超高效液相串联质谱法同时测定葛根黄芩黄连汤中4种成分含量  

Simultaneous determination of four kinds of components in Gegen-Huangqin-Huanglian Decoction by UPLC-MS/MS

作　　者：施晓卉 蒋志涛[1] 张卫 黄丽华[1] 韩怡[1] 陈虹 钱丽[1] Shi Xiaohui;Jiang Zhitao;Zhang Wei;Huang Lihua;Han Yi;Chen Hong;Qian Li(Department of Pharmacy,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药学部,215600

出　　处：《国际中医中药杂志》2020年第9期895-899,共5页International Journal of Traditional Chinese Medicine

摘　　要：目的建立同时测定葛根黄芩黄连汤中黄芩苷、小檗碱、甘草酸、葛根素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ACE Excel 3 C18色谱柱(2.1 mm×100 mm, 3 μm),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),外标法定量分析。用于定量分析的黄芩苷、小檗碱、甘草酸及葛根素检测离子对m/z分别为447.0→271.0;336.2→320.2;821.4→350.9;415.2→294.9。结果黄芩苷、小檗碱、甘草酸及葛根素分别在0.002~0.080、0.002~0.080、0.001~0.040、0.002~0.080 ng范围内与峰面积线性关系良好(r=0.998 3、0.999 4、0.997 9、0.999 5)。加样回收率在98.75%~100.86%范围内,RSD均低于0.74%。结论该法专属性强、快速灵敏,可用于葛根黄芩黄连汤中黄芩苷、小檗碱、甘草酸及葛根素的含量测定。Objective To develop an UPLC-MS/MS method for the simultaneous determination of baicalin, berberine, glycyrrhizic acid and puerarin in Gegen-Huangqin-Huanglian Decoction. Methods Isocratic elution was carried out with mobile phase consisting of acetonitrile - 4 mmol/L ammonium formate. The separation was performed on ACE Excel 3 C18 (2.1 mm × 100 mm, 3 μm), and the mass spectrometer was operated in the positive and negative ionization electrospray (ESI) mode using multiple monitoring (MRM) for analysis of four components. External standard method was used for fix quantity. The precursor to product ion transitions monitored for baicalin, berberine, glycyrrhizic acid and puerarin were m/z 447.0→271.0, 336.2→320.2, 821.4→350.9 and 415.2→294.9, respectively. Results Baicalin, berberine, glycyrrhizic acid and puerarin were all analyzed exactly, the linear ranges were 0.002-0.080, 0.002-0.080, 0.001-0.040, 0.002-0.080 ng, respectively. The r were 0.998 3, 0.999 4, 0.997 9 and 0.999 5, respectively. The recoveries of four analytes ranged from 98.75% to 100.86% and the relative standard deviations were all below 0.74%. Conclusions UPLC-MS/MS method is sensitive, accuate with rapid speed, which could be used for the determination of baicalin, berberine, glycyrrhizic acid and puerarin in Gegen-Huangqin-Huanglian Decoction.

关 键 词：葛根黄芩黄连汤 串联质谱法 黄芩苷 小檗碱 甘草酸 葛根素 含量测定(中药) 

分 类 号：R284.1[医药卫生—中药学]