超高效液相色谱串联质谱同时测定瓦布贝母中6个生物碱成分  

Simultaneous Determination of Six Alkaloid Components in Fritillaria unibracteata var. wabuensis by UPLC-MS/MS

作　　者：耿昭[1] 吴强 苟琰 高必兴 齐景梁 周勤梅[1] 郭力[1] 周娟 WU Qiang;G0U Yan;GA0Bi-xing;QI Jmg-hang;ZHOU Qin-mei;GUO Li;ZHOU Juan(State Key Laboratory Breeding Base of Systematic Research,Development and Utilization of Chinese Medicine Resources,Chengdu University of Traditional Chinese Medicine,Chengdu 611137,China;Sichuan Institute for Food and Drug Control,Chengdu 611731,China)

机构地区：[1]成都中医药大学中药资源系统研究与开发利用省部共建国家重点实验室培育基地,成都611137 [2]四川省食品药品检验检测院,成都611731

出　　处：《中国实验方剂学杂志》2018年第24期95-100,共6页Chinese Journal of Experimental Traditional Medical Formulae

摘　　要：目的:建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定瓦布贝母中西贝母碱苷、西贝母碱、贝母辛、贝母素甲、贝母素乙和湖贝甲素的方法。方法:采用Agilent Eclipse XDB C18色谱柱(2. 1 mm×100 mm,1. 8μm),流动相0. 1%甲酸溶液(含0. 01 mol·L-1甲酸铵)-乙腈,梯度洗脱,柱温35℃,流速0. 4 m L·min-1;采用电喷雾离子源(ESI),正离子模式扫描,质谱多反应监测(MRM)模式检测; 6个生物碱成分的定量定性离子对为西贝母碱苷m/z 592. 4> 574. 4,138. 2,96. 1,西贝母碱m/z 430. 4> 412. 3,138. 2,96. 1,贝母辛m/z 430. 4> 412. 3,109. 2,67. 2,贝母素甲m/z 432. 4> 414. 4,95. 2,67. 2,贝母素乙m/z 430. 4> 412. 3,396. 3,91. 1,湖贝甲素m/z 416. 4> 98. 2,81. 2,67. 2。结果 6个成分在各自线性范围内线性关系良好(r> 0. 999 1),方法精密度、重复性、稳定性良好,加样回收率在98. 07%106. 62%,RSD均<5%。结果:样品测定结果表明各批次间6个成分含量差异较大,总体上西贝母碱和西贝母碱苷含量最高,贝母辛居中,贝母素乙、贝母素甲和湖贝甲素依次递减。结论:所建立的方法灵敏准确,适用于瓦布贝母中生物碱成分的含量测定,并为瓦布贝母药材的质量控制和综合评价提供方法依据。Objective:To establish an analytical method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)for the simultaneous determination of imperialine-3β- D-glucoside,imperialine,peimisine,vertieine,verticinone and hupehenine in Fritillaria unibracteata var. wabuensis.Method:The separation was carried out on Agilent Eclipse XDB C18(2.1mm × 100mm,1.8μm) with 0.1%formic acid solution (containing 0.01mool·L^-1 ammonium formate)-acetonitrile as mobile phase forgradient elution at a flow rate of 0.4mL·min^-l,and column temperature was 35℃ .The target components were detected in multiple reaction monitoring mode by mass spectrometry with electrospray ionization (ESI)source under positive mode.The quantitative and qualitative ion pairs of the six analytes were as follows:imperialine-3β-D- glucoside m/z 592.4>574.4,138.2,96.1,imperialine m/z 430.4>412.3,138.2,96.1,peimisine m/z 430.4>412.3,109.2,67.2,verticine m/z 432.4>414.4,95.2,67.2,verticinone m/z 430.4>412.3,396.3, 91.1,and hupehenine m/z 416.4>98.2,81.2,67.2.The results showed that good linearity was achieved in their respective linear ranges (r >0.9991),with good preeision,repeatability and stability.The average recovery ranged from 98.07% to 106.62%,and the RSD was less than 5%.Result:There were great differences in the content of 6 components between various batches.In general,the contents were highest for imperialine and imperialine-3β-D- glucoside,followed by peimisine,verticinone,vertieine and hupehenine progressively.Conclusion:The method is sensitive and accurate,and suitable for the simultaneous determination of multiple components in Fritillaria unibracteata var.wabuensis,providing a basis for its quality control and comprehensive assessment.

关 键 词：瓦布贝母 超高效液相色谱一串联质谱法 生物碱成分 含量测定 多反应监测 

分 类 号：R284.1[医药卫生—中药学] R289[医药卫生—中医学]