Development of methods for the study of dicyclomine hydrochloride in combination with paracetamol as an object of forensic-pharmaceutical examination

Abstract

The aim. Selection and development of methods for the tasks of forensic pharmaceutical examination as case materials suspected of falsification or non-medical use of dicyclomine hydrochloride in combination with paracetamol in the form of tablets. Materials and methods. The study presents the developed methods of detection and identification of dicyclomine by TLC, IR spectroscopy and GC-MS, which were performed using reagents that meet the EP, USP and USPU requirements, Class A glassware and qualified devices. Identification by IR spectroscopy was performed in the range from 500 to 4000 cm-1 on the device “Nicolet 380 FT-IR Spectrometer by Thermo Fisher Scientific”. TLC was performed on Sorbfil plates for TLC-PET-H-UV and Sorbfil plates for TLC-AF-UV (CJSC “Sorbpolymer”, Russia). The following systems were used as mobile phases: dioxane-chloroform-acetone-25 % ammonia solution (47.5:45:5:2.5); toluene-acetone-ethanol-25 % ammonia solution (45:45:7.5:2.5); ethyl acetate-methanol-25 % ammonia solution (17:2:1)). The resulting chromatographic zones were detected by irradiation with UV light and further treatment with color reagents (30 % iron (III) chloride solution; Dragendorff's reagent modified by Munier; Marquis reagent; Froehde reagent; Mandelin reagent; FPN reagent). Analysis by gas chromatography with mass detection was performed using a gas chromatograph with a mass spectrometric detector GCMS-QP2020. Data were analyzed using the program: GCMSsolution, LabSolutions Insight (Shimadzu Corporation, Tokyo, Japan). Results. For the first time, the conditions for the extraction of dicyclomine hydrochloride from aqueous solutions were studied and the optimal conditions for their isolation as an object of forensic pharmaceutical examination is defined. The method of detection of dicyclomine hydrochloride and paracetamol in the drug “Trigan-D” by the methods of thin-layer chromatography, gas-liquid chromatography and chromato-mass spectrometry was developed, and the detection limits of the substances under study were determined. Conclusion. The developed methods for dicyclomine hydrochloride in the form of tablets with paracetamol meet the requirements of the current legislation of Ukraine and the Ministry of Justice of Ukraine. The data obtained prove the high sensitivity and reproducibility of the methods and prove the possibility of their introduction into the practice of forensic pharmaceutical examination