散结灵胶囊中松香酸的HPLC与UPLC-MS/MS检测方法研究

Determination of Abietic Acid in Sanjieling Capsules by HPLC and UPLC-MS/MS

目的:建立散结灵胶囊中非法添加松香酸的HPLC与UPLC-MS/MS检测方法。方法:采用Shiseido Capcell Pak C18色谱柱(250 mm×4.6 mm,5μm),流动相为0.1%甲酸-乙腈-四氢呋喃(40∶40∶20),流速为1.0 ml·min^-1,检测波长为241nm,柱温为30℃。同时采用UPLC-MS/MS方法对松香酸进一步确认,色谱柱为Agilent Poroshell 120 EC-C18柱(2.1 mm×50mm,2.7μm),流动相为0.1%甲酸-乙腈(32∶68),流速为0.2 ml·min^-1,离子化模式为ESI+扫描,碰撞能量15 ev。结果:松香酸在4.07~407.20μg·ml^-1(r=0.999 9)范围内线性关系良好,平均回收率为99.73%,RSD为0.53%(n=9)。结论:该方法简便、准确、重复性好,适用于散结灵胶囊中非法添加松香酸的检测。

Objective: To establish HPLC and UPLC-MS/MS methods to determine abietic acid in Sanjieling capsules.Methods:Using a column of Shiseido Capcell Pak C18(250 mm × 4.6 mm,5 μm) with 0.1% formic acid-acetonitrile-tetrahydrofuran(40∶40∶20) as the mobile phase at the flow rate of 1.0 ml·min^-1,the detection wavelength was 241 nm,and the column temperature was30℃.Meanwhile,in order to further confirm abietic acid,a UPLC-MS/MS method was used and performed on a column of Agilent Poroshell 120 EC-C18(2.1 mm×50 mm,2.7 μm) with the mobile phase of 0.1% formic acid-acetonitrile(32∶ 68) at the flow rate of0.2 ml·min^-1.The ionization mode was ESI+,and the collision energy was 15 ev.Results: The linear range of abietic acid was4.07-407.20 μg·ml^-1(r=0.999 9),and the average recovery was 99.73%(RSD=0.53%,n=9).Conclusion: The method is simple,accurate and reproducible,which can be used for the determination of abietic acid illegally added to Sanjieling capsules.