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首页> 外文期刊>RSC Advances >Quantitative analysis of five toxic alkaloids in Aconitum pendulum using ultra-performance convergence chromatography (UPC2) coupled with mass spectrometry
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Quantitative analysis of five toxic alkaloids in Aconitum pendulum using ultra-performance convergence chromatography (UPC2) coupled with mass spectrometry

机译：使用超高性能收敛色谱（UPC2）与质谱法耦合的乌头文锤中五种有毒生物碱的定量分析

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摘要

A rapid and efficient ultra-performance convergence chromatography (UPC2) method coupled with electrospray ionization single quadrupole mass spectrometry (ESI-MS) was developed and validated for the simultaneous quantification of five diester diterpenoid alkaloid constituents (3-acetylaconitine, hypaconitine, deoxyaconitine, mesaconitine, aconitine) in Aconitum pendulum. Optimum separation was achieved on a BEH 2-EP C-18 column (2.1 x 150 mm i.d., 1.7 mu m particle) with a gradient elution of a mixture of A (supercritical CO2) and B (methanol containing 10 mmol L-1 ammonium acetate) and at a flow rate of 0.8 mL min(-1) within 3 minutes. Quantification was performed using mass spectrometry in a positive ion ionization mode and selected ion recording (SIR) mode. The influences of column, modifier, additive, column temperature, and back pressure were investigated. The five alkaloids were identified and quantified using a comparison of retention time, ultraviolet spectrum, molecular ion peak (obtained from a selective ion recording mode) and peak areas with the reference compounds. The method was validated through linearity, limits of detection, limits of quantification, precision, stability, repeatability, and accuracy. The validated method was applied to analyze A. pendulum, which provided a reference for the quality evaluation of A. pendulum.
机译：快速且高效的超高性能收敛色谱（UPC2）方法与电喷雾电离单倍压杆质谱（ESI-MS）耦合，并验证了同时定量五二酯二萜类生物碱成分（3-乙酰酰基发碱，低氧碱，脱氧遗币，乳尾，穴位）在乌头穴位。在A BE 2-EP C-18柱（2.1×150mM ID，1.7μm粒子）上实现了最佳分离，其梯度洗脱（超临界CO 2）和B的混合物（含有10mmol L-1铵的甲醇）的梯度洗脱乙酸盐）在3分钟内以0.8mL min（-1）的流速。使用质谱法在正离子电离模式和所选离子记录（SIR）模式中进行定量。研究了柱，改性剂，添加剂，柱温和背压的影响。使用保留时间，紫外光谱，分子离子峰（从选择性离子记录模式获得）和具有参考化合物的峰面积的比较来鉴定和定量五种生物碱。通过线性度，检测限，定量限制，精度，稳定性，可重复性和准确性来验证该方法。应用了验证的方法来分析A.摆锤，为摆锤的质量评估提供了参考。

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  • 来源
    《RSC Advances》 |2015年第126期|共7页
  • 作者

    Zhao Tang-Juan; Qi Huan-Yang; Chen Juan; Shi Yan-Ping;

  • 作者单位

    Chinese Acad Sci Lanzhou Inst Chem Phys Key Lab Chem Northwestern Plant Resources Lanzhou 730000 Peoples R China;

    Chinese Acad Sci Lanzhou Inst Chem Phys Key Lab Chem Northwestern Plant Resources Lanzhou 730000 Peoples R China;

    Chinese Acad Sci Lanzhou Inst Chem Phys Key Lab Chem Northwestern Plant Resources Lanzhou 730000 Peoples R China;

    Chinese Acad Sci Lanzhou Inst Chem Phys Key Lab Chem Northwestern Plant Resources Lanzhou 730000 Peoples R China;

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  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 化学;
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