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Development of an analytical method for twelve dioscorea saponins using liquid chromatography coupled to Q-Exactive high resolution mass spectrometry
Talanta ( IF 5.6 ) Pub Date : 2018-08-14 , DOI: 10.1016/j.talanta.2018.08.040
Huawen Qi , Feng Feng , Junfeng Zhai , Fengming Chen , Tong Liu , Feifang Zhang , Feng Zhang

A rapid method using liquid chromatography coupled to Q-Exactive high resolution mass spectrometry was developed for determination of twelve dioscorea saponins in Polygonti Rhizome. The separation was performed on a Alorich Ascentis C8 column (100 mm × 4.6 mm, 3 µm) with gradient elution of water and acetonitrile. All calibration curves showed good linear regression (r2 >0.9947) within the linear range. The limits of detection and quantitation were in the range of 0.3–1.0 ng/mL and 1.0–3.0 ng/mL, respectively. The intra- and inter-day precision (RSD) were below 8.85% (n = 6) and 9.15% (n = 6), respectively. The recovery for the target compounds was within the range of 80.34–108.05%. The fragmentation pathways of twelve saponins were summarized in both positive and negative modes. The saponins which contain the same substituent groups and the different skeletons showed the same precursor ions and the similar fragmentation patterns in positive mode. However, different types of saponins can be distinguished in negative mode by the characteristic ions. The proposed method was applied to analyze six batches of Polygonti Rhizome samples for target compounds. This work promoted the quality control method for raw material or preparations which contain dioscorea saponins.



中文翻译:

液相色谱-Q-主动高分辨率质谱联用技术开发十二种薯os皂苷的分析方法

建立了一种使用液相色谱与Q-Exactive高分辨率质谱联用的快速方法,用于测定虎杖中的十二种薯os皂苷。在Alorich Ascentis C8色谱柱(100 mm×4.6 mm,3 µm)上进行分离,并用水和乙腈进行梯度洗脱。所有校准曲线均显示出良好的线性回归(r 2> 0.9947)。检测限和定量限分别在0.3–1.0 ng / mL和1.0–3.0 ng / mL的范围内。日内和日间精度(RSD)分别低于8.85%(n = 6)和9.15%(n = 6)。目标化合物的回收率在80.34–108.05%之间。总结了十二种皂苷的正向和负向断裂途径。含有相同取代基和不同骨架的皂苷在正离子模式下显示相同的前体离子和相似的碎片模式。但是,不同类型的皂苷可以通过特征离子在负离子模式下进行区分。该方法用于分析六批次的虎杖样品中的目标化合物。

更新日期:2018-08-14
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