HPLC-MS测定人血浆中美利曲辛及其在生物等效性研究中的应用

目的 建立测定人血浆中美利曲辛浓度的高效液相色谱-质谱联用法,并用于氟哌噻吨美利曲辛片的生物等效性研究.方法 血浆样品用乙酸乙酯萃取,采用Thermo Hypersil-HyPURITY C13色谱柱(150 mm×2.1mm,5μm)分离,以50 mmol·L-1乙酸铵溶液(pH=4.0)-甲醇-乙腈(45∶36∶19)为流动相,流速为0.22 mL·min-1.采用高效液相色谱-质谱电喷雾电离法,选择离子监测(SIM).结果 美利曲辛在0.4～50.0 μg·L-1线性关系良好,平均回收率为98.6％,日内RSD≤7.8％,日间RSD≤6.0％.结论 该方法准确、灵敏度高,适用于含美利曲辛制剂的人体药动学和生物等效性研究.

Determination of melitracen in human plasma by HPLC-MS and its bioequivalence

Objective To develop a high performance liquid chromatography-mass spectrometry(HPLC-MS) method for the determination of melitracen in human plasma and study its bioequivalence.Methods Melitracen concentration in the plasma was determined by HPLC-MS.Melitracen were extracted from the plasma by liquid-liquid extraction,and the separation was performed on a Thermo Hypersil-HyPURITY C18 column,using the mobile phase consisting of 50 mmol·L-1 ammonium acetate(pH=4.0)-methanol-acetonitrile(45∶36∶19) with a flow rate of 0.22 mL·min-1.The compounds were ionized in the electrospray ionization(ESI) ion source of the mass spectrometer and detected in the selected ion recording(SIR)mode.Results The calibration curve was linear at 0.4-50.0 μg·L-1(r=0.999 3),the average recovery was 98.6%,the RSDs of intra-and inter-day were less than 7.8% and 6.0%.Conclusion The method is accurate and sensitive for the determination of melitracen in human plasma.