| 张燕,张锁,丁靖,魏玮,赵彩萍,戴尊孝.采用HPLC-MS-AIS法测定钩藤中四种生物碱含量[J].四川精神卫生杂志,2022,35(4):325-330.Zhang Yan,Zhang Suo,Ding Jing,Wei Wei,Zhao Caiping,Dai Zunxiao,Content determination of four kinds of alkaloids in Uncaria by HPLC-MS-AIS[J].SICHUAN MENTAL HEALTH,2022,35(4):325-330 |
| 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 |
| 投稿时间：2021-09-07 |
| DOI：10.11886/scjsws20210907004 |
| 中文关键词: 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 |
| 英文关键词:HPLC-MS-AIS method Uncaria Rhynchophylline Isorhynchophylline Corynoxeine Isocorynoxeine Content determination |
| 基金项目: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） |
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| 中文摘要: |
| 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C18色谱柱（3.0 mm×50 mm，3.3 μm）；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4 000 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2 μL。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=0.999 3）、2.30~600.00 ng/mL（r=0.999 2）、2.47~650.00 ng/mL（r=0.999 4）、2.47~650.00 ng/mL（r=0.999 2），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。 |
| 英文摘要: |
| 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 C18 column （3.0 mm×50 mm， 3.3 μm）， 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 4 000 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 2 μL.Results The linear concentration ranges of rhynchophylline， isorhynchophylline， corynoxeine and isocorynoxeine were 2.30~600.00 ng/mL （r=0.999 3）， 2.30~600.00 ng/mL （r=0.999 2）， 2.47~650.00 ng/mL （r=0.999 4） and 2.47~650.00 ng/mL （r=0.999 2）， 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. |
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