HPLC-MS/MS 测定大鼠肝脏组织中丹参素钠的浓度

目的 建立液质联用色谱法(HPLC-MS/MS)测定SD大鼠肝脏组织中丹参素钠的浓度。 方法 肝脏组织样品制成匀浆后,加入内标酮洛芬,采用液液萃取方法进行预处理。色谱柱:Diamonsil C₁₈柱(200 mm×4.6 mm ,5 μm);流动相:甲醇-水(含0.01‰甲酸)(80:20);流速:1.0 ml/min;质谱条件:采用ESI离子源,负离子检测,选择MRM 测定丹参素钠和酮洛芬197→135 m/z 和 253→209 m/z。 结果 丹参素钠在20.2~1 010 n

Determination of sodium Danshensu in rat liver by HPLC-MS/MS

Objective To establish a HPLC-MS/MS method for determination of sodium Danshensu in SD rat liver.Methods Tissue samples were pretreated by liquid-liquid extraction method after homogenate,and ketoprofen was used as the internal standard.Analytical column was Diamonsil C18(200 mm×4.6 mm,5 μm).The mobile phase was methanol: water(0.01‰ formic acid)=8020 with flow rate as 1.0 ml/min.Mass spectrum determination was performed in the MRM mode with target ions m/z 197→135(Sodium Danshensu),m/z 253→209(ketoprofen),using ESI ion resource and negative ion detection.Results The calibration curve was linear over the range of 20.2～1 010 ng/ml.The LLOQ of sodium Danshensu in liver was 20.2 ng/ml.The intra-and inter-day RSD were both less than 10%.The extracted recovery rate ranged from 92% to 107%.Conclusion The method was sensitive,rapid,simple and accurate to determine sodium Danshensu distribution in rat liver and was suitable for preclinical test of Sodium Danshensu.