超高效液相串联质谱法同时测定膈下逐瘀汤中6种成分含量  

Simultaneous determination of six kinds of components in Gexia-Zhuyu Decoction by UPLC-MS/MS

作　　者：姚春娣 郁金芬[1] 温玲[1] 张建亚[1] 朱澄漪[1] Yao Chundi;Yu Jinfen;Wen Ling;Zhang Jianya;Zhu Chengyi(Department of Gynecology,Zhangjiagang Hospital Affiliated to Nanjing University of TCM,Zhangjiagang 215600,China)

机构地区：[1]南京中医药大学附属张家港医院妇科,215600

出　　处：《国际中医中药杂志》2020年第10期991-995,共5页International Journal of Traditional Chinese Medicine

基　　金：张家港市科技支撑计划(社会发展)项目(ZKS1830)。

摘　　要：目的:建立同时测定膈下逐瘀汤中芍药苷、川芎嗪、川陈皮素、丹皮酚、苦杏仁苷及藁本内酯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Waters XTerra MS C18柱(2.1 mm×50 mm, 3.5 μm),流动相为甲醇-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),外标法定量分析。用于定量分析的芍药苷、川芎嗪、川陈皮素、丹皮酚、苦杏仁苷及藁本内酯检测离子对 m/z分别为525.0→449.1;137.1→55.1;403.0→373.0;167.2→149.4;456.5→323.3;191.1→91.1。 结果:芍药苷、川芎嗪、川陈皮素、丹皮酚、苦杏仁苷及藁本内酯含量的质量浓度范围分别在0.000 2~0.012 8、0.000 8~0.051 2、0.000 1~0.006 4、0.000 2~0.012 8、0.000 6~0.038 4、0.000 1~0.006 4 ng范围内与各自的峰面积呈良好线性关系( r=0.999 3、0.997 5、0.999 6、0.992 6、0.995 5、0.999 1)。加样回收率在98.00%~105.30%范围内, RSD均低于2.47%。 结论:该法专属性强、快速灵敏,可用于膈下逐瘀汤中芍药苷、川芎嗪、川陈皮素、丹皮酚、苦杏仁苷及藁本内酯的含量测定。Objective To develop an UPLC-MS/MS method for the determination of paeoniflorin,tetramethylpyrazine,nobiletin,paeonol,amygdalin and ligustilide in Gexia-Zhuyu Decoction.Methods Isocratic elution was carried out with mobile phase consisting of methanol-4 mM ammonium formate.The separation was performed on Waters XTerra MS C18(2.1 mm×50 mm,3.5μm),and the mass spectrometer was operated in the positive and negative ionization electrospray(ESI)mode using multiple monitoring(MRM)for analysis of six components.Quantitative analysis by external standard method.The precursor to product ion transitions monitored for paeoniflorin,tetramethylpyrazine,nobiletin,paeonol,amygdalin and ligustilide were m/z 525.0→449.1,137.1→55.1,403.0→373.0,167.2→149.4,456.5→323.3 and 191.1→91.1,respectively.Results Paeoniflorin,tetramethylpyrazine,nobiletin,paeonol,amygdalin and ligustilide were all analyzed exactly,the linear ranges were 0.0002-0.0128,0.0008-0.0512,0.0001-0.0064,0.0002-0.0128,0.0006-0.0384,0.0001-0.0064 ng,respectively.The r were 0.9993,0.9975,0.9996,0.9926,0.9955 and 0.9991,respectively.The recoveries of six analytes ranged from 98.00%to 105.3%and the relative standard deviations(RSD)were all below 2.47%.Conclusions This method was sensitive,which could be applied for the determination of paeoniflorin,tetramethylpyrazine,nobiletin,paeonol,amygdalin and ligustilide in Gexia-Zhuyu Decoction.

关 键 词：膈下逐瘀汤 串联质谱法 芍药苷 川芎嗪 川陈皮素 丹皮酚 苦杏仁苷 藁本内酯 含量测定(中药) 

分 类 号：R286.0[医药卫生—中药学]