HPLC-MS/MS测定大鼠血浆中丹参素钠的浓度

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

目的建立液质联用色谱法(HPLC-MS/MS)测定SD大鼠血浆中丹参素钠的浓度。方法血浆样品采用液液萃取方法进行预处理。色谱柱为Diamonil C_(18)柱(4.6mm×200mm,5μm);流动相为甲醇-水(含0.01‰甲酸)=(80:20);流速为1.0ml/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→135m/z和253→209m/z。结果丹参素钠在10.6～1060ng/ml检测浓度范围内呈良好的线性关系(r=0.9996),最低定量限为10.6ng/ml,日内和日间精密度的RSD<7.8%,回收率在99%到102%之间。结论该方法灵敏度高、快速、简单、准确,适用于血浆样品中丹参素钠的含量测定以及临床前实验研究。

Objective To estiblish a method of determining sodium Danshensu in rat plasma by HPLC-MS/MS.Methods sodium Danshensu was extrated for determination by HPLC-MS/MS.Analytical column was Diamonsil C18（4.6 mm×200 mm,5μm）.The mobile phase was methanol：water（0.01‰formic acid ） = 80：20.Mass spectrum conditions were ESI performing in the MRM mode using target ions m/z 197→135（Sodium Danshensu）,m/z 253→209（keloprofen）.Results The calibration curve was liner over the range of 10.6～1 060 ng/ml.The LLOQ ol sodium Danshensu in plasma was 10.6 ng/ml.The intra-day and inter-day RSD were〈7.8%.The extracted recovery was ranged from 99%to 102%.Conclusion The method was sensitive,rapid,simple and accurate to sodium Danshensu plasma concertration and suitable to study preclinical test of sodium Danshensu.