【摘要】 目的:分离和鉴定健康志愿者口服盐酸小檗碱后尿中的未知代谢产物.方法:用大孔树酯柱层析方法分离和纯化代谢产物,电喷雾-离子化质谱（ESI-MS）及¹H核磁共振（¹H NMR）进行结构分析.结果:三个未知代谢产物（M1,M2和M3）被分离纯化,它们均对芳基硫酸酯酶敏感.电喷雾质谱中分别可见准分子离子峰[M+H]⁺417.9,404.0和402.0,以及脱SO₃片段的特征离子峰[M-80+H]⁺.测得各自的1H NMR谱,参考盐酸小檗碱的质子信号,确定了M1,M2和M3的质子信号归所及取代基的位置.结论:M1,M2和M3的结构可分别推定为药根碱-3-硫酸酯（M1）、脱亚甲基小檗碱-2-硫酸酯（M2）和Thalifendine-10-硫酸酯（M3）.其中M2为主要代谢产物.更多还原

【Abstract】 To identify the structure of unknown metabolites of berberine (Ber) in human urine after oral administration . METHODS: Urine samples were obtained from 5 volunteers after they orally took Ber chloride 0.9 g per day for three days. Metabolites in urine samples were isolated and purified by polyporous resin column chromatography. The individual metabolites were identified mainly using electrospray ionization mass spectro-scopy (ESI-MS) and proton nuclear magnetic resonance (H NMR) spectroscopy. RESULTS: Three unknown metabolites (Ml, M2, and M3) were isolated. They were susceptible to arylsufatase. ESI-MS measurements of Ml, M2, and M3 produced quasimolecular ions [ M + H+ . m/z 417.9, 404.0, and 402. 0 respectively. Especially, each of them produced a characteristic pro-tonated ion [M-80+H]+ , which can be ascribed as quasimolecular ions lost a SO3 fragment.1H NMR spectra of the metabolites were also obtained and each of ’H signals was assigned. CONCLUSION: Structures of Ml, M2, and M3 were firmly identified as jatror-rhizine-3-sulfate, demethyleneberberine-2-sulfate, and thalifendine-10-sulfate, and the major metabolite was M2.更多还原