人血浆中酚妥拉明浓度的LC-MS测定  

Determination of Phentolamine in Human Plasma by LC-MS

作　　者：胡敏[1] 施孝金[1] 李中东[1] 刘罡一 余琛 

机构地区：[1]复旦大学附属华山医院药剂科,上海200040 [2]上海徐汇区中心医院中心实验室,上海200031

出　　处：《中国医药工业杂志》2003年第11期565-567,共3页Chinese Journal of Pharmaceuticals

摘　　要：建立高效液相 -质谱法测定人血浆中酚妥拉明的浓度。采用 Inertsil ODS- 3色谱柱 ,柱温 2 0°C,流动相为0 .1%三氟乙酸水溶液 - 0 .1%三氟乙酸乙腈溶液 (45∶ 5 5 ) ,流速 0 .2 m l/ min,以 N-去二甲基西布曲明为内标。电喷雾离子源 (ESI) ,电离电压 5 k V,离子源温度 4 0 0°C,碰撞能量 4 0 e V,检测通道 (内标 ) 2 5 2 .3/ 12 5 .1,通道 (酚妥拉明 ) 2 82 .2 / 12 0 .2。在 1～ 15 0 ng/ ml范围内 ,样品与内标的峰面积比与样品浓度间加权 (1/ c)回归具有良好的线性关系 (r=0 .9999)。酚妥拉明和内标的平均提取回收率均大于 89%。血样经过 3次冻融仍保持稳定 ,待测样品在全自动进样器中 12 h稳定 。The LC-MS method for determination of the concentration of phentolamine in human plasma was presented. The Inertsil ODS-3 column was used, with mobile phase of 0.1% trifluoroacetic acid aqueous solution-0.1% trifluoroacetic acid in acetonitrile (45∶55). The flow rate was 0.2 ml/min. N -Di-desmethyl sibutramine was used as the internal standard. It was performed with electronic spray ion (ESI), ionization voltage 5 kV, ion source temperature 400 °C , collision energy 40 eV, detect channel Ⅰ (internal standard) 252.3/125.1, detect channel Ⅱ(phentolamine) 282.2/120.2. It had a good linearity ( 1/c weighted) ( r =0.9999) over the concentration range of 1～150 ng/ml. The absolute recovery was over 89%. Stability research results showed that the samples were stable after 3 times of frozen-thaw test, and the samples could remain unchanged for at least 12 h. The precisions of intra- and inter-batch were good.

关 键 词：酚妥拉明 N-去二甲基西布曲明 高效液相-质谱 测定 

分 类 号：TQ460.72[医药卫生—药物分析学] O657.72[化学工程—制药化工]