UPLC-MS/MS法测定湖北贝母药材中的6种生物碱  

Determination of six alkaloid components in Fritillaria hupehensis by UPLC-MS/MS

作　　者：金丽鑫 耿昭 苟琰[1,2] 周娟 黄泽玮 JIN Lixin;GENG Zhao;GOU Yan;ZHOU Juan;HUANG Zewei(Sichuan Institute for Food and Drug Control,Chengdu,Sichuan,611731 P.R.China;Chengdu University of Traditional Chinese Medicine,Chengdu,Sichuan,611137 P.R.China)

机构地区：[1]四川省食品药品检验检测院,四川成都611731 [2]成都中医药大学药学院,四川成都611137

出　　处：《华西药学杂志》2020年第4期428-431,共4页West China Journal of Pharmaceutical Sciences

摘　　要：目的采用超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定湖北贝母中6种甾体生物碱的含量。方法经液-液萃取后,采用Agilent Eclipse XDB C18色谱柱(100 mm×2.1 mm,1.8μm),流动相为0.01 mol·L-1甲酸铵水溶液(含0.1%甲酸)-乙腈,梯度洗脱,质谱采用ESI+离子源,多反应监测(MRM)模式检测。结果湖北贝母中6种生物碱成分在一定浓度范围内线性关系良好(r>0.9991),方法精密度、重复性、稳定性良好,平均回收率为89.03%~104.55%,RSD<5%(n=6)。经测定,湖北贝母中贝母乙素的含量最高,约占6种成分总量的50%,贝母新碱、新贝母碱、贝母甲素依次减少,西贝素和西贝碱苷之和占总量的1%以下。结论所用方法能全面、准确地测定湖北贝母中6种生物碱成分的含量。该研究可为湖北贝母药材的质量控制、临床应用和综合评价提供依据。OBJECTIVE To establish a UPLC-MS/MS method for simultaneously determining 6 kinds of alkaloids in Fritillaria hupehensis.METHODS The separation was carried out on an Agilent Eclipse XDB C18(100 mm×2.1 mm,1.8μm)with gradient elution of water(with 0.1%formic acid and 0.01 mol·L-1 ammonium formate)and acetonitrile.The target components were detected in multiple reaction monitoring mode by mass spectrometry with electrospray ionization(ESI)source operated in positive mode.RESULTS The results showed that good linearity was achieved in their respective linear ranges and fine determination coefficient(r>0.9991).The method was validated with respect to precision,repeatability and stability.The average recovery ranged from 89.03%to 104.55%,and the RSD was less than 5%.There were great differences in the content of 6 components between various batches.In general,the content of verticinone in F.hupehensis was the highest,accounting for about 50 percent of the total of 6 components.Peimisine,hupehenine,verticine decreased,and the sum of imperialine and imperialine-3β-D-glucoside accounted for less than 1%of the total.CONCLUSION The method can determine 6 kinds of alkaloids in F.hupehensis accurately.It provides a scientific reference for quality control,clinic application and comprehensive assessment for F.hupehensis.

关 键 词：湖北贝母 超高效液相色谱-串联质谱法 生物碱成分 专属性 精密度 重复性 稳定性 含量测定 

分 类 号：R917[医药卫生—药物分析学]