METHODS OF ZOPICLONE INVESTIGATION IN THE OBJECT OF FORENSIC EXAMINATION
Наукові журнали Тернопільського державного медичного університету імені І.Я.Горбачевського
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METHODS OF ZOPICLONE INVESTIGATION IN THE OBJECT OF FORENSIC EXAMINATION
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Korobchuk, V. M.; Тернопільський державний медичний університет, Тернопіль
Yatsyuk, V. M. Mykhalkiv, M. M. Ivanusa, I. B. |
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METHODS OF ZOPICLONE INVESTIGATION IN THE OBJECT OF FORENSIC EXAMINATIONV. M. Korobchuk1, V. M. Yatsyuk1, M. M. Mykhalkiv2, I. B. Ivanusa2Temopil Scientific and Research Forensic Centre of the Ministry of internal Affairs of Ukraine1Horbachevsky Ternopil State Medical University2Introduction. Zopiclone rapidly induces sleep, without decreasing the proportion of a fast sleep in its structure, and then supports sleep with preservation of normal phase composition. However, Zopiclone is found the non-medical usage. Perhaps drug dependents use zopiclone in the crisis period, or with opiates for the state of euphoria, sometimes in combination with other psychoactive substances.Zopiclone (C17H17ClN6O3) – (5RS)-6-(5-Chloropyridin-2-yl)-7-oxo-6,7-dihydro-5Hpyrrolo[3,4-b]pyrazin-5-yl 4-methylpiperazine-1-carboxylate – is white or slightly yellowish powder, practically insoluble in water, freely soluble in methylene chloride, sparingly soluble in acetone, practically insoluble in ethanol (96 per cent). It dissolves in dilute mineral acids.The most common methods for the qualitative detection of zopiclone are chemical reactions, chromatography in thin layer sorbent (TLC), gas-liquid chromatography (GLC), mass-, infrared (IR) -, ultraviolet (UV)- spectroscopy.Aim of investigation – a generalization of already existing methods for detection and quantitative determination of zopiclone in different objects and develop a new approach to the determination of zopiclone by TLC, GC, IR spectroscopy.Investigation methods. To solve this purpose, we used a sample of medicine "Sonnat zopiclone 0.0075 g", which was taken from the collection of the laboratory department of study materials, substances and products Ternopol scientific and research forensic centre the Ministry of internal Affairs of Ukraine. Identification of zopiclone was performed by chemical (qualitative reactions with Dragendorff’s, Bushard’s, Zonnenstein’s, Nessler’s, Scheibler's, Wagner’s, Marqui's reagents, 2,4-dinitrophenylhydrazine, freshly prepared 1% solution of Reinecke salt, rhodamine cobalt) and physical-chemical (infrared spectroscopy, TLC, GC, GC / MS) methods. IR spectroscopic investigation was performed on spectrophotometer SPECORD M80, the recording spectrum 4000-400 cm-1; integration time - 0.5 seconds; slit width – 12, GLC investigation were performed on chromatograph "HP 6890", GC / MS investigation on chromatograph GC / MS Agilent Technologies 6890N / 5975B.Results and discussion. To identify of zopiclone were used precipitation and color reactions. We observed the formation of the corresponding color precipitate with the precipitation reagent (Dragendorff’s, Bushard’s, Zonnenstein’s, Scheibler's, Wagner’s, etc.). To identify by color reactions were used various reagents recommended for examination of drastic substances (Nessler’s, Marqui's reagents, 2,4-dinitrophenylhydrazine, freshly prepared 1% solution of Reinecke salt, rhodamine cobalt). It has been established, only Nessler’s reagent dives with zopiclone orange color with the transition into gray, is opportunity to differ it from the ketamine, atropine, clophelin, dimedrol.TLC, IR spectroscopy is used in order to confirm quality results of chemical reactions. Chromatographic investigation was first conducted in three solvent systems: benzene - ethanol - triethylamine (9:1:1); chloroform - methanol (9:1) and chloroform - acetone (4:1). As developers are used UV irradiation (green fluorescence) and iodine vapor (light brown stain). Plates are processed by Nessler’s reagent after a complete sublimation of iodine from the surface (orange stain that gradually gray).In infrared spectroscopic investigation the spectrum was obtained with absorption bands characteristic for zopiclone (710, 750, 845, 980, 1090, 1140, 1290, 1380, 1440, 1710 sm-1). For the qualitative and quantitative determination of zopiclone selective method is gas chromatography with GC-MS detection. The obtained mass spectrum was compared with the mass spectrum drastic substances from the mass spectrum library. The comparison