Journal
JOURNAL OF PHARMACOLOGICAL AND TOXICOLOGICAL METHODS
Volume 108, Issue -, Pages -Publisher
ELSEVIER SCIENCE INC
DOI: 10.1016/j.vascn.2021.106949
Keywords
Biological samples; Chloroquine phosphate; Liquid phase microextraction; Magnetic solid phase extraction
Categories
Funding
- Health Institutes of Turkey (TUSEB) [2020CV01-8946]
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The VA-SFDF-LPME method was developed for determining trace levels of chloroquine phosphate in human samples, showing higher extraction efficiency compared to other methods. Optimization studies were conducted to determine the best extraction parameters.
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 ?g/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).
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