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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作者单位地址
张燕 西安市精神卫生中心 西安市长安区航天大道东段
张锁 西安市精神卫生中心 
丁靖 西安市精神卫生中心 
魏玮 西安市精神卫生中心 
赵彩萍 西安市精神卫生中心 
戴尊孝 西安市精神卫生中心 
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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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