Wang Hong, Wu Qinan, Wu Chengying, Jiang Zheng
The College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing, Jiangsu 210023, PR China.
The College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing, Jiangsu 210023, PR China Jiangsu Collaborative Innovation Center of Chinese Medicinal Resources Industrialization, Nanjing, Jiangsu 210023, PR China Jiangsu Key Laboratory for High Technology Research of TCM Formulae, Nanjing University of Chinese Medicine, Nanjing, Jinagsu 210023, PR China
J Chromatogr Sci. 2015 Sep;53(8):1386-94. doi: 10.1093/chromsci/bmv030. Epub 2015 May 6.
In this study, a simple, rapid, efficient analytical method was established for the qualification and quantification of 16 nucleosides and nucleobases in Euryale ferox Salisb. by using liquid chromatography coupled with electrospray ionization tandem triple quadrupole mass spectrometry (HPLC-ESI-TQ-MS/MS) in multiple-reaction monitoring (MRM) mode. Ideal separation of 16 target compounds was achieved on Xbridge Amide HILIC column (4.6 × 150 mm, 3.5 μm) with gradient elution in 11 min by optimized conditions. Variations of nucleosides and nucleobase in samples from different cultivation regions ranging from 190.50 to 1594.30 μg/g were obvious. The total nucleoside contents were higher than total nucleobases, especially in the compositions of guanosine, cytidine and 2'-deoxyguanosine. Samples 1-18 with dense thorns were better characters than samples 19-26 without thorns in terms of nucleosides and nucleobases concentrations in general. The limits of detection (LODs) and quantification (LOQs) for 16 analytical substances were investigated to be 0.11-6.33 ng/mL and 0.35-21.1 ng/mL, respectively. And the method was first applied to large aquatic plants with good linearity, precision, repeatability and accuracy. All present information provided a scientific and rational reference for quality assessment and control of Euryale ferox Salisb.
本研究建立了一种简单、快速、高效的分析方法，采用液相色谱-电喷雾电离串联三重四极杆质谱联用仪（HPLC-ESI-TQ-MS/MS）的多反应监测（MRM）模式，对芡实中的16种核苷和碱基进行定性和定量分析。在优化条件下，16种目标化合物在Xbridge酰胺HILIC柱（4.6×150 mm，3.5μm）上实现了理想分离，11分钟内梯度洗脱。不同种植区域样品中核苷和碱基的含量变化明显，范围为190.50至1594.30μg/g。总核苷含量高于总碱基含量，尤其是鸟苷、胞苷和2'-脱氧鸟苷的组成。总体而言，带刺的样品1-18在核苷和碱基浓度方面的品质优于无刺的样品19-26。研究了16种分析物的检测限（LOD）和定量限（LOQ），分别为0.11-6.33 ng/mL和0.35-21.1 ng/mL。该方法首次应用于大型水生植物，具有良好的线性、精密度、重复性和准确性。所有现有信息为芡实的质量评估和控制提供了科学合理的参考。
