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.
The applicability of capillary electrochromatography (CEC) with photodiode array UV detection for the analysis of cannabinoids is presented. Baseline separation of seven cannabinoids (cannabigerol, cannabidiol, cannabinol, delta-9-tetrahydrocannabinol, delta-8-tetrahydrocannabinol, cannabichromene, delta-9-tetrahydrocannabinolic acid) is obtained using a 3-micron CEC Hypersil C18 capillary with an acetonitrile/phosphate (pH 2.57) mobile phase. The effects of acetonitrile concentration, buffer concentration, voltage, temperature, stationary phase, and column length on the separation of the cannabinoids were investigated. Good short- and long-term precision in retention times are observed, with significant improvement obtained using relative retention times with cannabinol as reference compound. Although short- and long-term peak area precisions are poor, satisfactory reproducibility is obtained using relative peak areas with cannabinol as reference compound. The applicability of the CEC methodology to drug seizures was demonstrated on marijuana and hashish. Using a high-sensitivity UV flow cell with an extended path length of 1.2 mm, concentration sensitivities approaching HPLC were obtained.
Methodologies are presented for the qualitative and quantitative determinations of anabolic steroids in forensic exhibits using micellar electrokinetic capillary chromatography (MECC), high performance liquid chromatography (HPLC) and capillary gas chromatography (GC). Analyses of representative pharmaceutical dosage forms (including a commercial aqueous suspension, a commercial tablet, several commercial oil samples and various simulated dosage units) were performed using a simple, one step quantitative extraction procedure with methanol. Good agreement was obtained between all three techniques. Retention, migration and linearity data are presented and compared for over twenty anabolic steroids commonly encountered in forensic exhibits. A principal component analysis study confirmed the orthogonality of the three techniques.
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