色谱法
化学
芬戈莫德
高效液相色谱法
固相萃取
萃取(化学)
检出限
吸附
质谱法
解吸
分析化学(期刊)
多发性硬化
精神科
心理学
有机化学
作者
Esra Durgun,Halil İbrahim Ulusoy,İbrahim Narin
标识
DOI:10.1016/j.jchromb.2024.124071
摘要
An analytical methodology has been developed for trace amounts of Fingolimod (FIN) and Citalopram (CIT) drug molecules based on magnetic solid phase extraction (MSPE) and high performance liquid chromatographic determination with photodiode array detector (HPLC-DAD). Fingolimod is used in treatment of Multiple sclerosis (MS) disease and sometimes antidepressant drugs such as citalopram accompany to treatment. Both simultaneous analysis of these molecules and application of MSPE with a new adsorbent has been performed for first times. Fe3O4@L-Tyrosine magnetic particles has been synthetized and characterized as a new magnetic adsorbent. Experimental variables of MPSE were examined and optimized step by step such as pH, adsorption and desorption conditions, time effect, etc. Analytical parameters of the proposed method were studied and determined under optimized conditions according to international guidelines. HPLC analysis of FIN and CIT molecules was performed by isocratic elution of a mixture of 50 % Acetonitrile, 40 % pH:3 phosphate buffer and 10 % methanol with flow rate 1.0 mL min−1. The chosen wavelengths in PDA was determined as 238 nm for FIN and 213 nm for CIT. The limits of detection (LOD) for proposed method were 6.32 ng mL−1 for FIN and 6.85 ng mL−1 for CIT molecules. RSD % values were lower than 5.5 % in analysis of model solutions including 250 and 500 ng mL−1 of target molecules. Recovery values by means of synthetic urine and saliva samples were in the range of 95.7–105.4 % for both molecules.
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