高效液相色谱-质谱法测定杜仲样品中环烯醚萜含量

Analysis of Iridoids in Eucommia Samples with High Performance Liquid Chromatography-Electrospray Ionization Mass Spectrometry

建立了液相色潜-质谱联用测定不同杜仲样品中3种环烯醚萜类物质含量的方法。以50％的甲醇-水为溶剂采用超声波提取样品中的环烯醚萜类物质．采用选择离子方式（SIR），以丰度最高的[M＋Na]^＋特征离子作为监测离子进行定性和定量分析。其质荷比（m／z）分别为369（桃叶珊瑚甙，AU）、397（京尼平甙酸，GPA）和411（京尼平甙，GP）。方法的线性范围分别为AU：0．11～1．10μg，GPA：0．24—2．40μg，GP：0．31-4．65μg；相关系数r分别为：0．999，0．999，0．996。检出限依次为0．3、0．4、0．3ng；进行4次平行测定，平均回收率分别为98％、100％和95％，RSD分别为2．8％、3．1％和2．9％。该方法操作简便，重复性好，专属性强，准确可靠，适用于对复杂的天然产物样品的定性和定量分析。

A method for determination of three kinds of Iridoids in different Eucommia samples by high performance liquid chromatography - electrospray ionization mass spectrometry （HPLC - ESI MS） was established. Samples were extracted in ultrasonic bath with methanol - water （50 ： 50 by volume）. The intense fragment ions [ M ＋ Na ]^＋ with m/z 369 for Aucubin, m/z 397 for Geniposidic acid, and m/z 411 for Geniposide were chosen as monitoring ions for qualitative and quantitative analysis. The calibration curves were linear over the concentration ranges of 0. 11 to 1.1μg for Aucubin, 0. 24 to 2. 4μg for Geniposidic acid, and 0. 31 to 4.65 μg for Geniposide, respectively. The correlation coefficients were 0. 999, 0, 999 and 0. 996. The limits of detection were 0. 3 ng, 0.4 ng and 0. 3 ng, respectively. The average recoveries were 98% , 100% , and 95% , RSD were 2.8% , 3.1% , and 2.9% （n =4）. This method was proved to be repeatable, specific, qualitative and quantitative analyses of complicated accurate, and easy to operate. It is adoptable for natural products.