DETERMINATION AND METHOD VALIDATION OF HEROIN, MORPHINE, CODEINE AND 6-MONOACETYLMORPHINE BY GC-FID

Öz

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 Dichloromethaneisopropylalcohol 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 also found very important by the courts. For this reason validation and continual reclamation of methods that have been used in forensic laboratories is getting very important.

Anahtar Kelimeler

• Laboratory
• Quality
• Validation
• Forensic

Kaynakça

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