HFBA為衍生劑配合氣相層析質譜儀同步定性定量尿液中安非他命類愷他命之代謝物

Simultaneous Determinaltion of HFBA-Derivatized Amphetamines and Ketamines in the urine by Gc-MS

李慧華(Hei-Hwa Lee)

指導教授 ： 洪清吉 ； 蔡錦蓮

高雄醫學大學/生命科學院/醫藥暨應用化學研究所/碩士(2005年)

摘要

俱樂部藥丸的氾濫導致藥物濫用者同時使用多種毒品，目前毒品尿液檢驗均為單項檢驗，檢驗耗時又增加成本，本研究發展一運用固相萃取配合氣相色層質譜儀快速同步偵測6種含胺類結構之管制藥品及其代謝物；安非他命，甲基安非他命，搖頭丸 (MDA ，MDMA， MDEA) ，K 他命 (ketamine，norketamine，dehydronorketamine)，以提升實驗室效率。
本研究以D5-amphetamine、D8-methamphetamine、D5-MDA、D5-MDMA、D6-MDEA、D4-ketamine，D4-norketamine當內部標準品，尿液調整酸鹼值以固相萃取管DAU萃取後，HFBA當衍生劑衍生化後的衍生物以氣相色層質譜儀分析。質譜選擇特徵離子分別為Amphetamine（240，118，91）、Methamphetamine（254，210，118）、MDA（135，162，239）、MDMA（254，162，210）、MDEA（268，162，240）、Ketamine（210，392，378）、Norketamine（314，340，356）、Dehydronorketamine（314，102，137） ，本方法的線性定量範圍均在100至2000ng/ml之間，最低可定性、定量偵測極限各為amphetamine（60ng/ml、75ng/ml）、methamphetamine（60 ng/ml、75 ng/ml）、MDA（75 ng/ml、100 ng/ml）、MDMA（75 ng/ml、100 ng/ml）、MDEA（75 ng/ml、100 ng/ml）、ketamine（30 ng/ml、50 ng/ml）、norketamine（50 ng/ml、75 ng/ml）、Dehydronorketamine（50 ng/ml、125 ng/ml），回收率為amphetamine（94.4％）、methamphetamine（92.4％）、MDA（96.8％）、MDMA（99.2％）、MDEA（97.8％）、Ketamine（97.4％）、Norketamine（97.0％），在pH6.0本方法的穩定性及再現性良好，其同日間變異及異日間變異及正確性分別為amphetamine（0.47％，0.40％，97.89％）、methamphetamine（0.43％，1.06％，99.73％）、MDA（0.51％，1.49％，98.84％）、MDMA（0.47％，0.52％，99.93％）、MDEA（0.41％，2.85％，99.42％）、ketamine（0.62％，4.90％，99.93％）、norketamine（2.42％，1.86％，97.96％）、dehydronorketamine（3.21％，4.50％，117.76％）。

關鍵字

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並列摘要

This study developed a rapid, sensitive, and accurate method for the simultaneously determinations of 8 commonly abused drugs/metabolites containing amine functional groups, i.e., amphetamine, methamphetamine, MDA, MDMA, MDEA, ketamine, norketamine and dehydronorketamine. The protocol included solid phase extraction, HFBA derivatization and GC-MS analysis, using d5-amphetamine, d8-methamphetamine, d5-MDA, d5-MDMA, d6-MDEA, d4-ketamine and d4-norketamine were used as the internal standards. Identification of these compounds were based on retention time information and the relative abundance of the following ions established for each analyte as derivatized by HFBA: amphetamine: 240, 118, 91; methamphetamine: 254, 210, 118; MDA: 135, 162, 239; MDMA: 254, 162, 210; MDEA: 268,162, 240; ketamine: 210 392, 378; norketamine; 314, 340, 356; dehydronorketamine: 314,102, 137. The following analytical parameters have also been established: linear range: 100–2000 ng/ml; limits of detection and quantitations (all in ng/ml): 60 and 75 for amphetamine; 60 and 75 for methamphetamine; 75 and 100 for MDA; 75 and 100 for MDMA; 75 and 100 for MDEA; 30 and 50 for ketamine; 50 and 75 for norketamine and 50 and 125 for dehydronorketamine. The overall method recoveries of HFBA-derivatized amphetamine analogs were 92–99%, with less than 5% CV of intra-day and inter-day of the overall analytical data. In conclusion, this method provides a uniform procedure for confirmation tests of the amphetamines and ketamine drug categories under workplace drug testing settings. Under clinical testing environment, it can be effectively used for the preliminary and confirmation test of these 8 drugs/metabolites, otherwise will have to be first screened by three immunoassays, specific for amphetamine/methamphetamine, MDA/MDMA/MDEA, and ketamines, respectively.

並列關鍵字

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參考文獻

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