[关键词]
[摘要]
目的 建立超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定扶正化瘀胶囊(FHC)中12种成分(丹参素钠、原儿茶酸、原儿茶醛、咖啡酸、迷迭香酸、五味子醇甲、五味子醇乙、隐丹参酮、五味子甲素、丹参酮IIA、五味子乙素、五味子丙素)的定量方法。方法 选用Acquity UPLC? HSS T3色谱柱,以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,体积流量为0.3 mL/min,柱温45 ℃。质谱条件:ESI源,采用多反应检测模式(MRM),以保留时间及定性离子对之间的相对丰度定性,以定量离子对峰面积进行定量。结果 12种成分在进样质量浓度范围内呈现良好的线性关系(r>0.999 0),该方法回收率在97.1%~107%,RSD<2.0%(n=5)。结论 该方法快速、简便、重复性好,可用于同时测定FHC中多种成分。
[Key word]
[Abstract]
Objective To develop a ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of twelve major components (sodium danshensu, protocatechuic acid, protocatechuic aldehyde, caffeic acid, rosmarinic acid, schisandrin, schisandrol B, cryptotanshinone, deoxyschizandrin, tanshinone IIA, schisandrin B, and schisandrin C) in Fuzheng Huayu Capsules (FHC). Methods Chromatographic column: Acquity UPLC? HSS T3, mobile phase: acetonitrile-water (including 0.1% formic acid), and gradient elution, flow rate: 0.3 mL/min, column temperature: 45 ℃. MS condition: electrospray ionization (ESI) and multiple reaction monitoring (MRM) were adopted, the retention time and detected relative abundance of ion pairs were used for qualitative determination, the detected peak areas of ion pairs were used for quantitative determination. Results Good linear relationships of 12 components were provided over the investigated concentration ranges (r > 0.999 0). The overall average recovery rates were in the range of 97.1%-107% and RSD < 2.0% (n = 5). Conclusion The method is rapid, simple, repeatable, and can be used to determine the multi components in different batches of FHC simultaneously.
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[基金项目]
国家重点基础研究发展计划“973”项目(2006CB504801);上海市自然科学基金项目(10ZR1431000);上海市教育委员会E-研究院建设项目(E-03008);中国博士后基金(2012M520921);上海市博士后基金(12R21415400)