Study on feeding of ophiopogon in granules based on HPLC-MS/MS method
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目的 建立超高效液相色谱-串联质谱法(Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry,HPLC-MS/MS)同时测定玄麦甘桔颗粒中山麦冬皂苷B和短葶山麦冬皂苷C的含量.方法 分析采用OMNI Orca C18 色谱柱(2.1×100 mm,2.6 μm),流动相 10 mmol·L-1 乙酸铵溶液(A)-甲醇(B),梯度洗脱模式,色谱柱温度为 40℃,进样量为 1 μL,电喷雾离子源(ESI),正负离子同时扫描模式,监测模式:MRM.结果 山麦冬皂苷B和短葶山麦冬皂苷C在各自范围内线性关系良好,r大于 0.9995,平均回收率为 99.78%.结论 该方法结果准确可靠,可以用于判断市售玄麦甘桔颗粒中麦冬的投料情况及为监管部分提供方法参考.
Objective To establish an HPLC-MS/MS method for the simultaneous determination of saponin B and C in Xuanmai Ganjie granules.Methods Omni Orca C18 column(2.1×100 mm,2.6 μm)was used for analysis.The mobile phase was 10 mmol·L-1 ammonium acetate solution(a)-methanol(b),gradient elution mode,column temperature was 40℃,sample volume was 1 μL,electrospray ion source(ESI)was used,positive and negative ion scanning mode,monitoring mode:MRM.Results There was a good linear relationship between saponin B and saponin C,R was greater than 0.9995,the average recovery was 99.78%.Conclusion The method is accurate and reliable.It can be used to determine the material of Ophiopogon japonicus in the commercial xuanmai Ganju granules and provide reference for the supervision.