determined that the resulting mass spectrum was consistent with the mass spectrum of zopiclone.It was to explore the possibility of quantitative GC-determination of of zopiclone in the test object. Conditions of chromatography: capillary column (length -30 m; diameter -250 mm; phase thickness -0.25 m; constant flow carrier gas through the column - 2.0 ml / min.), carrier gas – helium, injector temperature -280 °C, detector – FID, internal standard – metylstearat, solvent – chloroform, sample volume - 1 mcl. Retention time of zopiclone - 9.949 min.Conclusions. It was research individual qualitative chemical reactions characteristic to identify of zopiclone, prompted to select Nessler’s reagent. It was analyzed and proposed eluent systems for thin-layer-chromatographic investigations. Screening of reagents for zopiclone zones detection after chromatography in a thin layer of sorbent was spend. It is proposed IR-spectroscopic method as a version of zopiclone investigation.A new modern approach to the identification of zopiclone and determination of its amount in the forensic objects is used GC and GC / MS methods. It was analyzed the possibility of application of UV and visible spectral regions, HPLC for the quantitative determination of zopiclone in the investigated objects.References1. Mashkovskiy M.D. Lekarstvennyye sredstva : v 2 t. / M.D. Mashkovskiy. – M., 2012. – T. 1. – 32 s.2. Abuse and dependence potential for the nonbenzodiazepid hipnotics zolpidem and zopiclon: a revier of case reports and epidemiological data / G. Hajak, W. E. Muller, D. Pittow, W. Kirch // Additson. – 2003. – V. 98 (10) - P. 1371–1378.3. Nakaz MOZ Ukrayiny № 490 vid 17.08.2007 “Pro zatverdzhennya Perelikiv otruynykh ta sylʹnodiyuchykh likarsʹkykh zasobiv”, zareyestrovanoho v Ministerstvi yustytsiyi Ukrayiny 03 veresnya 2007 roku za №1008/14275.4. Khimiko-toksikologicheskiy analiz imovana / YU.A. Khomov, N.V. Koksharova, M. Dayyekh, V.P. Garanin // Problemy ekspertizy v meditsine. – 2004. - № 13-1, tom 04. – S. 25-27.5. Bolotov V. V. Rozrobka kolʹorovykh reaktsiy na zopiklon / V. V. Bolotov, L. YU. Klymenko // Zhurnal orhanichnoyi ta farmatsevtychnoyi khimiyi. – 2005. – T. 3. – Vyp. 1 (9). – S. 65-69.6. Bolotov V. V. Vyvchennya metodiv izolyuvannya zopiklonu z ob'yektiv biolohichnoho pokhodzhennya / V. V. Bolotov, L. YU. Klymenko // Visnyk farmatsiyi. – 2006. – № 3 (47). – S. 26 – 30.7. TSKH-skrining toksikologicheski znachimykh soyedineniy, izoliruyemykh ekstraktsiyey i sorbtsiyey / Ramenskaya G.V. [i dr.], pod red. Arzamastseva A.P. //– M.: GEOTAR–Media, 2010. – 240 s.8. Khizhnichenko O.V. Khimiko-toksykolohichne doslidzhennya novykh likarsʹkykh zasobiv – potentsiynykh obʺyektiv nemedychnoho vykorystannya metodom khromatohrafiyi u tonkykh sharakh sorbentu / O.V. Khizhnichenko, N.V. Huzenko, O.V. Chubenko // Farmatsevtychnyy zhurnal. – 2012. – Vyp. 6. – S.74-78.9. Bolotov V. V. Spektrofotometrychne ta ekstraktsiyno-fotometrychne vyznachennya zopiklonu ta produktu yoho luzhnoho hidrolizu – 2-amino-5-khlorpirydynu / V. V. Bolotov, L. YU. Klymenko // Visnyk farmatsiyi. – 2004. – №4 (40). – S. 15 – 19.10. Zahorodniy S. L. Kilʹkisne vyznachennya zopiklonu u tabletkakh «Sonovan» metodom spektrofotometriyi / S. L. Zahorodniy, S. O. Vasyuk // Aktualʹni pytannya farmatsevtychnoyi i medychnoyi nauky ta praktyky. – 2014. – № 2 (15). – S. 23–26.11. Blazheyevskiy M. Ye. Development of the kinetic-spectrophotometric method for quantitative determination of zopiclone in tablets by the perhydrolysis reaction. / M.Ye. Blazheyevskiy, L.S.Kryskiw // Вісник фармації. – 2014. – 3(79). – С. 38-41.
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Тернопільський державний медичний університет ім. І.Я. Горбачевського
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—
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2016-04-07
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info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion — |
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application/pdf
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http://ojs.tdmu.edu.ua/index.php/pharm-chas/article/view/6053
10.11603/2312-0967.2016.1.6053 |
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Pharmaceutical Review; № 1 (2016)
Фармацевтичний часопис; № 1 (2016) 2414-9926 2312-0967 10.11603/2312-0967.2016.1 |
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ukr
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http://ojs.tdmu.edu.ua/index.php/pharm-chas/article/view/6053/5546
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