高效液相色谱-电喷雾串联质谱法测定肿节风中异秦皮啶的含量

High-performance liquid chromatography-electrospray ionization/tandem mass spectrometr of isofraxidin in Sarcandra glabra

目的建立异秦皮啶的高效液相色谱-电喷雾串联质谱含量测定方法。方法肿节风药材及清热消炎宁胶囊中异秦皮啶分别用乙酸乙酯和氯仿萃取,以高效液相色谱-电喷雾串联质谱进行分析,多反应监测扫描,母/子离子对为223/162。结果异秦皮啶保留时间为6.60min,标准曲线在484-9680ng/ml范围内线性关系良好(r=0.9996),回收率96.7%,RSD4.49%,最低检测限1ng/ml。结论该方法快速、准确、选择性好,灵敏度高,可为异秦皮啶的含量测定提供参考。

Objective To establish a method for determining isofraxidin concentrations in Sarccmdra glabra and Qingrexiooyanning capsules with high-performance liquid chromatographic-mass spectrometry. Methods Isofraxidin was extracted from Sarcandra glabra and Qingrexiaoyanning capsules with acetic ether and chloroform, respectively, and separated by isocratic reversed-phase chromatography. The mass spectrometric system was operated in multiple reaction monitoring mode. A pair of ions： precursor ion m/z 223 with product ion m/z 162 were chosen for the quantification of the analyte. Results The retention time of isofraxidin was 6.60 min, and the calibration curve was linear over a concentration range from 484 to 9 680 ng/ml. The average recovery was 96.7% and RSD 4.49%, with detection limit of 1 ng/ml. Conclusion The method is rapid, selective and sensitive for determining isofraxidin in Sarcandra glabra and Qingrexiooyanning capsules.