Simultaneous determination of 11 components in Fufang Duzhong Jiangu Granules by ultra high performance liquid chromatography-tandem mass spectrometry
摘要
建立了超高效液相色谱-串联质谱(UHPLC-MS/MS)法同时测定复方杜仲健骨颗粒中毛蕊异黄酮葡萄糖苷、盐酸小檗碱、甜菜碱、人参皂苷Rb1、川续断皂苷Ⅵ、芍药苷、松脂醇二葡萄糖苷、人参皂苷Rg1、三七皂苷R1、人参皂苷Re和黄芪甲苷11种活性成分的含量.选用UPLC BEH C18 色谱柱(100 mm×2.1 mm,1.7 µm),流动相A为0.01%(V/V)甲酸-水溶液,B为0.01%(V/V)甲酸-乙腈,梯度洗脱.毛蕊异黄酮葡萄糖苷、盐酸小檗碱、甜菜碱、人参皂苷Rb1的离子源为电喷雾离子源正离子模式(ESI+),其余成分为电喷雾离子源负离子模式(ESI-),采用多反应监测(MRM)扫描模式检测.11个成分在一定浓度范围内与峰面积呈良好的线性关系(r=0.9974～0.9996),平均加样回收率为96.0%～104.5%,相对标准偏差(RSD)为0.7%～3.8%.本方法可用于复方杜仲健骨颗粒中多种活性成分的含量测定.
Anultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)method was established for the simultaneous determination of 11 active ingredients in Fufang Duzhong Jiangu Granules,including calycosin 7-O-β-D-glucopyranoside,berberine hydrochloride,betaine,ginsenoside Rb1,asperosaponinⅥ,paeoniflorin,pinoresinol diglucoside,ginsenoside Rg1,notoginsenoside R1,ginsenoside Re,and astragalosideⅣ.UPLC BEH C18 chromatography column(100 mm×2.1 mm,1.7 µm)was used,with mobile phase A of 0.01%(V/V)formic acid water solution and phase B of 0.01%(V/V)formic acid acetonitrile.Positive ion mode of electric spray ion source(ESI+)was used for the calycosin 7-O-β-D-glucopyranoside,berberine hydrochloride,betaine,and ginsenoside Rb1,while negative ion mode of electric spray ion(ESI-)source was used for the other components.Multiple reaction monitoring(MRM)scanning was used for the detection.The 11 components showed good linear relationships within their respectively concentration range(r=0.9974‒0.9996),with the average recoveries of 96.0%‒104.5%and the relative standard deviations(RSDs)of 0.7%‒3.8%.This method can be used for the determination of multiple active ingredients in Fufang Duzhong Jiangu Granules,providing reference for the improvement of quality control of Fufang Duzhong Jiangu Granules.
