbul 34210, Turkey; Turkish Academy of Sciences (TÜBA), Piyade Street No: 27, Çankaya, Ankara 06690, Turkey.
J Pharmacol Toxicol Methods. 2021 Mar-Apr;108:106949. doi: 10.1016/j.vascn.2021.106949. Epub 2021 Jan 24.
A vortex assisted spraying based fine droplet formation liquid phase microextraction (VA-SFDF-LPME) method was developed to determine chloroquine phosphate at trace levels in human serum, urine and saliva samples by gas chromatography-mass spectrometry (GC-MS) with single quadrupole mass analyzer. In the first part, several liquid phase microextraction (LPME) and magnetic solid phase extraction (MSPE) methods were compared to each other in order to observe their extraction ability for the analyte. VA-SFDF-LPME method was selected as an efficient and easy extraction method due to its higher extraction efficiency. Optimization studies were carried out for the parameters such as extraction solvent type, sodium hydroxide volume/concentration, sample volume, spraying number and mixing type/period. Tukey's method based on post hoc test was applied to all experimental data for the selection of optimum values. Optimum extraction parameters were found to be 12 mL initial sample volume, two sprays of dichloromethane, 0.75 mL of 60 g/kg sodium hydroxide and 15 s vortex. Under the optimum conditions, limit of detection and quantification (LOD and LOQ) were calculated as 2.8 and 9.2 μg/kg, respectively. Detection power of the GC-MS system was increased by approximately 317 folds with the developed extraction/preconcentration method. The applicability and accuracy of the proposed method was evaluated by spiking experiments and percent recovery results for human urine, serum and saliva samples were found in the range of 90.9% and 114.0% with low standard deviation values (1.9-9.4).
基于涡旋辅助喷雾的液相比色微萃取（VA-SFDF-LPME）方法结合气相色谱-质谱（GC-MS）联用仪的单四极杆质量分析器，被用于测定痕量人血清、尿液和唾液中磷酸氯喹。在第一部分，比较了几种液相微萃取（LPME）和磁固相萃取（MSPE）方法，以观察它们对分析物的萃取能力。由于其更高的萃取效率，VA-SFDF-LPME 方法被选为一种高效且简单的萃取方法。对萃取溶剂类型、氢氧化钠体积/浓度、样品体积、喷雾次数和混合类型/周期等参数进行了优化研究。基于事后检验的 Tukey 法被应用于所有实验数据以选择最佳值。最佳萃取参数为初始样品体积 12 mL，二氯甲烷喷雾两次，60 g/kg 氢氧化钠 0.75 mL，涡旋 15 s。在最佳条件下，检测限和定量限（LOD 和 LOQ）分别计算为 2.8 和 9.2 μg/kg。通过开发的萃取/预浓缩方法，GC-MS 系统的检测能力提高了约 317 倍。通过加标实验评估了该方法的适用性和准确性，人尿液、血清和唾液样品的回收率在 90.9%至 114.0%之间，标准偏差值较低（1.9-9.4）。
