液质联用法测定龙胆水煎剂中三种环烯醚萜的含量

目的利用液质联用（LC／MS／MS）方法测定龙胆水煎剂中环烯醚萜类化合物龙胆苦苷、獐牙菜苦苷和马钱苷的含量。方法色谱柱为J’Sphere ODS-H80（150mm×2．0mm，4μm）；流动相为甲醇-10mmol·L^-1醋酸铵溶液（30：70）；流速为200μl／min。样品经电喷雾离子源（ESI）正离子化后，通过三级四极杆串联质谱仪，采用多反应离子监测方式测定样品中龙胆苦苷（m／z 357．2-195．3）、獐牙菜苦苷（m／z 392．1→195．2）和马钱苷（m／z 408．4→229．1）浓度。结果在该分析条件下，3种化合物能够同时进行检测。龙胆苦苷浓度在200～5000ng·ml^-1范围内线性关系良好，回归方程为Y=1．26×10^3X＋2．27×10^3，r=0．9983；獐牙菜苦苷浓度在20-500ng·ml^-1范围内线性关系良好，回归方程为Y=360X＋144，r=0．9991；马钱苷浓度在20-500ng·ml^-1范围内线性关系良好，回归方程为Y=782X＋42．6，r=0．9994。对照品峰面积精密度RSD分别为龙胆苦苷2．52％，獐牙菜苦苷2．77％和马钱苷2．89％；平均加样回收率分别为龙胆苦苷98．2％，獐牙菜苦苷99．1％和马钱苷99．7％。结论该方法灵敏、准确、特异性强。

Determination of Three Iridoids in Decoction of Gentianae Sceabra Bge by LC/MS/MS

Aim To study simultaneous quantification of the individual content of three iridoids contained in decoction of Genfianae Scabra Bge by using an HPLC/MS/MS method. Methods A JSphere ODS-H80 column （ 150×2.0mm,4μm） was used in the HPLC separation with a mobile phase consisting of methanol and 10mmol·L^-1 NH4OAC （30： 70, V/V） at a flow rate of 200μl/min. A triple quadruple tandem mass spectrometer was used as the detector and an electrospray ionization source operated in the positive ion mode was applied. Gentiopicroside, swertiamarin and loganin were detected by monitoring the ion transition of m/z 357.2→195.3, m/z 392.1→195.2 and m/z 408.4→229.1 respectively. Restults Linear ranges were found to be 200 - 5 000ng·ml^-1 （ r = 0.998 3 ） for gentiopicroside, 20 - 500ng·ml^-1 （ r = 0.999 1 ） for swertiamarin and 20 - 500ng·ml^-1 （ r = 0.999 4 ） for loganin. The RSD of precision was 2.52% for gentiopicroside, 2.77% for swertiamarin, 2.89% for loganin, and the average recovery was found to be 98.2% , 99.1% and 99.7% with RSD of 2.60%, 2.97% and 1.91%, respectively. Conclusion The method was proved to be sensitive, accurate and specific.