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| 钩藤中生物碱HPLC-MS-AIS分析方法的建立 |
| Establishment of HPLC-MS-AIS method for the analysis in alkaloids in uncaria |
| 投稿时间：2021-09-07 修订日期：2022-07-14 |
| DOI： |
| 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 Isorhychophylline Dehydrouncarine Isodehydrouncarine Content determination |
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| 中文摘要: |
| 目的 建立高效液相-质谱联用-自体内标法（HPLC-MS-AIS），同时测定钩藤药材中4个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）的含量。方法 采用HPLC-MS-AIS法，C18色谱柱（3.0×50 mm,3.3 μm）；乙腈（B）-0.1％甲酸水溶液（A）为流动相；等度洗脱；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m/z 385.25→160.10（钩藤碱）；m/z 385.30→160.10（异钩藤碱）；m/z 383.25→160.15（去氢钩藤碱）；m/z 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、异去氢钩藤碱采用AIS法碰撞能量相同，建立的方法线性关系良好，线性范围分别为2.30～600 ng/mL(r=0.9993)；2.30～600 ng/mL(r=0.9992)；2.47～650 ng/mL(r=0.9994)；2.47～650 ng/mL(r=0.9992)，RSD<5.00％，准确度为95.20%～104.01%。结论 本研究建立同时测定钩藤药材中四种成分的HPLC-MS-AIS定量方法简便精确，可作为钩藤药材的质量控制的新手段。 |
| 英文摘要: |
| Objective To establish a high performance liquid chromatography-mass spectrometry (HPLC-MS-AIS) method for the simultaneous determination of four major indole alkaloids (Rhynchophylline, Isorhychophylline Dehydrouncarine, Isodehydrouncarine) in Uncaria. Methods HPLC-MS-AIS was used for the determination on C18 column (3.0×50 mm,3.3 μm). Acetonitrile (B) -0.1% formic acid aqueous solution (A) was the mobile phase; Isometric elution; Flow rate: 0.5 mL/min; Column temperature: 30℃. Mass spectrum conditions: electrospray ion source; Positive ion multi-reaction monitoring mode; Capillary voltage of 4000 V; m/z 385.25→160.10 (rhynchophylline) was selected; m/z 385.30→160.10 (isorhynchophylline); m/z 383.25→160.15 (dehydrouncarine); m/z 383.25→160.15 (isodehydrouncarine) was used as the detection ion pair. Injection volume: 2 μL. Results The AIS collision energies of rhynchophylline, isorhynchophylline, dehydrouncarine and isodehydrouncarine were the same, and the linear range of the established methods was 2.30-600 ng/mL(r=0.9993). 2.30 ~ 600 ng/mL(r=0.9992); 2.47 ~ 650 ng/mL(r=0.9994); 2.47-650 ng/mL(r=0.9992), RSD<5.0% , The accuracy were 95.20%～104.01%. Conclusion The HPLC MS-AIS method for simultaneous determination of four components in uncaria is simple, rapid and accurate, and can be used as a new method for quality control of uncaria . |
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