高效液相色谱-电喷雾离子阱串联质谱分析水苏碱及其大鼠体内代谢物

目的鉴定水苏碱在大鼠体内的代谢物。方法应用高效液相色谱-电喷雾离子阱串联质谱(HPLC-ESI/MSⁿ)技术研究水苏碱的一级质谱电离规律、二级质谱裂解规律及其色谱保留，以此作为水苏碱大鼠体内代谢物分析鉴定的依据；再将健康大鼠空腹灌胃25 mg·kg^-1水苏碱，收集0～24 h的尿样，经C₁₈小柱固相萃取分离纯化后，应用HPLC-ESI/MS分析尿样中水苏碱代谢物。结果在大鼠尿样中发现了母药及其N-去甲基、氧化脱氢、环氧化等6种I相代谢产物及两种环氧化物的甘氨酸轭合II相代谢产物。结论HPLC-ESI/MS法灵敏度高，快速，定性能力强，适合于水苏碱大鼠体内代谢物的分析。

HPLC-ESI/MS analysis of stachydrine and its metabolites in rat urine

AIM: To identify the main metabolites of stachydrine in rat. METHODS: The ionization, cleavage and chromatographic characteristics of stachydrine were studied by using high-performance liquid chromatography-electrospray ionization ion trap tandem mass spectrometry (HPLC-ESI/MS) for the first time. These characteristics of stachydrine were used as the basis for the analyses of metabolites in rat urine. The 0 - 24 h urine samples of rats after ig 25 mg x kg(-1) stachydrine were collected and purified by using C10 solid-phase extraction cartridge, and then analyzed by HPLC-ESI/MS to identify stachydrine and its metabolites. RESULTS: The parent drug (stachydrine), 6 phase I metabolites (N-demethyl, dehydrogenation, ring-oxidation) and 2 phase II metabolites (glycine conjugates of 2 ring-oxidation products) were identified existing in rat urine. CONCLUSION: The presented method was proved to be sensitive, rapid, high selective and specific for the identification of stachydrine and its metabolites in rat urine.