Mesut ŞAHİN, Gürol BERBER, Muhammet Nabi KANTARCI, Neval BERBER, Eyüp KANDEMİR

Determination and method validation of heroin, morphine, codeine ve 6-monoacetylmorphine by GC-FID

AMAÇ: Bu çalışmamızda GC/FID cihazı ile uyuşturucu örneklerinde eroin (diasetilmorfin), morfin, kodein ve 6 asetilmorfin’in kantitatif tayini için kullanılan metodun validasyonu yapılmıştır. YÖNTEMLER: Çalışmamızda GC/FID Agilent 6890N cihazı ve Chemstation yazılımı, non polar yapıda %5 fenilmetilpolisiloksan analitik kolonu (DB-5: 10,0m x 100 µm x 0,17 µm) kullanıldı. Kullanılan standart madde ve solusyonlar ise Diklorometan-isopropilalcol (1: 1), Metanol, EroinHCl.H2O, KodeinHCI, MorfinHCI, 6-MonoasetilmorfinHCI, Parasetamol, kafein and n-dokosan referans ve internal standart olarak kullanılmıştır. Metodumuzda taşıyıcı gaz olarak Helyum kullanılmıştır. Enjeksiyon sıcaklığı 280 ˚C ve enjeksiyon hacmi 1 µl’dir. Tekrarlanabilirlik çalışması 4 operatör ile yeniden üretilebilirlik çalışması 3 operatör ile 29 gün için hesaplandı.BULGULAR: Çalışmamızda eroin (0.01-2.00mg mL-1), kodein (0,008-2 mg L-1), 6MAM (0,005-2 mg mL-1) ve morfin (0.015-0,75mg mL-1) için metot tüm dağılım boyunca lineer bulunmuştur. Korelasyon katsayıları 0.997 ve 0.999 arasında değişmektedir.SONUÇ: İnsan hakları talebindeki artışlar, özel sigortaların yaygınlaşması ile özellikle adli disiplinlerde olmak üzere toplam kalite prensiplerinin uygulamasını zorunlu hale getirmiştir. Güvenilirlik ve itibar mahkemelerce de önemli bulunmaktadır. Bu sebeple adli laboratuarlarda kullanılan metotların validasyonu ve devamlı iyileştirmesi oldukça önem kazanmaktadır.

GC-FID ile eroin, morfin, kodein ve 6-monoasetilmorfin tayini ve metodun validasyonu

OBJECTIVE: This study describes the development and validation of a gas chromatography–flame ionization detection (GC–FID) method for the quantitative heroin (diacetylmorphine), morphine, codeine (3-methylmorphine) and 6-monoacetylmorphine (6 MAM) in narcotics.METHODS: In our study, GC/FID Agilent 6890N (DB-5: 10,0m x 100 µm x 0,17 µm) with Chemstation software and 5% phenylmethylpolysiloxane non polar analytic colon (max 325 °C) was used for the analyses. Standards and reagents were Dichloromethane-isopropylalcohol mixture (1: 1), Methanol, HeroinHCl.H2O, CodeineHCI, MorphineHCI, 6-MonoacetylmorphineHCI, Paracetamol, caffeine and n-docosane which were used as reference standard and internal standard. Carrier gas was Helium. Injection temperature (T) was 280 ˚C, injection volume was 1 µl. Repeatability study was evaluated using 4 operators. Reproducibility study was evaluated using 3 operators during 29 days.RESULTS: The method is linear over the range (0.01-2.00mg mL-1) for heroin, (0,008-2 mg L-1) for codeine, (0,005-2 mg mL-1) for 6-monoacetylmorphine and (0.015-0,75mg mL-1) for morphine in the study. Correlation coefficients vary between 0.997 and 0.999 are detected. CONCLUSION: The increases in demanding of human rights, in getting prevalent of special insurances make it obligatory to perform total quality principles particularly for forensic disciplines. Reliability and credibility are found very important also by the courts. For this reason validation and continual reclamation of methods that have been used in forensic laboratories is getting very important.

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