采用HPLC-MS-AIS法测定钩藤中四种生物碱含量  

Content determination of four kinds of alkaloids in Uncaria by HPLC-MS-AIS

作　　者：张燕[1,2] 张锁 丁靖 魏玮 赵彩萍 戴尊孝 Zhang Yan;Zhang Suo;Ding Jing;Wei Wei;Zhao Caiping;Dai Zunxiao(Xi'an Mental Health Center,Xi'an 710100,China;Xi'an Key Laboratory of Pharmacy(Mental Health),Xi'an 710100,China)

机构地区：[1]西安市精神卫生中心,陕西西安710100 [2]西安市药学(精神卫生)重点实验室,陕西西安710100

出　　处：《四川精神卫生》2022年第4期325-330,共6页Sichuan Mental Health

基　　金：西安市科技计划项目(项目名称:西安市药学(精神卫生)重点实验室,项目编号:201805051ZD2CG35)。

摘　　要：目的采用高效液相-质谱联用-自体内标法(HPLC-MS-AIS)测定钩藤中四种主要的吲哚类生物碱(钩藤碱、异钩藤碱、去氢钩藤碱、异去氢钩藤碱)含量。方法采用C_(18)色谱柱(3.0 mm×50 mm,3.3μm);0.1%甲酸水溶液∶乙腈=82∶18为流动相;流速0.5 mL/min;柱温30℃。质谱条件:电喷雾离子源;正离子多反应监测模式;毛细管电压为4000 v;选择质子数/电荷数(m/z):385.25/160.10(钩藤碱)、385.30/160.10(异钩藤碱)、383.25/160.15(去氢钩藤碱)、383.25/160.15(异去氢钩藤碱)作为检测离子对;进样量2μL。结果钩藤碱、异钩藤碱、去氢钩藤碱、异去氢钩藤碱线性范围分别为2.30~600.00 ng/mL(r=0.9993)、2.30~600.00 ng/mL(r=0.9992)、2.47~650.00 ng/mL(r=0.9994)、2.47~650.00 ng/mL(r=0.9992),精密度和稳定性的相对标准偏差(RSD)均<5.00%,准确度为92.40%~104.10%,加样回收率为95.90%~104.60%。结论采用HPLC-MS-AIS法测定钩藤中四种生物碱含量简便准确,可作为钩藤药材质量控制的新方法。Objective To determine the contents of four kinds of indole alkaloids(rhynchophylline,isorhynchophylline,corynoxeine,isocorynoxeine)in Uncaria by high-performance liquid chromatography-mass spectrometry-automatic internal standard(HPLC-MS-AIS).Methods Chromatographic separation was performed using C_(18) column(3.0 mm×50 mm,3.3μm),and the mobile phase,comprising 0.1% formic acid aqueous solution-acetonitrile(82∶18,V/V),was eluted at a flow rate of 0.5 mL/min and column temperature of 30℃.Mass spectrometric detection was performed using an electrospray ionization source and positive multiple-reaction monitoring mode at a voltage capillary of 4000 V.The mass-to-charge ratio(m/z)transition was 385.25/160.10 for rhynchophylline,385.30/160.10 for isorhynchophylline,383.25/160.15 for corynoxeine and 383.25/160.15 for isocorynoxeine,respectively.The injection volume was kept constant at 2μL.Results The linear concentration ranges of rhynchophylline,isorhynchophylline,corynoxeine and isocorynoxeine were 2.30~600.00 ng/mL(r=0.9993),2.30~600.00 ng/mL(r=0.9992),2.47~650.00 ng/mL(r=0.9994)and 2.47~650.00 ng/mL(r=0.9992),respectively.The relative standard deviation(RSD)of precision and stability were all lower than 5.00%,the accuracy ranged from 92.40% to 104.10%,and the average recovery was 95.90%~104.60%.Conclusion HPLC-MS-AIS method is simple and accurate for the determination of four kinds of alkaloids in Uncaria,and can be used as a new method for quality control of Uncaria.

关 键 词：HPLC-MS-AIS法 钩藤 钩藤碱 异钩藤碱 去氢钩藤碱 异去氢钩藤碱 含量测定 

分 类 号：R749[医药卫生—神经病学与精神病学]