標題: 應用非水相毛細管電泳/質譜儀檢測麥角酸乙二胺與其代謝物
Determination of LSD and its metabolites by nonaqueous capillary electrophoresis-mass spectrometry
作者: 高婉君
Kao, Wan-Chun
謝有容
Hsieh, You-Zung
應用化學系碩博士班
關鍵字: 非水相毛細管電泳;質譜;nonaqueous capillary electrophoresis;mass spectrometry
公開日期: 2010
摘要: 近年來,濫用藥物的新聞層出不窮,其中麥角酸乙二胺為青少年常用的 濫用藥物之一。在本研究中,我們選用非水相毛細管電泳/質譜儀作為偵測 麥角酸乙二胺與其代謝物的方法。非水相毛細管電泳具有許多好處,如:有 機溶劑具有高揮發性與低表面張力,這些特性使其在分離效率佳之外,更適 合與大氣壓游離源串聯。首先,我們探討非水相毛細管電泳法中,各種參數 對解析度的影響。有機酸的種類和濃度影響分析物質子化的程度,不同比例 的有機溶劑和鹽類濃度也對電滲流的速度有所影響。爾後,利用非水相毛細 管電泳/質譜儀,探討鞘流組成與流速、霧化氣體壓力、乾燥氣體流量與毛 細管溫度對游離效率之影響。最後,我們使用的系統為100 mM 甲酸,30 mM 甲酸銨,溶液組成為甲醇-乙腈(90:10, v/v)的背景電解液,輔助鞘流為流 速5 μL/min 的甲醇-水(90:10, v/v)溶液,霧化氣體壓力為4 psi,毛細管溫 度為250 ℃且乾燥氣體流量為4 L/min。在最佳化條件下,此方法能在22 分鐘內成功分離麥角酸乙二胺與其代謝物,線性範圍為50-1000 ng/mL,線 性相關係數(r2)皆大於0.9909,表示其線性關係良好。顯示非水相毛細管電 泳/質譜儀能成功應用於麥角酸乙二胺與其代謝物的檢測,確實為一種具有 高再現性以及高分離效率的分析方法。
Lysergic acid diethylamide(LSD)is a kind of hallucinogenic drug that is abused by teenagers in Taiwan. Therefore, to develop a rapid, sensitive method for analyzing these drugs is important and necessary. In this study, we used nonaqueous capillary electrophoresis(NACE)/electrospray ionization mass spectrometry (ESI-MS) to investigate LSD, Nor-LSD and 2-oxo-3-hydroxy-LSD. In order to get satisfied separation efficiency and sensitivity, several experimental parameters were optimized, example for the buffer composition, the nonaqueous solvent’s proportion, and the concentration of salts in the nonaqueous buffer for NACE separation; Then, the composition and flow rate of sheath liquid, nebulizer gas pressure, dry gas flow rate and capillary temperature were investigated by NACE-ESI-MS. Under the optimal condition—background electrolyte comprising a mixture of methanol/acetonitrile (90:10, v/v) and 100 mM formic acid /30 mM ammonium formate and sheath liquid containing MeOH/water (90:10, v/v) delivered at 5 μL/min—the satisfied separation was obtained for all analytes. Therefore, the NACE-ESI-MS method was validated and applied to determine LSD and it metabolites.
URI: http://140.113.39.130/cdrfb3/record/nctu/#GT079825504
http://hdl.handle.net/11536/47591
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