LC-MS/MS法同时测定知母提取物中7种成分的含量

Simultaneous Determination of Seven Components in Anemarrhena asphodeloides Extract by Liquid Chromatography-tandem Mass Spectrometry

建立了LC-MS/MS法同时测定知母提取物中7种活性成分(新芒果苷、芒果苷、异芒果苷、知母皂苷BⅡ、宝藿苷Ⅰ、知母皂苷AⅢ、菝葜皂苷元)含量的分析方法。采用SB-C18色谱柱,流动相A为0.1%甲酸溶液(含10 mmol/L甲酸铵),流动相B为乙腈,线性梯度洗脱;采用电喷雾离子(ESI)源、正离子扫描模式、多反应监测条件下进行定量分析。结果表明,所测7种成分的分离度良好,在相应浓度范围内线性良好,7种成分的定量限和检测限分别在0.02~0.63 ng/ml和0.01~0.29 ng/ml范围内。精密度、重复性、稳定性的RSD(n=5)均小于4%;平均加样回收率在90.9%~108.9%,RSD(n=9)均小于4.5%。该方法可靠、准确、快速、重复性好,可用于知母中7种成分的含量测定,并为知母药材的质量控制提供依据。

A LC-MS/MS method was established for simultaneous determination of the seven active components(neomangiferin,mangiferin,isomangiferin,timosaponin BⅡ,baohuosideⅠ,timosaponin AⅢand sarsasapogenin)in Anemarrhena asphodeloides extract.A SB-C18 chromatographic column was used,with the mobile phase A(0.1%formic acid solution containing 10 mmol/L ammonium formate)and mobile phase B(acetonitrile)by linear gradient elution.The seven components were detected and quantified by electrospray ion(ESI)source in the positve mode under multi-reaction monitoring(MRM)condition.The results showed that the resolution of seven components was good and it was linear for the seven components in the corresponding concentration ranges.The LOQs and LODs of the seven components were 0.02-0.63 ng/ml and 0.01-0.29 ng/ml,respectively.The RSDs(n=5)of precision,repeatability and stability were all less than 4%.The average recovery rates were between 90.9%and 108.9%,and the RSDs(n=9)were all less than 4.5%.The method was reliable,accurate,fast,and repeatable,which could be used to determine the content of the seven components in Anemarrhena asphodeloides and provided a reference for the quality control of Anemarrhena asphodeloides.