【摘要】 目的:采用超高效液相色谱串联三重四级杆质谱（UPLC-QqQ-MS）技术对安宫牛黄丸中12种质量标志物进行含量检测方法的建立，为安宫牛黄丸的生物效应指标的质量评价奠定基础。方法:采用UPLC-QqQ-MS法，色谱条件：Waters CORTECS UPLC C18色谱柱（2.1mm×100mm, 1.6μm）,流动相乙腈（B）-0.1%甲酸水溶液（A）,梯度洗脱，流速0.25mL·min^-1；柱温45℃；进样量2μL。质谱条件：采用正负切换离子模式，多反应监测（MRM）模式进行检测方法构建。结果：利用UPLC-QqQ-MS法在12min内对安宫牛黄丸中包括：胆酸、去氧胆酸、鹅去氧胆酸、小檗碱、巴马汀、表小檗碱、黄芩苷、黄芩素、汉黄芩苷、栀子苷、异槲皮苷和京尼平苷酸等12种化学成分进行定量分析。各化学成分在考察的浓度范围内均具有良好的线性关系（r>0.9980），回收率均在97.6%～100.7%，其RSD在1.4%～3.4%范围内，且精密度、稳定性和重复性均符合分析要求。含量测定结果显示安宫牛黄丸12种化学成分中，胆酸、去氧胆酸、小檗碱、黄芩苷、汉黄芩苷和栀子苷的含量较高，其均值分别为4.522、1.870、6.634、6.365、1.402、3.390mg·g^-1。结论：本实验采用UPLC-QqQ-MS法高效，快速，全面地对安宫牛黄丸的12种质量标志物进行分析与含量测定，为安宫牛黄丸药效物质基础研究及生物效应质量评价奠定基础。更多还原

【Abstract】 Object:The establishment of a method for the detection of 12 quality markers in Angong Niuhuang Pill by ultra-performance liquid chromatography tandem triple quadrupole mass spectrometry（UPLC-QqQ-MS）, laid a foundation for the quality evaluation of the biological effect of Angong Niuhuang Pill. Methods:UPLC-QqQ-MS was used, Waters CORTECS UPLC C18 Column（2.1mm×100mm, 1.6μm）, mobile acetonitrile（B）-0.1% formic acid in water（A）, gradient elution, flow rate 0.25mL·min^-1; Column temperature 45℃; The injection volume was 2μL. In mass spectrometry, the detection method was constructed by using positive and negative switching ion modes and multiple reaction monitoring（MRM） modes. Results:UPLC-QqQ-MS method was used to quantitatively analyze 12 chemical components in Angong Niuhuang Pill, including cholic acid, deoxycholic acid, chenodeoxycholic acid, berberine, parmatine, epiberberine, baicalin, baicalin, baicalin, gardenin, isoquercitrin and genipine glycotide, within 12min. The chemical components had a good linear relationship（r>0.9980） in the concentration range examined, the recoveries were 97.6%～100.7%, and the RSD was in the range of 1.4%～3.4%, and the precision, stability and repeatability met the analytical requirements. The results showed that among the 12 chemical components of Angong Niuhuang Pill, the contents of bile acid, deoxycholic acid, berberine, baicalin, baicalin and gardenin were relatively high, and the average values were 3.445, 1.290, 4.712, 5.514, 1.112 and 2.779mg·g^-1, respectively. Conclusion:In this study, UPLC-QqQ-MS method was used to analyze and determine the content of 12 quality markers of Angong Niuhuang Pill, the method was efficient, rapid and comprehensive, which laid a foundation for the pharmacodynamic substances and quality evaluation of Angong Niuhuang Pill.更多还原