Methodology has been developed which utilizes static headspace-gas chromatography-mass spectrometry (SHS-GC-MS) to identify and quantitate residual solvents occluded in illicit cocaine HCl and heroin HCl. The liberation of the occluded solvents was ensured by complete solubilization of the crystal matrices in aqueous 22% sodium sulfate. Ion trap mass spectrometry is used for both identification and quantitation; five deuterated, structurally related internal standards are utilized for more accurate quantitation. Overall method precision for 25 commonly encountered solvents averaged 6.7% RSD. Minimum detection limits ranged from 3 to 87 ppm for a 15 mg equivalent cocaine sample weight, and from 2 to 43 ppm for a 30 mg equivalent heroin sample weight. Qualitative and quantitative data for the 25 most commonly encountered occluded solvents in cocaine HCl and heroin HCl exhibits are presented.
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