建立了基于超高压液相色谱-电喷雾-高分辨质谱联用技术（ UHPLC-ESI-HRMS）的中药虎杖化学成分的快速定性分析方法。采用 Waters UPLC C18色谱柱，乙腈-甲酸水系统梯度洗脱，采用 ESI-LTQ-Orbitrap 高分辨杂交质谱技术负离子采集，线性离子阱质谱进行多级质谱碎裂，轨道离子阱高分辨检测，获取多维质谱数据。利用代表性成分的诊断离子进行搜寻，结合质谱偶电子规律、氮规律、不饱和度和同位素峰等信息，参阅文献，总结主要成分的裂解规律，对主要峰进行指认与鉴定。结果显示，整个分析过程在10 min 内完成，该方法分离良好，灵敏度高。对虎杖根中的34种成分进行了结构分析，研究从中药虎杖中发现了多种酚酸取代二苯乙烯苷、酚酸取代蒽醌苷和蒽醌硫酸盐衍生物等成分。研究结果表明本方法为虎杖的后续化学成分研究、相关产品的质量控制和药效物质基础的研究提供了一种高效、可靠的检测手段。
A method for qualitative analysis of constituents in Polygonum cuspidatum by ultra-high-pressure liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometry ( UHPLC-LTQ-Orbitrap MS)has been established. The methanol extract of Polygonum cuspida-tum was separated on a Waters UPLC C 18 column using acetonitrile-water( containing formic acid)eluting system and detected by LTQ-Orbitrap hybrid mass spectrometer in negative mode. The targeted components were further fragmented in LTQ and high accuracy data were acquired by Orbitrap MS. The summarized fragmentation pathways of typical reference components and a diagnostic fragment ions-searching-based strategy were used for detection and identification of the main phenolic components in Polygonum cuspidatum. Other clues such as nitrogen rule, even electron rule,degree of unsaturation rule and isotopic peak data were included for the structural elucidation as well. The whole analytical procedure was within 10 min and more than 30 components were identified or tentatively identified. This method is helpful for further phyto-chemical research and quality control on Polygonum cuspidatum and related preparations.
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