大鼠粪样中山莨菪碱及其代谢物的串联质谱法检测

目的运用液相色谱-电喷雾串联质谱(LC-MSn)法检测大鼠粪样中山莨菪碱及其代谢物。方法收集灌胃山莨菪碱(25 mg·kg^-1)的大鼠粪样,用水浸泡后,以乙酸乙酯萃取,采用LC-MS及LC-MSn等方法检测原药及其代谢物。根据代谢物相对分子质量的变化(ΔM)及其多级质谱数据,鉴定并阐述其结构,同时与空白粪样及山莨菪碱相比较。结果在服药后的大鼠粪样中发现山莨菪碱及其7种代谢产物, 分别为6β-羟基托品、N-去甲基-6β-羟基托品、N-去甲基脱水山莨菪碱、脱水山莨菪碱、N-去甲基山莨菪碱、羟基山莨菪碱以及托品酸等。结论该方法灵敏、快速、简便、有效,适合于生物样品中的药物及其代谢产物的快速鉴定。

Detection of anisodamine and its metabolites in rat feces by tandem mass spectrometry

AIM: To establish a LC-MS(n) method for the identification of anisodamine and its metabolites in rat feces. METHODS: Feces samples were collected after single administration of 25 mg x kg(-1) anisodamine to rats, and dipped in water for 1 h. Samples were then extracted by ethyl acetate. The pretreated samples were separated on a reversed-phase C18 column using a mobile phase of methanol / 0.01% triethylamine (adjusted to pH 3.5 with formic acid) (60 : 40, v/v) and detected by LC-MS". Identification of the metabolites and elucidation of their structures were performed by comparing their changes in molecular masses (deltaM), retention-times and full scan MS(n) spectra with those of the parent drug and blank feces. RESULTS: The parent drug and its seven metabolites (6beta-hydroxytropine, nor-6beta-hydroxytropine, aponoranisodamine, apoanisodamine, noranisodamine and hydroxyanisodamine, tropic acid) were found in rat feces. CONCLUSION: This method is sensitive, rapid, simple, effective, and suitable for the rapid identification of drug and its metabolites in biologic samples.