人体内的内源性生物碱。XXVI. 使用气相色谱-选择离子监测法测定生物样品中的多巴胺能神经毒素1-三氯甲基-1,2,3,4-四氢-β-咔啉（TaClo）

Endogenous alkaloids in man. XXVI. Determination of the dopaminergic neurotoxin 1-trichloromethyl-1,2,3,4-tetrahydro-beta-carboline (TaClo) in biological samples using gas chromatography with selected ion monitoring.

作者信息

Bringmann G, Friedrich H, Birner G, Koob M, Sontag K H, Heim C, Kolasiewicz W, Fähr S, Stäblein M, God R, Feineis D

机构信息

Institute of Organic Chemistry, University of Würzburg, Germany.

出版信息

J Chromatogr B Biomed Appl. 1996 Dec 13;687(2):337-48. doi: 10.1016/s0378-4347(96)00255-1.

DOI:10.1016/s0378-4347(96)00255-1

PMID:9017456

Abstract

Highly chlorinated beta-carbolines have a potential in vivo relevance to Parkinson's disease. In this paper, a gas chromatographic method for the determination of the neurotoxic 1-trichloromethyl-1,2,3,4-tetrahydro-beta-carboline (TaClo), the condensation product of tryptamine and chloral hydrate, is described. The specific and sensitive assay involves purification of the biological samples by solid-phase extraction with C18 cartridges, derivatization with heptafluorobutyric anhydride, and chromatography on a non-polar fused-silica capillary column. Detection of TaClo was achieved by the registration of characteristic mass fragments of the TaClo heptafluorobutyric amide derivative using selected ion monitoring. The method was utilized to detect and quantify TaClo in blood, urine, bile, faeces, and brain tissue of rats treated with this alkaloid-type heterocycle. Four-fold deuterium-labelled TaClo was used as an internal standard.

摘要

高度氯化的β-咔啉在体内与帕金森病具有潜在关联。本文描述了一种气相色谱法，用于测定神经毒性物质1-三氯甲基-1,2,3,4-四氢-β-咔啉（TaClo），即色胺与水合氯醛的缩合产物。该特异性且灵敏的分析方法包括通过C18柱固相萃取对生物样品进行纯化、用七氟丁酸酐进行衍生化，以及在非极性熔融石英毛细管柱上进行色谱分析。通过使用选择离子监测记录TaClo七氟丁酰胺衍生物的特征质量碎片来实现对TaClo的检测。该方法用于检测和定量用这种生物碱型杂环化合物处理的大鼠的血液、尿液、胆汁、粪便和脑组织中的TaClo。四倍氘标记的TaClo用作内标。