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目的建立高效液相色谱-电雾式检测器(HPLC-CAD)同时测定知母根茎与须根中5种呋甾皂苷含量的方法。方法采用Tech Mate C18-ST-Ⅱ色谱柱(250 mm×4.6 mm,5μm);流动相:乙腈-水(22∶78,V/V);流速1.0 ml/min;柱温30℃;CAD检测器参数:采集频率10 Hz;雾化温度55℃;filter:5 s。结果知母中5种主要呋甾皂苷:知母皂苷N、知母皂苷L、知母皂苷BⅡ、25R-知母皂苷BⅡ和25S-officinalisnin-Ⅰ分别在一定范围内呈良好的线性关系,相关系数为0.9992~0.9998,检测限分别为0.28、0.92、0.92、0.92和0.92 ng,定量限分别为0.92、2.77、2.77、2.77和2.76 ng,精密度、重复性、48 h稳定性的RSD均<3.0%,平均加样回收率分别为98.17%、101.37%、98.53%、97.63%和98.17%。结论本研究建立的HPLC-CAD法重复性好,结果准确可靠,可作为中药知母多成分含量测定的方法。
OBJECTIVE To establish a method for the simultaneous determination of five furosetron saponins in rhizomes and fibrous roots of Rhizoma Anemarrhenae by high performance liquid chromatography-electrospray ionization detector (HPLC-CAD). Methods The mobile phase consisted of acetonitrile-water (22:78, V / V), flow rate of 1.0 ml / min, column temperature of 30 ℃ and column temperature of 30 ℃ with Tech Mate C18-ST-Ⅱ column (250 mm × 4.6 mm, Parameters: Acquisition frequency 10 Hz; atomization temperature 55 ℃; filter: 5 s. Results The five main furciferin saponins: timosaponin N, timosaponin L, timosaponin B Ⅱ, 25R-timosaponin B Ⅱ and 25S-officinalisnin-Ⅰ were in a certain range, respectively, a good linear relationship, the correlation The coefficients of quantification were 0.9992-0.9989. The limits of detection were 0.28, 0.92, 0.92, 0.92 and 0.92 ng, respectively. The limits of quantification were 0.92, 2.77, 2.77, 2.77 and 2.76 ng, respectively. The RSDs of precision, repeatability, 3.0%, the average recovery was 98.17%, 101.37%, 98.53%, 97.63% and 98.17%, respectively. Conclusion The HPLC-CAD method established in this study has good repeatability, accurate and reliable results and can be used as a method for determination of multi-component content of Chinese traditional medicine.