基于UPLC-LTQ-Orbitrap高分辨质谱的地骨皮化学成分分析

Identification of compounds in Lycii Cortex by UPLC-LTQ-Orbitrap-MS

基于超高效液相色谱-线性离子阱-静电场轨道阱高分辨质谱系统(UPLC-LTQ-Orbitrap-MS)分析鉴定中药地骨皮的化学成分。采用Waters Xbridge Shield RP18色谱柱(4. 6 mm×250 mm,5μm),用0. 1%甲酸水溶液(A)-乙腈(B)为流动相进行梯度洗脱,流速1. 0 m L·min-1,柱温35℃。质谱使用ESI离子源,正、负离子分析模式采集数据,通过高分辨质谱解析,并结合相关文献和对照品进行比对共指认出55个化合物,包括酚酰胺成分39个,有机酸成分6个,环肽类成分3个,香豆素类成分2个和5个其他成分。该实验应用UPLC-LTQ-Orbitrap高分辨液质联用技术对地骨皮的化学成分进行较为全面地分析,并归纳总结地骨皮中酚酰胺化学成分的裂解规律,为进一步研究地骨皮的化学成分提供了良好的基础。

This experiment was performed to analyze and identify the chemical constituents of Lycii Cortex by UPLC-LTQ-OrbitrapMS.The analysis was performed on a Waters Xbridge Shield RP18(4.6 mm×250 mm,5μm)column with the mobile phase of 0.1%formic acid(A)-acetonitrile(B)under gradient conditions at a flow rate of 1.0 m L·min-1 and the temperature maintained at 35℃.Electrospray ionization ion trap time-off light multistage mass spectrometry was applied for qualitative analysis under positive and negative ion modes.The results indicated that 55 compounds consisted of 39 phenolic amides,6 organic acids,3 cyclic peptides,2 coumarins and 5 others.In conclusion,an UPLC-LTQ-Orbitrap-MS method was established to qualitative analysis of Lycii Cortex in this study,and the fragmentation rules of phenolic amides were summarized,which provides a good foundation for further study of Lycii Cortex.