[关键词]
[摘要]
目的 采用超高效液相色谱-四极杆飞行时间质谱技术分析不同产地槐角的主要共性成分和差异性成分。方法 BEH C18色谱柱(100 mm×2.1 mm,1.7 μm),0.1%甲酸水溶液-0.1%甲酸乙腈为流动相梯度洗脱;质谱采用电喷雾(ESI)离子源,在正、负离子模式下采集数据。通过Markerview 1.2.1软件提取11个产地样本中1 000个离子,按离子在所有样本中均出现,且相对强度基本大于1×104的原则选取共有离子;通过主成分分析找出不同产地槐角差异性特征化合物。通过Peakview 2.0/Masterview 1.0软件,依据精确质量数和同位素峰度比确定分子式,通过二级谱图比对、对照品裂解规律分析,结合文献报道,确定结构式。结果 鉴定或推断了不同产地槐角药材中共有的24个化合物的结构,以黄酮类成分为主,筛选并推断了21个差异性化合物的结构。结论 该方法检测快速、准确,为槐角药材的化学成分鉴定提供一种新的策略,主要共性成分的确定为质量评价指标选择及药效物质深入研究奠定了基础,差异成分亦可作为槐角药材产地鉴别及道地性评价的依据之一加以深入研究。
[Key word]
[Abstract]
Objective To identify the common compounds and variance compounds of Sophorae Fructus from different regions by ultra performance liquid chromatography coupled with time-of-fight mass spectrometry (UFLC-Q-TOF-MS). Methods The separation was performed on Waters Acquity UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm), with a mobile phase using water with 0.1% formic acid (A) and acetonitrile with 0.1% formic acid (B) for gradient elution; Q-TOF/MS and electrospray ion (ESI) source were applied for the analysis under the positive ion mode and the negative ion mode; 1 000 ions were extracted through Markerview 1.2.1 software from Sophorae Fructus of 11 different regions. And common ions (compounds) were selected according to the following principles:One ion can be detected in all samples, and most of the peak area was greater than the 1×104; The variance ions (compounds) were selected according to principal components analysis. The formula of common ions was then determined by accurate mass and isotopic abundance ratio from target screening function of Peakview 2.0/masterview 1.0 software, and its structure were determined by analysis of MS/MS fragment or comparison with standard substances and references. Results A total of 24 common compounds and 21 variance compounds were identified and inferred in Sophorae Fructus from different producing areas. Conclusion UPLC-Q-TOF/MS method which develops a new strategy can identify the main chemical constituents from Sophorae Fructus rapidly and accurately. The determination of the main common components lays a foundation for the selection of quality evaluation indexes and the in-depth study of pharmacodynamic substances. The variance components can also be used as one of the bases for the identification of origin and authentic evaluation of Sophorae Fructus.
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[基金项目]
国家中药材产业技术体系专项资金(CARS-21)