固相萃取-HPLC/MS/MS法测定血浆中苦木碱丁的浓度  

SPE-LC/MS/MS determination of 4,5-dimethoxy-canthin-one in plasma

作　　者：李慧[1] 张源[1] 林哲绚[1] 罗文鸿[1] 

机构地区：[1]汕头大学医学院中心实验室,汕头515041

出　　处：《药物分析杂志》2006年第4期525-527,共3页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立测定血浆中苦木碱丁浓度的高效液相色谱/质谱/质谱分析方法。方法:液相色谱:流动相为甲醇-0.01 mol·L^(-1)乙酸铵水溶液(80:20),流速0.2 mL·min^(-1);色谱柱为 SYMMETRY C_(18)(2.1 mm×50 mm,3.5 μm),柱温30℃。质谱:电喷雾电离源(ESI),采用多反应监测(MRM)方式进行检测,m/z 281.4→237.1。血浆样本经固相萃取小柱提取处理后进样分析。结果:苦木碱丁在5～100 ng·mL^(-1)浓度范围内线性关系良好。萃取回收率98.3%～107%。日内误差(RSD)小于4.7%,日间误差(RSD)小于5.1%。结论:本方法具有特异性高、灵敏度好、测定快速等优点,适用于血浆中的苦木碱丁的含量测定。Objective：To establish an I.E/MS/MS method for the quantitative determination of 4,5 -dimethoxy - canthin-one in plasma. Method： Plasma samples were prepared by C18 solid phase extraction（SPE）. LC mobile phase：methanol-0. 01 mol L^-1 ammonium acetate（80： 20）,flow rate 0. 2 mL·min^-1; chromatography column： Waters Symmetry C18 （ 2.1 mm × 50 mm, 3.5 μm）. MS/MS： electrospray （ESI） with MRM detection mode, positive ion,m/z 281.4→237.1. Results. Linear range for the calibration curve was between 5 - 100 ng · mL^-1 （r = 0. 9999）. Spike recoveries were between 98.3% - 107% with within - day and day - to - day RSD less than 5. 1%. Conclusion：The method is sensitive, rapid and reliable for the quantitative determination of 4,5 -dimethoxy - canthin - one in plasma.

关 键 词：苦木碱丁 高效液相色谱/质谱/质谱 固相萃取 

分 类 号：R917[医药卫生—药物分析学]