HPLC-MS测定大鼠血浆中薯蓣皂苷元的浓度  

HPLC-MS determination of diosgenin in rat plasma

作　　者：刘海峰[1] 陈晓春[1] 严敏[1] 薛洪宝[1] 李晖[1] 

机构地区：[1]四川大学化学工程学院,成都610065

出　　处：《药物分析杂志》2009年第7期1096-1098,共3页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立测定大鼠血浆中薯蓣皂苷元的液相色谱-质谱法(HPLC-MS)定量分析方法。方法:血浆样品加入内标丹参酮ⅡA(TanshinoneⅡA),酸化后用乙酸乙酯提取,进行HPLC-MS测定。色谱柱为ALLTIMA-C18(3.5μm,2.1mm×150mm),流动相为乙腈-0.1%三氟乙酸水溶液(95∶5),流速为0.2mL.min-1;采用HPLC-MS,选择离子监测(SIM)法检测薯蓣皂苷元([M+H]+,m/z415.4),丹参酮ⅡA(内标,[M+H]+,m/z295.2)。结果:血浆中杂质不干扰样品和内标的测定,线性范围为1～100μg·mL-1;方法回收率大于70%,日内、日间精密度RSD小于16%,稳定性符合生物样品测定要求。结论:经方法学确证和稳定性评价,该方法可用于薯蓣皂苷元的药动学研究。Objective ：To develop an HPLC - MS method for the determination of diosgenin in rat plasma. Methods： Add the standard of tanshinone ⅡA into the plasma samples ,then add some acid into the samples. The plasma samples were extracted with ethyl acetate. The ALLTIMA- C18 （3.5 μm,2. 1 mm × 150 mm） column was adopted. The mobile phase was consisted of acetonitrile - water including 0. 1% trifluoroacetie acid （TFA） （95：5 ）. Electrospray ionization （ESI）and selected ion mass（SIM） were used to determine the diosgenin （ [ M ＋ H ] ^＋ , m/z 415.4）and tanshinone ⅡA （ internal standard, [ M ＋ H]^＋ ,m/z 295.2）. Results：The linear range of diosgenin was 1 to 100 μg· mL^-1 The recovery was above 70%. The intra -and inter- day RSDs were less than 16%. Conclusion：This method is sensitive, specific and rapid. Therefore, it can be used for pharmacokinetic study of diosgenin. ;

关 键 词：薯蓣皂苷元 血药浓度 高效液相色谱-质谱 

分 类 号：R917[医药卫生—药物分析学]