Investigation of Conditions for the Extraction of Medicinal Preparations from Hair and Their Analysis by Means of Gas Chromatography-Mass Spectrometry
YA. YU. KISLYAKOVA, T. F. SHASHKO, YU. M. SEROV
Russian University of Peoples' Friendship, Ul. Miklukho-Maklaya 8, build. 1, Moscow119571 (Russia)
Keywords: анализ волос, ГХ-МС, амитриптилин, карбамазепин, щелочной гидролиз, analysis of hair, GC-MS, amitriptyline, carbamazepine, alkaline hydrolysis
Abstract
For medical preparations of antidepressant class (amitriptyline, carbamazepine) as examples, experimental evaluation of the dependence of extraction extent on the parameters of alkaline destruction (concentration of potassium hydroxide, hydrolysis temperature, exposure) and organic solvent used to extract the target substances from hair hydrolyzate was carried out.. Relying on the results of the studies, a universal method of hair sample preparation within chemical toxicological analysis was proposed: hydrolysis of the sample in a 1.5 M KOH solution at 60 °C for 1.5 h, subsequent extraction with a mixture of hexane with ethyl acetate at the volume ratio of 5 : 1. The parameters of gas chromatographic-mass spectrometric detection of the target substances were optimized. A procedure for the analysis of amitriptyline and carbamazepine in hair by means of GC-MS was developed. Validation of this procedure was carried out, the working range of the procedure was determined to be 1-100 ng/mg; detection limits for amitriptyline and carbamazepine were determined to be 0.5 and 1 ng/mg, respectively. This procedure was successfully tested with heal hair samples.
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