Object:The establishment of a method for the detection of 12 quality markers in Angong Niuhuang Pill by ultraperformance 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.
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