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目的建立同时测定丹灯通脑软胶囊中9种活性成分(丹参素、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)量的UPLC-MS/MS分析方法,并采用模式识别技术综合评价其药物质量。方法采用UPLC-MS/MS分析检测,色谱柱为Acquity UPLC?BEH C18(50 mm×2.1 mm,1.8μm),流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,体积流量为0.2 m L/min,ESI正、负离子同时采集,除熊果酸为选择离子监测(SIR)外,其余8种成分均为多反应监测(MRM);多批次丹灯通脑软胶囊定量测定结果采用多元数据处理软件SIMCA 14.0进行模式识别分析,并评价其质量。结果在优化的色谱质谱条件下,丹参素、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、熊果酸分别在100.0~1 000.0、1.0~10.0、8.0~80.0、120.0~1 200.0、15.0~150.0、40.0~400.0、10.0~100.0、10.0~100.0、1.2~12.0μg/m L线性关系良好(r≥0.999 6);加样回收率在98%~101%,RSD小于3%;10批丹灯通脑软胶囊中各成分的平均量分别为(4.854±0.314)、(0.063±0.005)、(0.764±0.070)、(12.937±0.648)、(1.954±0.178)、(3.623±0.221)、(0.720±0.062)、(1.437±0.116)、(0.073±0.007)mg/g;定量测定数据经SIMCA 14.0软件进行分析,分析结果表明10批丹灯通脑软胶囊质量偏差均在2 SD(标准偏差,standard deviation,SD)范围内。结论建立的UPLC-MS/MS定量分析方法简便、灵敏度高且准确性好,可用于丹灯通脑软胶囊中多种主要活性成分的快速测定;定量测定结果表明不同批次丹灯通脑软胶囊总体质量较为稳定,结果分析使用的多元数据模式识别方法可从整体上综合评价药物质量,为丹灯通脑软胶囊的质量控制研究提供新的科学依据和数据处理方法。
Objective To establish a method for the simultaneous determination of nine active ingredients (danshensu, caffeic acid, rosmarinic acid, salvianolic acid B, salvianolic acid A, tanshinone I, cryptotanshinone, tanshinone IIA, ursolic acid) Amount of UPLC-MS / MS analysis methods, and the use of pattern recognition technology to evaluate the quality of their drugs. The method was analyzed by UPLC-MS / MS. The mobile phase consisted of Acquity UPLC-BEH C18 (50 mm × 2.1 mm, 1.8 μm) with a mobile phase of acetonitrile-0.1% formic acid and eluted with a gradient of 0.2 m L / min, ESI positive and negative ions were collected at the same time. Except for ursolic acid as selective ion monitoring (SIR), the other 8 components were all MRM. The results of multiple quantitative determination of Dandengtongntong soft capsules were analyzed by multivariate data Processing software SIMCA 14.0 performs pattern recognition analysis and evaluates its quality. Results Under the optimized chromatographic and mass spectrometric conditions, the concentrations of danshensu, caffeic acid, rosmarinic acid, salvianolic acid B, salvianolic acid A, tanshinone I, cryptotanshinone, tanshinone IIA and ursolic acid were in the range of 100.0-1000.0,1.0 ~ 10.0,8.0 ~ 80.0,120.0 ~ 1 200.0,15.0 ~ 150.0,40.0 ~ 400.0,10.0 ~ 100.0,10.0 ~ 100.0,1.2 ~ 12.0μg / m L (r≥0.9996) 98% ~ 101% and RSD less than 3% respectively. The average amounts of each component in 10 batches of Dan Dengtongnao soft capsules were (4.854 ± 0.314), (0.063 ± 0.005), (0.764 ± 0.070) and (12.937 ± 0.648) (1.954 ± 0.178), (3.623 ± 0.221), (0.720 ± 0.062), (1.437 ± 0.116) and (0.073 ± 0.007) mg / g, respectively. The quantitative analysis data were analyzed by SIMCA 14.0 software. The quality deviation of Dengtong Soft Capsule is within 2 SD (standard deviation, SD). Conclusion The established UPLC-MS / MS quantitative analysis method is simple, sensitive and accurate, and can be used for the rapid determination of a variety of major active ingredients in Dan Dengtongnao soft capsules. Quantitative determination results show that different batches of Dan Deng Tong brain soft capsules The overall quality is relatively stable. The multivariate data pattern recognition method used in the result analysis can comprehensively evaluate the drug quality, providing a new scientific basis and data processing method for the quality control of Dandeng Tongnao Soft Capsule.