以毛細管電泳螢光光譜法對尿液及藥錠中3,4-亞甲雙氧甲基安非他命(3,4-MDMA)及相關濫用藥物光學異構物之分析研究

dc.contributor林震煌zh_TW
dc.contributorCheng-Huang Linen_US
dc.contributor.author黃鈺珊zh_TW
dc.contributor.authorYu-San Huangen_US
dc.date.accessioned2019-09-04T09:31:28Z
dc.date.available2007-6-14
dc.date.available2019-09-04T09:31:28Z
dc.date.issued2006
dc.description.abstract製備R-(-)-和S-(+)-3,4-MDMA的光學異構物,並以GC-MS鑑認其化學結構與純度之後,以此為標準品,做為毛細管電泳分離分析法時標準添加之用。本研究以毛細管電泳的方式成功分離了R-(-)-和S-(+)-3,4-MDMA及其相關的類似化合物,並探討電泳緩衝溶液中β-CD濃度、有機溶劑比例等電泳,以求得最佳化的分離條件。最後以此做為判定藥錠及尿液中(RS)-MDA和(RS)-MDMA的存在與否的方法,並找出R-(-)-和S-(+)-型藥錠中及尿液代謝物中彼此的相對存在量。 本研究分別比較了水相與非水相毛細管電泳/螢光偵測法在進行光學異構物的分離與在進行線上濃縮時的優缺點,並探討當緩衝溶液中添加不同濃度的ß-CD時,SDS-陰離子界面活性劑與CTAB-陽離子界面活性劑對電泳分離的影響。實驗選用R-(-)-/S-(+)型的MDMA及其相關狡詐家藥物(MDA, DMMDA, MBDB, BDB )做為測試樣品。實驗首先合成並分離了單一型的R-(-)-與S-(+)-MDMA 標準品,經GC/MS及旋光光譜儀鑑定無誤後,做為標準添加之用。電泳分離結果發現,對於水相毛細管電泳在進行光學異構物的分離時發現β-CD與CTAB所組成的溶液(β-CD與SDS所組成的緩衝溶液)對光學異構物的分離效果較佳,可使八種光學異構物達到完全分離的效果。對非水相電泳分離而言,當非水相緩衝溶液使用150 mM CTAB (MeOH:foramide = 7: 3; v/v)時,可使MDA、MDMA、DMMDA、MBDB完全分離。而當非水相緩衝溶液添加150 mM 的β-CD,可使R-(-)-與S-(+)-型等八種光學異構物達到完全分離的效果。實驗並成功鑑定了R-(-)-與S-(+)-MDMA在MDMA藥錠及吸食MDMA者尿液中各異構物存在的比例。此外,當比較水相與非水相毛細管電泳術對線上濃縮技術時發現,以sweeping-MEKC為電泳模式的最佳緩衝溶液條件為SDS 50mM 溶解於含有機修飾劑(MeOH:ACN:H2O = 30 : 7:63 ; v/v/v;pH=2;導電度=4.4ms/cm)的溶液的效果最好。最佳進樣長度為40 cm(毛細管總長87/92cm)時的偵測極限可達1 ppb。但是SDS不適合做為非水相sweeping-MEKC之用;以非水相-stacking的技術,偵測極限仍可達2.6 ×10-8 M。zh_TW
dc.description.abstractThe R-(-)- and S-(+)-isomers of 3,4-methylenedioxymethamphetamine (MDMA) and its metabolite 3,4-methylenedioxyamphetamine (MDA) were prepared, identified by GC/MS and then used as standards in a series of CE experiments. Using these R-(-)- and S-(+)-isomers, the distribution of (RS)-MDA and (RS)-MDMA stereoisomers in clandestine tablets and suspect urine samples were identified. Several electrophoretic parameters, such as the concentration of -cyclodextrin used in the electrophoretic separation and the amount of organic solvents required for the separation were optimized. A comparison of the use of aqueous and non-aqueous solutions in association with -cyclodextrin for the chiral separation of (R)- and (S)-3,4-methylenedioxymethamphetamine and related compounds is described. The (R)- and (S)-isomers of 3,4-methylenedioxymethamphetamine (MDMA) and its major metabolite 3,4-methylenedioxyamphetamine (MDA) were prepared. Under aqueous and non-aqueous solution conditions and based on the CZE and MEKC modes, the order of migration of (R)-MDA, (S)-MDA, (R)-MDMA and the (S)-MDMA enantioisomers were determined. Several electrophoretic parameters, including the concentration of -cyclodextrin (aqueous, 25 ~ 60 mM; non-aqueous, 20 ~ 150 mM) used in the electrophoretic separation and the amount of organic solvents required for the separation were optimized.en_US
dc.description.sponsorship化學系zh_TW
dc.identifierGN0693420063
dc.identifier.urihttp://etds.lib.ntnu.edu.tw/cgi-bin/gs32/gsweb.cgi?o=dstdcdr&s=id=%22GN0693420063%22.&%22.id.&
dc.identifier.urihttp://rportal.lib.ntnu.edu.tw:80/handle/20.500.12235/100487
dc.language中文
dc.subject毛細管電泳zh_TW
dc.subjectMDMAzh_TW
dc.subject螢光zh_TW
dc.subject非水相zh_TW
dc.subjectCTABzh_TW
dc.subject光學異構物zh_TW
dc.title以毛細管電泳螢光光譜法對尿液及藥錠中3,4-亞甲雙氧甲基安非他命(3,4-MDMA)及相關濫用藥物光學異構物之分析研究zh_TW
dc.titleCHIRAL SEPARATION OF 3,4-MDMA AND RELATED COMPOUNDS IN CLANDESTINE TABLETS AND URINE SAMPLES BY CAPILLARY ELECTROPHORESIS / FLUORESCENCE SPECTROSCOPYen_US

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