Identification and quantitation of ibogaine and an o-demethylated metabolite in brain and biological fluids using gas chromatography-mass spectrometry.
Identification and quantitation of ibogaine and an o-demethylated metabolite in brain and biological fluids using gas chromatography-mass spectrometry.
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使用气相色谱-质谱法对大脑和生物体液中的伊博加因和邻去甲基化代谢物进行鉴定和定量。
DOI：
10.1093/jat/19.6.427
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发表时间：
1995
影响因子：
2.5
通讯作者：
Mash,DC
中科院分区：
文献类型：
--
作者：
Hearn,WL;Pablo,J;Hime,GW;Mash,DC
本报告描述了一种灵敏的方法，用于定量生物体液和脑组织中的伊波替尼和单一主要代谢物。我们通过全扫描、电子轰击气相色谱-质谱（GC-MS）鉴定了代谢产物12-羟基-伊博加明（12-OH-伊博加明或诺利博明）。在碱性条件下通过溶剂萃取分离伊波加因、12-OH-伊波加明和do-（甲基）-伊波加因-d3（伊波加因-d3）内标物。将得到的有机萃取物蒸发至干，并在二甲基亚砜中，在三甲基苯胺氢氧化物存在下，在室温下用碘乙烷将残余物衍生化。通过酸化终止反应，并用有机溶剂洗涤以除去杂质。然后将水相碱化并再萃取。浓缩有机萃取物并通过GC-MS进行分析。基于分子离子的比率（对于伊波替尼为atm/z310，对于伊波加因-d3为m/z313，对于12-OH-伊波加明乙醚为m/z324）进行定量。对于伊波替尼和衍生的12-OH-伊波加明，检测限均为5 ng/mL，对于所有检测基质，定量限均在5 - 10 ng/mL之间。两种分析物的校准曲线在5-1000 ng/mL或ng/g范围内呈线性。
This report describes a sensitive method for quantitating ibogaine and a single major metabolite in biological fluids and brain tissue. We identified the metabolite as 12-hydroxy-ibogamine (12-OH-ibogamine or noribogaine) by full-scan, electron-impact gas chromatography-mass spectrometry (GC-MS). Ibogaine, 12-OH-ibogamine, ando-(methyl)-ibogaine-d3(ibogaine-d3) internal standard were isolated by solvent extraction under basic conditions. The resulting organic extract was evaporated to dryness, and the residue was derivatized at room temperature with ethyl iodide in the presence of trimethyl anilinium hydroxide in dimetbyl sulfoxide. The reaction was terminated by acidification and washed with organic solvents to remove impurities. The aqueous phase was then alkalinized and reextracted. The organic extract was concentrated and analyzed by GC-MS. Quantitation was based upon the ratios of the molecular ions atm/z310 for ibogaine,m/z313 for ibogaine-d3, andm/z324 for 12-OH-ibogamine ethyl ether. The limit of detection was 5 ng/mL for both ibogaine and derivatized 12-OH-ibogamine, and limits of quantitation were between 5 and 10 ng/mL for all matrices tested. Calibration curves were linear in the range of 5–1000 ng/mL or ng/g for both analytes.