基于质谱-主成分分析法的冠心丹参胶囊中10个活性成分含量测定及质量评价研究  

Quantitative and quality evaluation research of multiple principal active components in Guanxin Danshen capsules by MS-principal component analysis

作　　者：周霖[1] 姜晓芳[1] 左莉华[1] 孙志[1] 刘新[1] 徐昙烨 王晓霞 贾萌萌[1] 康建[1] 张晓坚[1] ZHOU Lin JIANG Xiao-fang ZUO Li-hua SUN Zhi LIU Xin XU Tan-ye WANG Xiao-xia JIA Meng-meng KANG Jian ZHANG Xiao-jian(Pharmaceutical department, The First Affiliated Hospital of Zhengzhou University, Zhengzhou 450000, Chin)

机构地区：[1]郑州大学第一附属医院药学部,郑州450000

出　　处：《药物分析杂志》2017年第10期1824-1831,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：郑州大学第一附属医院创新基金项目(2015)

摘　　要：目的:建立同时测定冠心丹参胶囊中10个活性成分含量的质谱分析方法,并采用主成分分析技术综合评价该药物质量。方法:采用液质联用法(UPLC-MS/MS)分析检测,色谱柱为UPLC BEH C18(2.1 mm×50 mm,1.7μm),流动相为乙腈-0.1%甲酸水,梯度洗脱,流速为0.2 mL·min^(-1),ESI正、负离子同时采集,除熊果酸采用选择离子监测(SIR)外,其余9个成分均采用多反应监测(MRM);多批次冠心丹参胶囊含量测定结果采用多元数据处理软件SIMCA 14.0进行主成分分析。结果:在优化的色谱质谱条件下,丹参素、原儿茶醛、咖啡酸、迷迭香酸、丹酚酸B、丹酚酸A、丹参酮Ⅰ、隐丹参酮、丹参酮ⅡA、熊果酸质量浓度分别在50.0~500.0、2.4~24.0、0.2~2.0、8.0~80.0、6.0~60.0、1.0~10.0、8.0~80.0、12.0~120.0、10.0~100.0和1.0~10.0μg·mL^(-1)范围内线性关系良好(r≥0.999 6);加样回收率在98%~101%范围内,RSD小于3%;10批冠心丹参胶囊含量分别为3.060~3.914、0.279~0.358、0.021~0.028、0.610~0.839、0.655~0.835、0.087~0.106、0.883~1.111、1.073~1.393、0.972~1.170和0.071~0.095 mg·g^(-1);含量测定数据经SIMCA 14.0软件进行主成分分析,结果表明10批冠心丹参胶囊质量偏差均在标准偏差范围内。结论:该方法可用于冠心丹参胶囊中多种主要活性成分的快速测定;不同批次冠心丹参胶囊总体质量较为稳定。Objective：This study was aimed to establish a method for simultaneous determination of ten principal active components in Guanxin Danshen capsules,and to give a comprehensive evaluation of the quality of the drug by principal component analysis technology. Methods：The UPLC-MS/MS method was used and the chromatographic conditions were as follows：ACQUITY UPLC？ BEH C18（2.1 mm×50 mm,1.7 μm） column with gradient elution of acetonitrile-water（containing 0.1% formic acid） at a flow rate of 0.2 mL·min-1. Mass spectrometer conditions：A triple quadrupole mass spectrometer equipped with electrospray ionization source（ESI） was used in positive and negative ion modes,and multiple reaction monitoring（MRM） was performed except ursolic acid in selected ion recording（SIR） for quantitative analysis of the compounds. Determination results were evaluated by principal component analysis with multivariate data processing software SIMCA14.0. Results：Under the optimized conditions,danshensu,protocatechuic aldehyde,caffeic acid,rosmarinic,salvianolic acid B,salvianolic acid A,tanshinone I,cryptotanshinone,tanshinone ⅡA and ursolic acid showed good linearity in the range of 50.0-500.0 μg·mL-1,2.4-24.0 μg·mL-1,0.2-2.0 μg·mL-1,8.0-80.0 μg·mL-1,6.0-60.0 μg·mL-1,1.0-10.0 μg·mL-1,8.0-80.0 μg·mL-1,12.0-120.0 μg·mL-1,10.0-100.0 μg·mL-1 and 1.0-10.0 μg·mL-1,respectively（r≥0.999 6）. The recoveries ranged from 98%-101% with RSDs below 3%. And the contents in ten batches of Guanxin Danshen capsules were 3.060-3.914 mg·g-1,0.279-0.358 mg·g-1,0.021-0.028 mg·g-1,0.610-0.839 mg·g-1,0.655-0.835 mg·g-1,0.087-0.106 mg·g-1,0.883-1.11 mg·g-11,1.073-1.393 mg·g-1,0.972-1.170 mg·g-1 and 0.071-0.095 mg·g-1,respectively. The data was analyzed by SIMCA14.0 software,and the results showed that the quality deviation of the 10 batches of Guanxin Danshen capsules was below the standard deviation. Conclusion：The proposed method could be used for the rapid determination of various main active com

关 键 词：冠心丹参胶囊 丹参素 原儿茶醛 咖啡酸 迷迭香酸 丹酚酸 丹参酮 隐丹参酮 熊果酸 中成药活性成分测定 质量评价 超高效液相色谱-串联质谱 主成分分析 

分 类 号：R917[医药卫生—药物分析学]