LC-MS/MS测定家兔胆汁中淫羊藿次苷Ⅱ  

Quantitative analysis of icariside Ⅱ in rabbit bile by LC-MS/MS

作　　者：张依[1] 姚志红[1,2] 秦子飞[1] 李凯宇[1] 戴毅[1,2] 姚新生[1,2] 

机构地区：[1]暨南大学药学院中药及天然药物研究所,广东广州510632 [2]中药药效物质基础及创新药物研究广东省高校重点实验室,广东广州510632

出　　处：《暨南大学学报（自然科学与医学版）》2012年第3期305-310,共6页Journal of Jinan University(Natural Science & Medicine Edition)

基　　金：国家自然科学基金中港基金资助项目(30831160510)

摘　　要：建立能定量分析家兔胆汁中淫羊藿次苷Ⅱ的液相色谱-串联质谱联用法(LC-MS/MS).以水饱和乙酸乙酯萃取为家兔胆汁样本前处理方法,采用OSD柱(150×4.6 mm,i.d.,5μm),以乙腈-水(各含0.1%的甲酸)为流动相进行梯度洗脱,采用电喷雾离子源(ESI),二级质谱全扫描,负离子方式下检测.方法学考察结果显示,该方法专属性良好;日内精密度(RSD)不大于10.6%,日间精密度(RSD)不大于8.3%,准确度(RE)在-4.4%～+5.0%范围以内;胆汁样本稳定性良好;基质效应对测定影响可以忽略不计且提取率较高并稳定.该方法快速而灵敏,可用于家兔灌胃给以淫羊藿总黄酮后胆汁中的活性代谢物淫羊藿次苷Ⅱ的动态变化研究.A liquid chromatography-tandem mass spectrometry （LC-MS/MS） method was developed for quantitative analysis of icariside II in rabbit bile. Water-saturated ethyl acetate extraction was used for pretreatment of bile sample. The separation was achieved on ODS column（ 150 ×4. 6 mm, i. d. ,5 μm） by gradient elution with acetonitrile-water （ including 0. 1% formic acid respectively） as mobile phase. The ion acquisition was performed by full scan MS/MS in negative ion mode. The method was specific, accurate, precise and reproducible with intra-day RSD less than 10. 6%, inter-day RSD less than 8.3% and relative error between -4. 4% and 5.0%. Moreover, the samples exhibited good stability and high recovery. The matrix effect can be neglected. Taken together, this method can be applied to the dynamic analysi of icariside II, an active metabolite in bile after intragastric administration of Epimedium Flavonoids （EF） to rabbits.

关 键 词：淫羊藿次苷Ⅱ 液相色谱-串联质谱联用法 定量分析 活性代谢物 淫羊藿总黄酮 家兔胆汁 

分 类 号：O174.52[理学—数学]