A novel method for deducing the origins of heroin and the reagent used for acetylization was established based on δ13C determinations of heroin and its hydrolysate, morphine, using gas chromatography 13C isotope ratio mass spectrometry (GC-C-IRMS). The alkaline and acid hydrolysis conditions of heroin were optimized. Both yield and purity of morphine produced could meet the requirement for a GC-C-IRMS analysis. Using (2-diethylaminoethyl-2,2- diphenylvalerate) as internal standard the determinations of heroin and morphine contents were performed with a GC method in a linear range of 0.2 to 2.0 mg mL−1 that was required to gain the isotope ratio results. The hydrolysis and synthesis of heroin did not change the δ13C value of morphine. The precision for δ13C detection of both heroin and morphine was sufficient for origin differentiation of heroin samples. The information about the origins of acetylation regents could be deduced from the difference of δ13C values between heroin and morphine. The results for origin differentiation of ten heroin samples grouped into different regions and their acetylating agents were satisfactory.
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