Abstract
AbstractA variety of drugs including opiates, amphetamines, MDMA, MDA, ketamine, and marijuana are nowadays commonly abused in Taiwan. This thesis aimed to analyze such controlled substances in samples of urine, head hair, and indoor air using various kinds of pretreatment strategies coupled to gas chromatography-mass spectrometry (GC-MS).This work includes five parts. Part I: An analytical scheme using GC-MS assisted by precedent liquid-liquid extraction (LLE) and chemical derivatization with petafluorobenzoyl chloride (PFBC) is described for the simultaneous determination of ketamine (KT) and its major metabolite, norketamine (NK), in urine specimens. Part II: Preceding the extraction procedure, the urine and hair samples after adequate preparation were treated, respectively, with acid, alkaline, and methanol hydrolysis. The solid-phase extraction (SPE) instrument equipped with a HCX column was employed to recover codeine, morphine, and 6-acetylmorphine from both samples. The extracted solution was dried, devirated by MSTFA, and followed by GC-MS analysis with the purpose to investigate qualification and quantification of opiates and the metabolites in urine and hair. Part III: In this study, a total of seven items including table salt, liquid soap, chlorine bleach, Vitali drinking soda water, tap water, potassium dichromate, and aluminum ammonium sulfate were adulterated respectively with three different concentrations (5%, 10%, and 15%) to urine samples containing morphine/codeine, MDA/MDMA, or AP/MP. The adulterated urine samples were screened using TDx and Beckman LX/20 instrument. The adulterating impact on urine analysis of abused drugs was evaluated as a function of TDx values, creatinine, gravity, pH, nitrite, color, and odor. GC-MS analysis was then followed for confirmatory purpose. The effects and variations were analyzed by SPSS. Part IV: The aim of this part was to optimize the storage conditions of urine samples. The five drugs including THC-COOH, AP, MA, MDMA, and MDA contained in urines were analyzed by GC-MS. Based on the raw data obtained, the optimization of storage conditions was established by using the orthogonal arrays of L64421 and L16215, coupled with the statistical analyses of ANOVA by SPSS software. Part V: A simple and affordable method for the determination of Δ9-tetrahydrocannabinol (Δ9-THC) in indoor air was described. A personal air-sampler pump fitted with the GC liner-tube packed with Tenax-TA adsorbent was used for air sampling. The GC-adsorbent tube was placed in the GC injector port and desorbed directly, followed by GC-MS analysis for the determination of Δ9-THC in indoor air.Major results of the five are briefly described as the following. Part I: The derivatives of KT and NK in urine specimens can be successfully identified. The mass spectra can always distinctly reflect the natural-abundance ratio of Cl35 and Cl37 isotopes, i.e., Im/z M+!/Im/z M+3≒3:1, thereby facilitating the confirmation of KTs. Part II: A total of 30 paired samples of hair and urine from the same individual were analyzed. All the 30 paired samples were concluded to be morphine-positive, with emphasizing that the 6-acetylmorphine couldn’t be detected from the urine. The percentage of 6-acetylmorphine detected in the inmates’ hair samples with methanol hydrolysis were found to be 63.3% (19 out of 30). Part III: All the seven tested adulterants would render significant impacts on forensic amphetamines urinalysis by TDx screening and GC-MS confirmatory tests, with chlorine bleach being most likely to give false negatives, especially on near-cutoff specimens. Part IV: For the optimized period of storage, the THC-COOH was found to be within 40 days, and the other four were within 90 days. The best raw materials built into containers for the AP, MA, and THC-COOH was glass, and PP material for MDMA and MDA. All five drugs had an optimized storage condition of temperature at -20℃. As for the factor of drug concentration, the five drugs at 1.25 times of their respective cut-off value were revealed to be the best. Part V: The characteristic Δ9-THC peak in chromatogram can serve as the indicator of marijuana. The average desorption efficiency and limit of detection for Δ9-THC were 89% and 0.1 μg m-3, respectively, approximately needing 1.09 mg of marijuana leaves smoked in an unventilated closed room (3.0m × 2.4m × 2.7m) to reach this level.The proposed methods and thus obtained results in this thesis would provide useful information for practical forensic drug testing.