摘要
目的建立同时测定桃核承气汤中苦杏仁苷、肉桂酸、大黄酸、大黄素、甘草酸含量的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)方法。方法采用Supelco Discovery C18色谱柱,流动相为乙腈-4 mmol/L甲酸铵水溶液(等度洗脱),采用电喷雾电离源,多反应离子监测(MRM),用于定量分析的苦杏仁苷、肉桂酸、大黄酸、大黄素及甘草酸检测离子对m/z分别为458.2→296.0、146.8→103.1、283.7→239.9、269.7→226.1、821.4→350.9。结果苦杏仁苷、肉桂酸、大黄酸、大黄素及甘草酸含量的质量浓度范围分别在0.0016~0.1024、0.0016~0.1024、0.0016~0.1024、0.0008~0.0512、0.0004~0.2560 ng范围内与各自的峰面积呈良好的线性关系(r=0.9987、0.9991、0.9995、0.9989、0.9986)。加样回收率在97.33%~105.33%范围内,RSD均低于2.69%。结论该法专属性强、快速灵敏,可用于桃核承气汤中苦杏仁苷、肉桂酸、大黄酸、大黄素及甘草酸的定量分析。
Objective To develop the UPLC-MS/MS method for the determination of amygdalin,cinnamic acid,rhein,emodin and glycyrrhizic acid in Taohe-Chengqi Decoction simutaneously.Methods The separation was performed on Supelco Discovery C18,and isocratic elution was carried out with mobile phase consisting of acetonitrile-4 mmol/L ammonium formate.The mass spectrometer was operated in the positive and negative ionization electrospray(ESI)mode using multiple monitoring(MRM)to analize of five ingredients.The precursor to product ion transitions monitored for amygdalin,cinnamic acid,rhein,emodin and glycyrrhizic acid were m/z 458.2→296.0,146.8→103.1,283.7→239.9,269.7→226.1 and 821.4→350.9,respectively.Results Amygdalin,cinnamic acid,rhein,emodin and glycyrrhizic acid were analyzed,the linear ranges were 0.0016-0.1024,0.0016-0.1024,0.0016-0.1024,0.0008-0.0512 and 0.0004-0.2560 ng,respectively.The r were 0.9987,0.9991,0.9995,0.9989 and 0.9986,respectively.The recovery of five analytes ranges from 97.33%to 105.33%and the Relative Standard Deviations were all below 2.69%.Conclusion This UPLC-MS/MS method is exclusive,rapid and sensitivewhich could be applied for the determination of amygdalin,cinnamic acid,rhein,emodin and glycyrrhizic acid in Taohe-Chengqi Decoction.
作者
郭佳宇
钱梦溪
Guo Jiayu;Qian Mengxi(Department of Pharmacy,Zhangjiagang Hospital Affiliated to Nanjing University of Chinese Medicine,Zhangjiagang 215600,China)
出处
《国际中医中药杂志》
2021年第9期893-897,共5页
International Journal of Traditional Chinese Medicine
