基于UPLC-Q-Exactive Orbitrap-MS和碎片离子检索技术分析莱菔子中硫苷类化合物

Glucosinolates analysis in Raphani Semen based on UPLC-Q-Exactive Orbitrap-MS and fragment ion search technology

目的:基于超高效液相色谱-四极杆-静电场轨道阱质谱(UPLC-Q-Exactive Orbitrap-MS)结合碎片离子检索技术全面表征莱菔子中的硫苷类化合物。方法:采用UPLC-Q-Exactive Orbitrap-MS采集质谱数据,根据硫苷标准品的MS/MS质谱图以及相关文献,确定硫苷类化合物特征性碎片离子。基于Mass Frontier 7.0中碎片离子检索技术,利用硫苷类化合物的特征碎片离子,实现对硫苷类化合物快速定位,并根据质谱所提供的保留时间、精确分子量、对照品信息和相关文献鉴定硫苷。结果:确定硫苷类化合物的特征碎片离子为m/z 290.9844、274.9895、259.0124、241.0018、195.0327、96.9596和79.9568,并从莱菔子中共鉴定出21个硫苷类化合物,包含12个脂肪族硫苷,3个芳香族硫苷,4个吲哚族硫苷以及2个未知硫苷。结论:该方法能够实现对莱菔子中的硫苷类化合物快速识别和准确鉴定,为莱菔子的药效物质深入研究及质量控制奠定基础。

Objective:To characterize the glucosinolates in Raphani Semen using ultra-high performance liquid chromatography-quadrupole exactive Orbitrap mass spectrometry(UPLC-Q-Exactive Orbitrap-MS)combined with fragment ion search technology.Methods:The mass data was acquired using the UPLC-Q-Exactive Orbitrap-MS,and the characteristic fragment ions of glucosinolates were determined according to the MS/MS mass spectra of standards and related literatures.The fragment ion search technology in Mass Frontier 7.0 was used to quickly locate glucosinolates,and the glucosinolates were further identified based on the retention time,accurate molecular weight,and related literature references.Results:The characteristic fragments of glucosinolates were determined at m/z 290.9844,274.9895,259.0124,241.0018,195.0327,96.9596 and 79.9568.A total of 21 glucosinolates were identified from Raphani Semen,including 12 aliphatic glucosinolates,3 aromatic glucosinolates,4 indole glucosinolates and two unknowns.Conclusion:This method could rapidly identify glucosinolate,laying a foundation for in-depth research andqualitycontrol of Raphani Semen.