目的:建立家兔血液及关节微透析液中青藤碱的高效液相色谱-质谱联用测定方法,并应用于青藤碱在家兔体内的整体药动学及局部药动学的研究。方法:采用Hypersil GOLD C18柱(150mm×2.1mm,3μm),流动相为甲醇-0.1%甲酸(30:70),流速0.2mL·min^-1,质谱为电喷雾离子源,选择反应离子监测,质荷比为239和181,采用外标法,微透析样品直接进样分析。结果:在0.336-172μg·L。范围内呈线性关系良好,r=0.9972,定量下限为0.336μg·L^-1,低、中、高浓度质控样品的日内及日间精密度符合要求。结论:本方法灵敏度高,操作简便,能满足体内微透析样品中低浓度的测定,可用于青藤碱药物动力学特性的研究C0m
OBJECTIVE To develop a liquid chromatography-electrospray mass spectrometry (HPLC-MS) method for the determination of sinomenine in microdialysis samples in rabbit blood and joint fluid. METHODS A Hypersit C-OLD C18 column (1511 mm× 2. 1 mm,3 μm)was used and the mobile phase consisted of methanol:0. 1% fomic acid (30:70) at the flow rate of 0.2 mL·min^-1. The microdialysis samples were directly injected into the HPLC-MS system equipped with an electrospray ionization source, operated in the positiveion detection mode. In selected reaction monitoring mode, the ion combinations of m/z 239 and m/z 181 were used to qualify sinomenine. RESULTS The method was linear over the range of 0. 336-172 μg·L^-1(r=0.997 2), the limit of detection was 0. 336μg·L^-1,the inter-and intra-day variation of the low, middle and high concentrations were accord with requirement. CONCLUSION The method appeared to be sensitive and simple. It is suitable for the pharmaco kinetics study of sinomenine.