Химико-токсикологический анализ циталопрама в биологическом материале

Abstract

Разработан эффективный метод выделения циталопрама из биологического материала, учитывающего липофильность исследуемого препарата. Метод основан на элюировании циталопрама из гомогенизированной ткани путем растирания ее с безводным натрия сульфатом и последующей экстракционной очисткой элюатов с помощью системы растворителей гексан–ацетонитрил. Разрешающая способность метода составила 60,0±6,9%.

Citalopram is one of the most-used selective serotonin reuptake inhibitor antidepressants and repeatedly a cause of fatal poisoning. An effective method was developed to isolate citalopram from a biological material, which made allowance for the lipophilicity of the test drug. The method was based on the elution of citalopram from homogenized and dehydrated tissue through its grinding with anhydrous sodium sulfate, followed by the extraction and purification of eluates, by using a hexane-acetonitrile solvent system. The resolving power of the method was 60.0±4.2%. The citalopram isolated from the biological material was identified using color reactions, thin-layer chromatography, ultraviolet (UV) spectroscopy, and high performance liquid chromatography (HPLC) with multiwave UV detection. The content of citalopram in the eluates was estimated by HPLC at 240 nm. By using the standard solutions of citalopram in methanol, the investigators established the calibration relationship of the area of the chromatographic peak (Y) to the concentration (X), which is described by the following equation: Y=2.96•10-3X+7.9•10-4 (r=0.999; S2=4.4•10-7). In addition, they assessed some validation characteristics of the procedure: its linearity range was 2.24 to 100 μg/ml; LOQ = 2.24 μg/ml (criterion 10 σ). The correctness and accuracy of the procedure were (n = 5): the range of low, moderate, and high concentrations was 101.7%; (RSD = 1.8%), 100.4% (RSD = 0.6%), and 100.3% (RSD = 0.8%), respectively.