Chen Yong, Shen Shao-Lin, Chen Huai-Xia, Han Feng-Mei
Bio-Technology of Traditional Chinese Medicine Key Lab of Hubei Province, Hubei University, Wuhan 430062, China.
Yao Xue Xue Bao. 2005 Sep;40(9):838-41.
To estabilish a rapid and sensitive LC-ESI-ITMSn method for the identification of ephedrine and its main metabolites in rat urine.
After optimizing the detection condition of LC-ESI-ITMSn chromatography and mass spectrometry by using a standard ephedrine, the ionization and cleavage rules of ephedrine in ESI-MS and ESI-MSn modes were summarized, and then serving as the basis for the metabolite analysis of ephedrine in rat urine. Rat urine samples of 0-48 h were collected after ig 10 mg x kg(-1) ephedrine, then the samples were purified through C18 solid-phase extraction cartridge. The purified samples were analyzed by LC-ESI-ITMSn.
The structures of ephedrine metabolites were elucidated according to the changes of the molecular weights of the metabolites (deltaM) and their cleavage pattern in ESI-ITMSn. As a result, three phase I metabolites and the parent drug ephedrine were identified existing in rat urine, but no phase II metabolites were found.
The LC-ESI-ITMSn method is rapid and highly sensitive and sepecific, it is suitable for the identification of ephedrine and its metabolites in rat urine.
建立一种快速、灵敏的液相色谱-电喷雾离子阱多级质谱(LC-ESI-ITMSn)方法,用于鉴定大鼠尿液中麻黄碱及其主要代谢产物。
采用标准麻黄碱优化LC-ESI-ITMSn色谱和质谱检测条件,总结麻黄碱在电喷雾质谱(ESI-MS)和电喷雾多级质谱(ESI-MSn)模式下的离子化和裂解规律,以此作为大鼠尿液中麻黄碱代谢产物分析的依据。大鼠灌胃10 mg·kg⁻¹麻黄碱后,收集0~48 h的尿液样本,然后通过C18固相萃取柱进行纯化。纯化后的样本采用LC-ESI-ITMSn进行分析。
根据代谢产物分子量的变化(ΔM)及其在ESI-ITMSn中的裂解模式,阐明了麻黄碱代谢产物的结构。结果表明,大鼠尿液中存在3种Ⅰ相代谢产物和母体药物麻黄碱,但未发现Ⅱ相代谢产物。
LC-ESI-ITMSn方法快速、灵敏且特异,适用于鉴定大鼠尿液中麻黄碱及其代谢产物。