摘要
目的建立HPLC-MS/MS法测定人血浆中美洛昔康（meloxicam）的浓度。方法色谱柱为Phenomenex Luna C18（150 mm×4.6 mm,5μm）,流动相为乙腈-20 mmol·L-1醋酸铵水溶液（水中含体积分数为0.2%的甲酸）（体积比为70∶30）,提取剂为乙酸乙酯-异丙醇（体积比为9∶1）,内标物为吡罗昔康,离子源为ESI,流速为0.4 m L·min-1,柱温为30℃。结果美洛昔康线性为0.1~40.0μg·L-1（r=0.993 1）,定量下限为0.1μg·L-1,日间和日内精密度RSD均小于11.7%,提取回收率在83.4%~87.1%之间。20名健康受试者背部涂抹美洛昔康凝胶剂后,其主要药物动力学参数为：ρmax=（18.7±9.3）μg·L-1,tmax=（60.0±24.7）h,t1/2=（59.4±27.3）h,AUC0→t=（2 105.9±1 573.4）μg·h·L-1,AUC0→∞（2 297.1±1 734.7）μg·h·L-1。结论本方法适用于测定美洛昔康在人血浆中的浓度。
Objective To develop an HPLC-M S/M S method for determining the concentration of meloxicam in human phasma.Methods Separation was achieved on a reversed-phase C18 column with a mobile phase of acetonitrile-0.2%（φ） FA in water with 20 mmol·L-1ammonium acetate（V ∶ V = 7 ∶ 30）.Ethyl acetate-isopropyl alcohol was used as extraction agent.The flow rate was 0.4 m L·min-1and the column temperature was 30 ℃.Piroxicam was used as an internal standard.Results The calibration curve of meloxicam was linear in the concentration ranges of 0.1-40.0 μg·L-1（r = 0.993 1）.The lower limit of quantification was0.1 μg·L-1.The RSDs of inter-and intra-day were less than 11.7% and the average recovery of meloxicam was from 83.4% to 87.1%.The main pharmacokinetics parameters of meloxivam were as follow s：ρmax（18.7 ± 9.3） ng·m L-1,tmax（60.0 ± 24.7） h,t1/2（59.4 ± 27.3） h,AUC0→t（2 105.9 ± 1 573.4） μg·h·L-1,AUC0→∞（2 297.1 ± 1 734.7） μg·h·L-1.Conclusions This method is simple,quick with good reproducibility,and was suitable for determination of meloxicam in human plasma.
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2014年第12期993-997,共5页
Journal of Shenyang Pharmaceutical University
