Liu Ping, Liang Sun, Wang Ben-Jie, Guo Rui-Chen
Institute of Clinical Pharmacology, Qilu Hospital of Shandong University, Jinan 250012, China.
Eur J Drug Metab Pharmacokinet. 2009 Jul-Sep;34(3-4):185-92. doi: 10.1007/BF03191172.
A sensitive and selective liquid chromatography-tandem mass spectrometric (LC-MS) method was developed and validated for the determination of Tramadol in human plasma and urine. The analyte was separated on a Diamonsil C18 column with ammonium acetate (5 mmol x L(-1))-methanol (50:50,v:v) adjusted PH by caustic soda at a flow rate of 0.8 ml min(-1), and analyzed by mass spectrometry is in positive ion mode. The ion mass spectrum of m/z were 264.1 for Tramadol and 248.0 for Tinidazole (I.S.), respectively. The weighted (1/x2) calibration curve was linear over plasma concentration range 1.00-400.00 ng/ml and urine concentration range 0.01-16.00 microg/ml, with a correlation coefficient (r) of 0.9995 and 0.9997, respectively. The lower limit of quantification in human plasma was 1.00 ng/ml. The inter-and intra-day precisions (CV%) in both plasma and urine were lower than 10%, the mean method accuracies and recoveries from spiked plasma samples at three concentrations ranged from 98.2 to 100.1% and 61.6 to 62.9%, respectively. The developed method was successfully applied to determine Tramadol in human plasma and urine, and provided suitable profiles for clinical pharmacokinetic study of Tramadol.
建立了一种灵敏、选择性好的液相色谱 - 串联质谱（LC-MS）方法并进行了验证，用于测定人血浆和尿液中的曲马多。分析物在迪马硅C18柱上分离，流动相为醋酸铵（5 mmol·L⁻¹）-甲醇（50:50，v:v），用氢氧化钠调节pH值，流速为0.8 ml·min⁻¹，质谱分析采用正离子模式。曲马多的离子质荷比为m/z 264.1，替硝唑（内标）为m/z 248.0。加权（1/x²）校准曲线在血浆浓度范围1.00 - 400.00 ng/ml和尿液浓度范围0.01 - 16.00 μg/ml内呈线性，相关系数（r）分别为0.9995和0.9997。人血浆中的定量下限为1.00 ng/ml。血浆和尿液中的批内和批间精密度（CV%）均低于10%，三种浓度加标血浆样品的平均方法准确度和回收率分别为98.2%至100.1%和61.6%至62.9%。所建立的方法成功应用于测定人血浆和尿液中的曲马多，并为曲马多的临床药代动力学研究提供了合适的图谱。
