UPLC-MS/MS法同时测定灯盏生脉胶囊中的11个活性成分的含量  

Simultaneous determination of eleven active components in Dengzhanshengmai capsules by ultra performance liquid chromatography with tandem mass spectrometry

作　　者：覃莎[1,2] 王锦[2] 朱平川[1] 徐远金[1,2] 

机构地区：[1]广西大学亚热带农业生物资源保护与利用国家重点实验室,南宁530004 [2]广西大学化学化工学院,南宁530004

出　　处：《药物分析杂志》2013年第8期1336-1341,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立超高效液相色谱-串联质谱法应用于灯盏生脉胶囊中11个活性成分的定量方法。方法:采用Agilent ZOR-BAX RRHD Eclipse Plus C18(2.1 mm×50 mm,1.8μm)色谱柱;以0.15%甲酸水溶液(A)-乙腈(B)为流动相,梯度洗脱,流速为0.35 mL.min-1;离子源为电喷雾电离源,采用正/负离子模式检测,多重反应监测模式采集并定量。结果:灯盏生脉胶囊中11个活性成分在30 min内达到基线分离,绿原酸、咖啡酸、灯盏花乙素、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、五味子醇甲、麦冬皂苷D、五味子酯甲、五味子甲素、五味子乙素的线性范围分别为0.0060～40、0.040～50、1.00～625、0.020～50、0.020～60、0.0020～40、0.0040～40、0.010～25、0.0020～40、0.00080～40、0.0012～48 mg.L-1各自质量浓度在相应的范围内与峰面积呈良好的线性关系,r>0.9990;检出限分别为1.5、10、2.0、5.0、5.0、0.50、1.0、2.5、0.50、0.20、0.30μg.L-1。11个成分的加样回收率为96.5%～105%,RSD(n=3)均小于3.0%。结论:本方法准确,灵敏,简便快速,重复性好,可用于灯盏生脉胶囊的质量控制。Objective： To develop a quantitative method for simultaneous determination of eleven effective components in Dengzhanshengmai capsules by ultra performance liquid chromatography with tandem mass spectrometry（UPLC-MS/MS）.Methods： The UPLC separation was performed on a ZORBAX RRHD Eclipse Plus C18column（2.1 mm ×50 mm,1.8 μm） by using water containing 0.15% formic acid and acetonitrile as the mobile phase with the gradient elution at a flow rate of 0.35 mL.min-1.The negative / positive ion mode was utilized for collection and quantification in a multiple reaction monitoring mode with icon source as the electrospray ionization（ESI） source.Results： Eleven active components in Dengzhanshengmai capsules were baseline separated in 30 minutes.Under the optimized conditions,the calibration curves were linear（r 0.9990） in the range of 0.0060-40 mg.L-1 for chlorogenic acid,0.040-50 mg.L-1 for caffeic acid,1.00-625 mg.L-1 for scutellarin,0.020-50 mg.L-1 for ginsenoside Rg1,0.020-60 mg.L-1 for ginsenoside Re,0.0020-40 mg.L-1 for ginsenoside Rb1,0.0040-40 mg.L-1 for schisandrin,0.010-25 mg.L-1 for ophiopogonin D,0.0020-40 mg.L-1 for schisantherin,0.00080 40 mg.L-1 for deoxyschizandrin,0.0012-48 mg.L-1 for γ-schisandrin with detection limits of 1.5,10,2.0,5.0,5.0,0.50,1.0,2.5,0.50,0.20,0.30 μg.L-1,respectively.The recoveries ranged from 96.5% to 105% with all relative standard deviations no more than 3.0%.Conclusion： The developed method is accurate,sensitive,simple,rapid and highly repeatable which can be used for quality control of Dengzhanshengmai capsules.

关 键 词：超高效液相色谱-串联质谱(UPLC-MS MS) 灯盏生脉胶囊 中成药活性成分 绿原酸 咖啡酸 灯盏花乙素 人参皂苷 麦冬皂苷 五味子素 

分 类 号：R917[医药卫生—药物分析学]