建立2D-HPLC同时检测钩藤碱、异钩藤碱、去氢钩藤碱、异去氢钩藤碱的方法
Establishment of 2D-HPLC method for simultaneous determination of rhynchophylline, isorhynchophylline, corynoxeine and isocorynoxeine
投稿时间:2021-09-08  修订日期:2022-09-20
DOI:
中文关键词:  钩藤碱  异钩藤碱  去氢钩藤碱  异去氢钩藤碱  二维高相液相色谱法
英文关键词:Rhynchophylline  Isorhynchophylline  Corynoxeine  Isocorynoxeine  Two dimensional high performance liquid chromatography
基金项目:
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
魏玮 西安市精神卫生中心 
苏艳丽 西安市精神卫生中心 
丁靖 西安市精神卫生中心 
张锁 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 
王慧 西安市精神卫生中心 
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中文摘要:
      目的 建立二维高效液相(2D-HPLC)同时检测钩藤碱、异钩藤碱、去氢钩藤碱、异去氢钩藤碱4种成分的方法。方法 采用Aston SC2(3.5 mm×25 mm,5 μm)一维色谱柱,Aston SH C18(3.5 mm×10 mm,5 μm)中间色谱柱,Aston SCB(4.6 mm×125 mm,5 μm)分析色谱柱,一维流动相为CAA-1,分析流动相为BPI-1﹕MPI-1﹕OPI=45﹕14﹕41,流速1.0 mL/min,柱温40℃,检测波长254 nm,进样量500 μL,分析时间9.5 min。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9.77~10 000 ng/mL(r=0.999 6);10.74~11 000 ng/mL(r=0.999 7);10.74~11 000 ng/mL(r=0.999 7);10.74~11 000 ng/mL(r=0.999 6),精密度、稳定性和重复性RSD<5.00%,准确度为95.20%~104.01%,方法回收率为93.63%~101.38%。结论 建立的2D-HPLC同时检测钩藤碱、异钩藤碱、去氢钩藤碱、异去氢钩藤碱四种生物碱含量的方法简单准确,可作为钩藤药材质量控制的新方法。
英文摘要:
      Objective Establishment of two-dimensional high performance liquid chromatography (2D-HPLC) method for simultaneous determination of rhynchophylline, isorhynchophylline, corynoxeine and isocorynoxeine. Methods Aston SC2 (3.5 mm × 25 mm, 5 μm) is as one dimensional column, Aston sh C18 (3.5 mm × 10 mm, 5 μm) is as Intermediate column, Aston SCB (4.6 mm × 125 mm, 5 μm) is as analysis column, the one-dimensional mobile phase is CAA-1, the analysis mobile phase is BPI-1:MPI-1:OPI = 45:14:41, the flow rate is 1.0 mL / min, the column temperature is 40 ℃, the detection wavelength is 254 nm, and the injection volume is 500 μL. The analysis time was 9.5 min. Results The linear ranges of rhynchophylline, isorhynchophylline, corynoxeine and isocorynoxeine were 9.77~10 000 ng/mL (r=0.999 6), 10.74~11 000 ng/mL (r=0.999 7), 10.74~11 000 ng/mL (r=0.999 7), 10.74~11 000 ng/mL (r=0.999 6). The RSD of precision, stability and repeatability were lower than 5.00%, the accuracy was 95.20%-104.01%. The method recoveries were 95.9%~104.6%. Conclusion 2D-HPLC method is simple and accurate for the determination of four alkaloids in uncaria, and can be used as a new method for quality control of uncaria.
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